Yan-ping Shi

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Organization: Chinese Academy of Sciences
Department: Lanzhou Institute of Chemical Physics
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Co-reporter:Hai-Long Jiang, Jun-Li Yang, Yan-Ping Shi
Ultrasonics Sonochemistry 2017 Volume 34() pp:325-331
Publication Date(Web):January 2017
DOI:10.1016/j.ultsonch.2016.06.003
•Ultrasonic cell grinder extraction (UCGE) was firstly applied to extract anthocyanins from blueberry.•Extraction conditions were optimized by response surface methodology (RSM) using Box-Behnken design.•Scanning electron microscopy (SEM) was used to discuss the UCGE mechanism.•UCGE was an innovative, efficient and environment friendly method in ultrasonic extraction field.Ultrasonic cell grinder extraction (UCGE), using water as the solvent, was firstly applied to extract anthocyanins from blueberry. Extraction yield was related with four variables, including ratio of solution to solid, extraction power, buffer time, and extraction time. On the basis of response surface methodology (RSM), the optimal conditions were determined to be the ratio of solution to solid as 25:1 (mL/g), the extraction power as 1500 W, the buffer time as 3.0 s, and the extraction time as 40 min. The experimental yield of anthocyanins using UCGE was 2.89 mg/g higher than that of conventional ultrasound-assisted extraction (CUAE). This study indicated that UCGE was an innovative, efficient, and environment friendly method in ultrasonic extraction fields, and had a potential to effectively extract other bioactive constituents.
Co-reporter:Lei-Lei Liu, Thi Kim Quy Ha, Wei Ha, Won Keun Oh, Jun-Li YangYan-Ping Shi
Journal of Natural Products 2017 Volume 80(Issue 2) pp:
Publication Date(Web):February 3, 2017
DOI:10.1021/acs.jnatprod.6b00694
A phytochemical investigation of the flowers of Chrysanthemum indicum yielded sesquiterpenoids 1–25 with various carbocyclic skeletons, including 10 new (1–10) and 15 known (11–25) analogues. The structures were elucidated via their physical data, while the absolute configuration of compounds 6, 8, and 10 was assessed via electronic circular dichroism analysis. The evaluation of the effect of sesquiterpenoids on porcine epidemic diarrhea virus (PEDV) replication showed that compounds 1–5, 12, 14, 16, 17, 19, and 21 increased cell viability against cell death in PEDV-injected cells. Compounds 2, 12, and 17 were selected and investigated for their inhibition of proteins required for PEDV replication. Compounds 2 and 17 significantly reduced PEDV nucleocapsid and spike protein synthesis compared with azauridin as a positive control.
Co-reporter:Yan-Ming Wang, Jian-Qiang Zhao, Jun-Li Yang, Yan-Duo Tao, Li-Juan Mei, Yan-Ping Shi
Biochemical Systematics and Ecology 2017 Volume 72(Volume 72) pp:
Publication Date(Web):1 June 2017
DOI:10.1016/j.bse.2017.03.007
•First phytochemical investigation on L. purdomii.•18 compounds were identified from the acetone extract of L. purdomii.•Four compounds were reported from the genus Ligularia for the first time.•The results had important significance for chemotaxonomy of L. purdomii.The first phytochemical investigation on the roots of Ligularia purdomii led to the isolation and identification of 18 compounds, including two eremophilane sesquiterpenoids (1 and 2), three benzofuran derivatives (3–5), a triterpenoid (6), two steroids (7 and 8), nine phenolic components (9–17), and a monofatty glyceride (18). The structural elucidation of the isolated compounds was performed by spectroscopic data and comparison with the literature. Compounds (−)-syringaresinol (11), scopoletin (13), 3,5-dimethoxy-4-hydroxy-benzaldehyde (14), and glycerol monolinoleate (18) have not been recorded in Ligularia genus previously. The chemotaxonomic significance of these isolated compounds has been summarized.
Co-reporter:Wen-kui Li, Hai-xia Zhang, Yan-ping Shi
Journal of Chromatography B 2017 Volume 1059(Volume 1059) pp:
Publication Date(Web):1 August 2017
DOI:10.1016/j.jchromb.2017.05.025
•An efficient MSPE-HPLC-UV method was established for AAAs determination.•An explored composite of MOFs and magnetic CNTs was employed for the MSPE of AAAs.•The MSPE mechanisms were attributed to multiple hydrogen bonding and π-π EDA interactions.•The proposed method was evaluated by MSPE of Trp, Tyr and Phe from Lanzhou lily samples.A novel magnetic solid-phase extraction (MSPE) based method was established for aromatic amino acids (AAAs) selective determination. Central to the method was the adopted extractant. An explored composite of metal organic frameworks (MOFs) and magnetic carbon nanotubes (CNTs) was employed for that, which exhibited superior adsorption affinity and selectivity to AAAs as compared to other amino acids with the mechanisms attributed to multiple hydrogen bonding and π-π electron-donor-acceptor (EDA) interactions. The morphology, structure and magnetic behavior of the composite were characterized and related MSPE procedure was established. Critical extraction conditions including pH, extraction time, temperature and salt addition were investigated and optimized. Subsequently the concentrations of three AAAs tryptophan (Trp), tyrosine (Tyr) and phenylalanine (Phe) in Lanzhou lily were determined by the composite based MSPE procedure coupled with high performance liquid chromatography-ultraviolet detection (HPLC-UV). The composite provided a superior sample clean-up function and many of the matrix interferences were eliminated, thus ensured AAAs were accurately and efficiently determined. The results showed that the method had good linearities with the linear coefficients above 0.99, desirable recoveries ranged from 88.0% to 96.8% with the RSD less than 5.1%, satisfactory precision and low limits of detection (LODs) which were respectively 0.04, 0.11, and 0.87 ng/g for Trp, Tyr and Phe. The composite based MSPE-HPLC-UV method has great potentials for the AAAs selective determination from complex matrix samples.
Co-reporter:Jian-Qiang Zhao, Yan-Ming Wang, Yan-Long Yang, Ying Zeng, Li-Juan Mei, Yan-Ping Shi, Yan-Duo Tao
Food Chemistry 2017 Volume 230(Volume 230) pp:
Publication Date(Web):1 September 2017
DOI:10.1016/j.foodchem.2017.03.024
•Twenty-five phenolic compounds were isolated and identified from “Liucha”.•Twenty-three compounds were reported from Sibiraea laevigata for the first time.•Phenolic compounds showed potent α-glucosidase inhibition and antioxidant activities.•Sorbitol ester F showed the best α-glucosidase inhibitory activity in vitro.The young leaves and shoots of Sibiraea laevigata, known as “Liucha”, are used as tea by Tibetans to improve digestion after meals. Long-term consumption of “Liucha” will cause weight loss. In present work, we reported on the isolation and NMR and chemical analysis-based elucidation of seven new sorbitol O-caffeic acid ester derivatives named sorbitol esters A–G (1–7) and eighteen known phenolic compounds from S. laevigata. All of the isolates were evaluated for their antioxidant and α-glucosidase inhibitory activities. Among them sorbitol ester A (1), sorbitol ester D (4), sorbitol ester F (6), sorbitol ester G (7), isoferulic acid (15), methyl caffeate (18), trans-p-hydroxycinnamic acid (19), and kaempferol 3-O-β-d-(6″-E-p-coumaroyl)-glucopyranoside (25) showed more potent α-glucosidase inhibitory activity than the clinical drug acarbose.
Co-reporter:Wen-kui Li, Hai-xia Zhang, Yan-ping Shi
Applied Surface Science 2017 Volume 416(Volume 416) pp:
Publication Date(Web):15 September 2017
DOI:10.1016/j.apsusc.2017.04.202
•A novel, efficient, and high-selectivity magnetic adsorbent was fabricated for adsorption and determination of aromatic acids.•The adsorbent was sensitive to adsorbates with multi-ring, multi-carboxylic and electron-withdrawing group substituted structures.•Selective adsorption of aromatic acids by the novel adsorbent was attributed to π-π EDA and hydrogen-bonding interactions.•Adsorption of aromatic acids was spontaneous and endothermic, well fit for the Dubinin-Ashtakhov model and pseudo-second-order model.A novel magnetic adsorbent was designed and synthesized for adsorption and determination of hazardous aromatic acids (AAs) based on the zeolite imidazolate frameworks of Eu (ZIF-Eu), Fe3O4 and carboxyl multi-walled carbon nanotubes (MWCNTs-COOH). ZIF-Eu was fabricated for the first time, and Fe3O4 nanoparticles were encapsulated in MWCNTs-COOH, which made the separation procedure simple and easy-realizable. Adsorption experiments indicated that the adsorbent had superior affinity and selectivity to adsorbates with multi-ring, multi-carboxylic and electron-withdrawing group substituted structures, and it can achieve the selective adsorption of AAs from the aromatic mixture, the mechanism of which was evaluated and attributed to the intermolecular π-π electron-donor-acceptor (EDA) and hydrogen-bonding interactions. Seven AAs with different substituents were selected as target adsorbates to investigate the influences of critical experimental conditions on the adsorption efficiencies. Adsorption isotherms and kinetics were investigated and indicated that Dubinin-Ashtakhov model and pseudo-second-order model could well describe the adsorption of AAs on the nanocomposite. Adsorption thermodynamics study suggested that the adsorption reactions were spontaneous, endothermic and thermodynamically favorable. In addition, desorption conditions for AAs, and reusability of the novel adsorbent was evaluated, which confirmed the recyclability of the novel adsorbent.Download high-res image (185KB)Download full-size image
Co-reporter:Xiao-Bo Zhao;Wei Ha;Kan Jiang;Juan Chen;Jun-Li Yang
Green Chemistry (1999-Present) 2017 vol. 19(Issue 5) pp:1399-1406
Publication Date(Web):2017/03/06
DOI:10.1039/C6GC03119F
In this work, for the first time, we report an efficient, simple strategy for synthesizing active camptothecin (CPT) derivatives in water. A novel macroporous adsorption resin-supported gold nanoparticle (MAR-AuNP) was first in situ prepared in water. The resulting MAR-AuNPs swell in water and were applied not only as an efficient adsorbent for hydrophobic CPT molecules, but also as a catalyst for the Mannich reaction of CPT, formaldehyde and amines with water as a solvent. A series of novel CPT propargylamine derivatives were successfully obtained with high yields by virtue of such a strategy. Moreover, the resulting CPT propargylamine derivatives exhibited excellent cytotoxicity against two different tumor cell lines. This novel and efficient strategy, avoiding the use of toxic solvents, represents a promising green route for drug discovery from natural products and shows great potential in the green pharmaceutical industry.
Co-reporter:Run-tian Ma;Xiao-yu Sun;Wei Ha;Juan Chen
Journal of Materials Chemistry B 2017 vol. 5(Issue 36) pp:7512-7518
Publication Date(Web):2017/09/20
DOI:10.1039/C7TB01519D
We wished to improve the unsatisfactory adsorption and elution efficiencies in conventional magnetic molecular imprinting technology. In this work, a reliable strategy to prepare magnetic molecularly imprinted nanoparticles (MMINs) with rapid rebinding and elution speed was introduced. To decrease the mass-transfer retention of the templates, glycoprotein immunoglobulin (Ig)G was pre-immobilized to form homogeneous and monostratified three-dimensionally imprinted cavities on the surface of magnetic carriers. To shorten the transfer route of the templates, the polymerizaiton process was controlled precisely to form well-defined molecularly imprinted polymer (MIP) films of thickness 12 nm. In this way, the effectiveness of the mass transfer of the templates was maximized, and the length of the transfer route was minimized. As a result, the prepared MMINs showed improved adsorption and elution efficiencies compared with the conventional magnetic molecularly imprinted polymers (MMIPs), and exhibited great selectivity towards the templates.
Co-reporter:Wen-kui Li, Juan Chen, Hai-xia Zhang, Yan-ping Shi
Talanta 2017 Volume 168(Volume 168) pp:
Publication Date(Web):1 June 2017
DOI:10.1016/j.talanta.2017.03.034
•A novel and efficient MSPE adsorbent was designed for aromatic acids.•The adsorbent can achieve the selective extraction of aromatic acids from the aromatic mixture.•The selective extraction of aromatic acids was attributed to hydrogen bonding and π-π EDA interactions.•The potential application of the adsorbent was evaluated by MSPE of trace NAA, TPA and CA from apple samples.A novel, efficient, and high-selectivity magnetic solid-phase extraction (MSPE) adsorbent based on Fe3O4 nanoparticles, hydroxylated multi-walled carbon nanotubes (MWCNTs-OH) and metal-organic frameworks (MOFs) was prepared and applied for trace aromatic acids determination in solid samples by applying a template-free in situ strategy. The morphology, configuration and magnetic behavior of the adsorbent were characterized by scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectra, and vibrating sample magnetometer (VSM). The adsorbent can achieve the selective extraction of aromatic acids from the aromatic mixture in apple samples, which was mainly promoted by intermolecular hydrogen bonding and π-π electron-donor-acceptor (EDA) interaction. The potential application of the adsorbent was evaluated by MSPE of trace 1-naphthylacetic acid (NAA), cinnamic acid (CA) and terephthalic acid (TPA) from apple samples under the optimal conditions which were investigated. Satisfactory linearities were obtained in a range of 5–500 ng/g and the recoveries of three aromatic acids at three spiked levels ranged from 91.2% to 98.0% with the relative standard deviations (RSD) of less than 5.5%. The limits of detection (LODs) for CA, TPA and NAA were 0.17, 0.61, and 0.86 ng/g. The satisfactory results confirmed the great potential of the novel adsorbent for the selective extraction of aromatic acids from complex sample matrices.Download high-res image (258KB)Download full-size image
Co-reporter:Xiao-Yu Sun;Run-Tian Ma;Juan Chen
Microchimica Acta 2017 Volume 184( Issue 9) pp:3637-3637
Publication Date(Web):01 August 2017
DOI:10.1007/s00604-017-2431-9
Erratum to: Microchimica ActaDOI: 10.1007/s00604-017-2373-2The original version of this article unfortunately contained a mistake in the Acknowledgements section. Given in this article is the correct acknowledgement statement.
Co-reporter:Dong-Mei Liu, Juan Chen, Yan-Ping Shi
Talanta 2017 Volume 164() pp:548-555
Publication Date(Web):1 March 2017
DOI:10.1016/j.talanta.2016.12.028
•Fe3O4/CS/GA/α-Glu coupled with CE was developed for screening enzyme inhibitors.•Fe3O4/CS/GA/α-Glu was prepared by using CS as modifier and GA as cross linker.•The dispersity of Fe3O4 nanoparticles was improved by solvothermal method.•α-Glucosidase inhibitors were screened from 18 TCMs in this study.As the close correlation between α-glucosidase inhibitors and the treatment of diabetes, in combination with capillary electrophoresis (CE), a method was developed to screen α-glucosidase inhibitors from traditional Chinese medicines (TCMs) by immobilizing α-glucosidase on magnetic nanoparticles. Such a magnetic immobilization would be beneficial for enzyme reusability, stability and separation. In this work, Fe3O4 nanoparticles were synthesized by solvothermal method. And the prepared nanoparticles were characterized by transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), size and zeta potential analysis. With the modification of chitosan (CS) and glutaraldehyde (GA), α-glucosidase was successfully immobilized on the magnetic nanoparticles. The pH and temperature endurance, storage stability and reusability of the immobilized α-glucosidase were studied and compared with those of the free one. With the magnetic immobilized α-glucosidase, the Michaelis-Menten constant (Km) was calculated to be 0.85 mM, and the inhibition constant (Ki) and half-maximal inhibitory concentration (IC50) for acarbose were determined to be 7.37 and 13.69 μM, respectively. Finally, the developed method was applied to screen α-glucosidase inhibitors from 18 TCMs.Highly dispersed magnetic nanoparticles were synthesized by solvothermal method and α-glucosidase was immobilized on the magnetic nanoparticles with the modification of chitosan and glutaraldehyde. With α-glucosidase-immobilized magnetic nanoparticles, an efficient method was developed to screen α-glucosidase inhibitors from traditional Chinese medicines in combination with capillary electrophoresis.
Co-reporter:Run-Tian Ma, Wei Ha, Juan Chen and Yan-Ping Shi  
Journal of Materials Chemistry A 2016 vol. 4(Issue 15) pp:2620-2627
Publication Date(Web):17 Mar 2016
DOI:10.1039/C6TB00409A
Antibody-free analysis is a potential method for glycoprotein analysis, but the development of this method has been limited by its unfavorable selectivity in recent years. Magnetic molecular imprinting, which integrates the fast separation of magnetic materials with high selectivity towards templates in molecular imprinting, was expected to be an effective sample pretreatment in antibody-free analysis for glycoproteins. However, the aggregation of magnetic imprinted nanoparticles and thick molecularly imprinted polymer (MIP) shells on the surface of magnetic carriers caused an unfavorable adsorption capacity, and unsatisfactory rebinding and elution rates, and has limited its application in glycoprotein extraction. Thus, highly dispersed magnetic molecularly imprinted nanoparticles (MMINs) with a well-defined thin film for the selective extraction of glycoprotein HRP were developed in this work. A solvothermal method was used in this work to improve the dispersity of Fe3O4 NPs (nanoparticles) and the MMINs. The thickness of the MIP film was optimized to provide the optimum extraction efficiency. Thus the adsorption capacity of the MMINs, the rebinding rate and the elution rate of the templates were greatly improved. As a result, the prepared MMINs not only exhibited excellent selectivity and high adsorption capacity to HRP, and an outstanding tolerance for interference, but also showed excellent rebinding and elution rates for extraction application. Furthermore, this method provided a reliable way to improve conventional magnetic molecular imprinting, and showed great potential for the analysis of glycoprotein tumor biomarkers in clinics in the future.
Co-reporter:Na Li, Juan Chen, Yan-Ping Shi
Journal of Chromatography A 2016 Volume 1441() pp:24-33
Publication Date(Web):8 April 2016
DOI:10.1016/j.chroma.2016.02.077
•Fe3O4/RGO@(*)β-CD was prepared by modifying Fe3O4/RGO with β-CD.•Fe3O4/RGO@β-CD was applied in MSPE to study its extraction performance in real samples.•Fe3O4/RGO@β-CD showed good molecular selectivity toward naphthalene-derived phytohormones.•RSM was used to optimize experimental parameters affecting the extraction efficiency in detail.•The proposed method had merits of simplicity, high sensitivity and selectivity.A β-cyclodextrin (β-CD) functionalized magnetic reduced graphene oxide composite (Fe3O4/RGO@β-CD) has been prepared and its application as a selective adsorbent for the determination of the two naphthalene-derived phytohormones (1-naphthalene acetic acid (NAA) and 2-naphthoxyacetic acid (2-NOA)) has been investigated. Magnetic reduced graphene oxide composite (Fe3O4/RGO) was first synthesized via in situ chemical precipitation method and then β-CD was applied to further functionalize the resultant Fe3O4/RGO composite. The as-prepared Fe3O4/RGO@β-CD was characterized by Fourier transform infrared spectrometry (FT-IR), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM). Compared with Fe3O4/RGO, the as-prepared Fe3O4/RGO@β-CD showed better molecular selectivity and higher extraction efficiency for NAA and 2-NOA by dint of the size complementarity brought by the introduction of β-CD. Response surface methodology (RSM), a multivariate experimental design technique, was used to optimize experimental parameters affecting the extraction efficiency in detail. Under the optimal conditions, good performance data was obtained. The calibration curves were linear over the concentration ranging from 2 to 600 ng g−1 with correlation coefficients (R2) between 0.9995 and 0.9997 for all the analytes. The limits of detection (LODs) were 0.67 ng g−1 for both NAA and 2-NOA. The intra- and inter-day relative standard deviations (RSDs) were less than 6.02% and 7.34%, respectively. The recoveries ranged from 91.45% to 95.89%. Taken together, the proposed method was an efficient pretreatment and enrichment procedure and could be successfully applied for selective extraction and determination of naphthalene-derived phytormones in complex matrices.
Co-reporter:Yan-Ming Wang, Jian-Qiang Zhao, Jun-Li Yang, Yan-Duo Tao, Li-Juan Mei, and Yan-Ping Shi
Journal of Agricultural and Food Chemistry 2016 Volume 64(Issue 24) pp:4950-4957
Publication Date(Web):May 27, 2016
DOI:10.1021/acs.jafc.6b02096
Asterothamnus centrali-asiaticus, a kind of characteristic shrub abundant in grassland and desert areas, has been used as forage fodder for camels and goats in Central Asia, and this plant also plays a critical role in the maintenance of desert grassland ecosystems as a result of its tolerance to poor soils and sand burial. However, its chemical composition has been rarely reported. In this study, phytochemical investigation of this pasturage was performed and three new triterpenoid saponins (1–3) were isolated together with nine known triterpenoid saponins (4–12) using preparative two-dimensional reversed-phase liquid chromatography/hydrophilic interaction chromatography (2D RPLC/HILIC). Their structures were elucidated via diverse spectroscopic analyses, including infrared (IR) spectrometry, high-resolution electrospray ionization mass spectrometry (HR-ESIMS), and one-dimensional (1D) and 2D nuclear magnetic resonance (NMR). All isolated triterpenoid saponins (1–12) were reported from this genus for the first time, and they were further evaluated for their cytotoxicity against four cancer cell lines (A549, HepG2, MGC-803, and MFC), which indicated that compound 11 showed potent cytotoxicity against the HepG2 cell line, with an IC50 value of 6.85 μg/mL.
Co-reporter:Yan-Ming Wang, Jian-Qiang Zhao, Chun-Yan Yang, Yan-Duo Tao, Li-Juan Mei, Yan-Ping Shi
Phytochemistry Letters 2016 Volume 17() pp:71-74
Publication Date(Web):September 2016
DOI:10.1016/j.phytol.2016.07.021
⿢Two new phenolic acids (1⿿2) were isolated from the aerial parts of Asterothamnus centrali-asiaticus.⿢Five knownphenolic acids (3⿿7) were also obtained from the title plant.⿢1⿿7 were evaluated for their anti-oxidant activity.⿢1⿿7 showed anti-oxidant activity with IC50 values ranging from 7.65 to 22.44 μg/mL.Two new phenolic acids 2-hydroxy-5-[(6⿲-O-(E)-caffeoyl)-β-d-glucopyranosyl]-oxybenzoic acid (1) and 2-hydroxy-5-[(3⿲-O-(E)-caffeoyl)-β-d-glucopyranosyl]-oxybenzoic acid (2) were isolated from the aerial parts of Asterothamnus centrali-asiaticus, together with five known ones (3-7). Their structures were elucidated by extensive 1D and 2D NMR studies and HRESIMS investigations. The anti-oxidant activity of the isolates was evaluated through ABTS radical cation decolorization assay. The results showed that all of them exhibited anti-oxidant activity, and compound 7 was the most active compound with an IC50 value of 7.65 μg/mL.
Co-reporter:Hai-Long Jiang, Wei Ha, Jun-Li Yang, Yan-Ping Shi
Phytochemistry Letters 2016 Volume 17() pp:1-5
Publication Date(Web):September 2016
DOI:10.1016/j.phytol.2016.06.004
⿢Two new sesquiterpenepolyol esters were isolated from Pseudolarix kaempferi.⿢All known compounds were isolated from Pseudolarix genus for the first time.⿢CD exciton chirality method was used to determine the absolute configuration of new compounds.A series of sesquiterpene polyol esters, including two new β-dihydroagarofuran sesquiterpenes (1-2) and 14 known compounds (3-16), were isolated from the root bark of Pseudolarix kaempferi. The esters⿿ structures were elucidated by employing extensive spectroscopic analyses and by comparison to literature compounds. The absolute configurations of the two new compounds were determined by the CD exciton chirality method. The known compounds 3-16 were isolated from the Pseudolarix genus for the first time.
Co-reporter:Jun-Li Yang;Ya-Min Zhao
Natural Products and Bioprospecting 2016 Volume 6( Issue 4) pp:211-216
Publication Date(Web):2016 August
DOI:10.1007/s13659-016-0104-8
Naturally occurring oplopanane sesquiterpenoids are rarely reported. A phytochemical investigation on the rhizomes of Homalomena occulta (Lours) has resulted in the discovery of six oplopanane sesquiterpenoids (1–6), including four new (1–4) and one 3,5-seco-oplopanane (6), together with three previously reported sesquiterpenoids (7−9). In addition three new oplopananes (2a–4a) were also obtained by chemical transformation. All structures of these sesquiterpenoids were established based on the comprehensive spectroscopic analyses, including NMR, MS, and IR, and comparing with the literatures.
Co-reporter:Yan-Ming Wang, Jian-Qiang Zhao, Shuang-Yan Zhou, Jun-Li Yang, Xiao-Jun Yao, Yan-Duo Tao, Li-Juan Mei, Yan-Ping Shi
Tetrahedron 2016 Volume 72(Issue 32) pp:4910-4917
Publication Date(Web):11 August 2016
DOI:10.1016/j.tet.2016.06.061
Phytochemical investigation on Asterothamnus centrali-asiaticus afforded four new sesquiterpenes, asterothamnones A–D (1–4), and three new benzofuran derivatives (5–7) together with ten known compounds (8–17). Their structures were elucidated using 1D and 2D NMR and X-ray diffraction analyses. Compounds 1–4 were verified to be unusual eudesmane sesquiterpenes possessing 4,6-dien-3-one or 1,4,6-triene-3-one conjugated system. The absolute configurations of compounds 1–8 were established by means of calculated electronic circular dichroism (ECD). Furthermore, all isolates were evaluated for their cytotoxic and anti-oxidant activities. Results showed that 10, 12 and, 14 exhibited cytotoxic activity against HepG2 cancer cells and 14 displayed cytotoxicity against MGC-803 cancer cells. Compounds 10 and 17 showed anti-oxidant effect.
Co-reporter:Ying-pei Sun, Wei Ha, Juan Chen, Huan-yang Qi, Yan-ping Shi
TrAC Trends in Analytical Chemistry 2016 Volume 84(Part A) pp:12-21
Publication Date(Web):November 2016
DOI:10.1016/j.trac.2016.03.002
•G-C3N4 had been applied to sample pretreatment with SPE, MSPE and SPME modes.•The in-built N-rich functional groups and electronic delocalization properties endow g-C3N4 with complex sorption mechanism.•The physicochemical properties and sorption behaviors of g-C3N4 can be influenced by the polymerization temperature, the type of precursors, and the solution pH and ion strength.•Numerous modification methods had been exploited to enhance the sorption ability of g-C3N4.As a green and efficient sorbent, graphitic carbon nitride (g-C3N4) with aromatic tri-s-triazine units has shown great potential for the enrichment or removal of metal ions and organic aromatic compounds, which makes it a promising candidate to complement graphenes in analytical chemistry. The in-built N-rich functional groups and electronic delocalization properties endow g-C3N4 with complex sorption mechanism, containing complexion, hydrogen bond, redox reaction, π – π conjugation, hydrophobic effect, acid-base reaction and electrostatic interaction. The structure and surface physicochemical properties related to the sorption behavior are mainly depended on the preparation and sorption conditions, such as polymerization temperature, polymerization precursors, the solution pH and ionic strength. As a new sorbent, g-C3N4 has been applied to the sample pretreatment in analytical chemistry with solid-phase extraction (SPE), magnetic solid-phase extraction (MSPE), and solid-phase microextraction (SPME) modes, recently. At the same time, a series of modification methods and technologies have been exploited to modify the structural and surface physicochemical properties of g-C3N4, facilitating more effective and selective sorption process. To raise awareness of the superior properties of g-C3N4 and facilitate its applications as a sorbent in analytical chemistry, the sorption properties (sorption mechanism, influence factors of sorption behavior), applications to the sample pretreatment and structural modifications of g-C3N4 are reviewed.
Co-reporter:Wei Ha, Xin-yue Song, Juan Chen and Yan-ping Shi  
Nanoscale 2015 vol. 7(Issue 44) pp:18619-18627
Publication Date(Web):09 Oct 2015
DOI:10.1039/C5NR05454K
In this paper, we demonstrate a novel carbon nanotube (CNT) reinforced macroporous adsorption resin (MAR) for the first time. The CNTs were dispersed in water via sonication, and then in situ physically entrapped in the pores of MAR by capillary forces and sonication. The resulting CNT reinforced MAR (CNT–MAR) was proved by transmission electron microscopy (TEM) and confocal laser scanning microscopy (CLSM), and subsequently applied to extract a mixture of 8 types, 14 natural products. For comparison, the extraction efficiency of original MAR without CNTs was also evaluated. After extraction, the supernatants were detected via high-performance liquid chromatography (HPLC). The results indicated that the introduction of carbon nanotubes (CNTs) into the pores of MAR can significantly improve the adsorptive selectivity of MAR for natural products. The original MAR without CNTs has almost the same adsorption capacity for selectively extracting 3 types of natural products (phenols, alkaloids and anthraquinones). However, the CNT–MAR only could selectively extract anthraquinones and the adsorption capacity for three anthraquinone natural products is 1.46–1.83 times higher than that of unmodified MAR. In order to achieve the highest extraction efficiency of CNT–MAR for anthraquinone natural products, the main extraction parameters such as the extraction time and the pH value were also optimized. The CNT–MAR demonstrated an excellent ability to extract anthraquinone natural products with high selectivity and adsorption capacity. Due to its low cost, easy preparation and use, and operational characteristics, it shows great potential for selective extraction of natural products.
Co-reporter:Xin-Yue Song, Juan Chen and Yan-Ping Shi  
New Journal of Chemistry 2015 vol. 39(Issue 12) pp:9191-9199
Publication Date(Web):11 Sep 2015
DOI:10.1039/C5NJ01683E
In this work, an electromembrane extraction (EME) technique based on carbon nanotubes reinforced hollow fiber (CNTs-HF) was developed and applied to determine two plant hormones in tomato samples. The CNTs-HF was prepared by a feasible physical method in which CNTs were dispersed in 1-hexanol and then immobilized into the wall pores of HF supported by capillary forces and sonication. Subsequently, the CNTs-HF was placed in tomato samples to extract plant hormones under electric field drive. In this mode, porous HF held the extractants and provided excellent sample clean-up ability. 1-Hexanol and CNTs held in the wall pores of HF served as a supported liquid membrane (SLM) and a sorbent, respectively, enabling the enrichment and migration of the analytes. The comparison between CNTs-HF-EME and HF-EME showed that CNTs could increase the overall partition coefficient of analyte in the membrane due to their large surface area and high adsorption capacity. In order to achieve the best extraction efficiency, optimal conditions of CNTs-HF-EME were obtained using 1-hexanol as the SLM, 105 V of applied voltage, pH 9 and 13 of the sample solution and the acceptor phase, respectively, an extraction time of 0.5 min and a stirring rate of 1200 ± 24 rpm. Under these conditions, CNTs-HF-EME was able to provide higher enrichment factors and lower limits of detection and quantification within a shorter extraction time, compared to the HF-EME. This newly developed extraction method has been shown to be a rapid, feasible, and cost-effective sample pretreatment technique for trace analysis in complex matrices.
Co-reporter:Tang-Juan Zhao, Huan-Yang Qi, Juan Chen and Yan-Ping Shi  
RSC Advances 2015 vol. 5(Issue 126) pp:103869-103875
Publication Date(Web):20 Nov 2015
DOI:10.1039/C5RA21233B
A rapid and efficient ultra-performance convergence chromatography (UPC2) method coupled with electrospray ionization single quadrupole mass spectrometry (ESI-MS) was developed and validated for the simultaneous quantification of five diester diterpenoid alkaloid constituents (3-acetylaconitine, hypaconitine, deoxyaconitine, mesaconitine, aconitine) in Aconitum pendulum. Optimum separation was achieved on a BEH 2-EP C18 column (2.1 × 150 mm i.d., 1.7 μm particle) with a gradient elution of a mixture of A (supercritical CO2) and B (methanol containing 10 mmol L−1 ammonium acetate) and at a flow rate of 0.8 mL min−1 within 3 minutes. Quantification was performed using mass spectrometry in a positive ion ionization mode and selected ion recording (SIR) mode. The influences of column, modifier, additive, column temperature, and back pressure were investigated. The five alkaloids were identified and quantified using a comparison of retention time, ultraviolet spectrum, molecular ion peak (obtained from a selective ion recording mode) and peak areas with the reference compounds. The method was validated through linearity, limits of detection, limits of quantification, precision, stability, repeatability, and accuracy. The validated method was applied to analyze A. pendulum, which provided a reference for the quality evaluation of A. pendulum.
Co-reporter:Dong-Mei Liu, Juan Chen and Yan-Ping Shi  
RSC Advances 2015 vol. 5(Issue 70) pp:56841-56847
Publication Date(Web):29 Jun 2015
DOI:10.1039/C5RA07982A
In this work, a facile protocol for preparing an online immobilized α-glucosidase microreactor was described, and also the enzyme kinetics and inhibition kinetics of such an immobilized enzyme were studied. In this procedure, α-glucosidase was immobilized on the inner wall of the capillary treated with 3-aminopropyltriethoxysilane (3-APTES) and the homobifunctional linker glutaraldehyde (GA). With cross-linking technology, the immobilized α-glucosidase microreactor was fabricated. As the key point for studying the enzyme kinetics and inhibition kinetics of the immobilized α-glucosidase with the developed microreactor, pressure was applied as the driving force to push the reaction mixture to the detection window, and the detection wavelength was set to 405 nm at which only the formed p-nitrophenol (pNP) could be detected. More importantly, with such a detection wavelength it is unnecessary to separate the substrate from the reaction mixture by applying the alkaline inactivating background electrolyte (BGE, borate buffer, pH ≥ 9.0) which is favorable for the separation. So the incubation buffer (phosphate buffer, pH 7.0) could be used as the running buffer making the online study of the enzyme kinetics and inhibition kinetics of immobilized α-glucosidase come true. The inhibition assay was performed by using acarbose as a model inhibitor, and under the optimized conditions, the Michaelis–Menten constant (Km), inhibition constant (Ki), and half-maximal inhibitory concentration (IC50) for the immobilized α-glucosidase were determined as 0.43 mM, 30.65 μM and 99.48 μM, respectively. This study indicates, for the first time, that the immobilized α-glucosidase microreactor could be used for studying the enzyme kinetics and inhibition kinetics online.
Co-reporter:Tang-Juan Zhao, Juan Chen and Yan-Ping Shi  
Analytical Methods 2015 vol. 7(Issue 16) pp:6810-6820
Publication Date(Web):10 Jul 2015
DOI:10.1039/C5AY01093D
An efficient, accurate and reliable chromatographic fingerprint based on ultra-performance liquid chromatography coupled with photodiode array detection and electrospray ionization mass spectrometry (UPLC-PDA-ESI-MS) was developed for the identification and quality control of Oxytropis falcate Bunge. The method was validated for precision, repeatability, stability, and specificity. The RSD values of retention times and peak areas of the common peaks were 0–0.7% and 1.0–3.6% for within-day precision, while 0–0.5% and 1.5–6.1% for between-day precision. For repeatability, the values were lower than 0.5% and 2.6%, respectively, and for stability (24 h), the values were lower than 0.9% and 3.3%, respectively. Twenty-one batches of O. falcate obtained from different regions were analyzed by employing the developed method. Several multivariate statistical analysis including similarity analysis (SA), hierarchical clustering analysis (HCA) and principal component analysis (PCA) were applied to cluster and evaluate the O. falcate samples according to their collection sites. The results showed that the quality of O. falcate did not merely depend on the geographic origin. Thirty common peaks were found in the chromatographic fingerprints of O. falcate and eleven of them were identified by comparing the retention time, the ultraviolet spectrum and the molecular ion peaks (obtained from selective ion recording mode) with the reference compounds. This method with high precision, reliable stability and good repeatability can provide a reference for the quality evaluation of O. falcate.
Co-reporter:Yang Yang, Juan Chen, Yan-Ping Shi
TrAC Trends in Analytical Chemistry 2015 Volume 64() pp:109-117
Publication Date(Web):January 2015
DOI:10.1016/j.trac.2014.08.016
•We review four ways of modifying hollow fibers of polypropylene.•We review applications of hollow-fiber-based solid-phase microextraction (HF-SPME).•Modified HF-SPME has advantages over conventional SPME.Polypropylene hollow fibers (PPHFs) are usually applied for HF liquid-phase microextraction and have proved effective in various applications. By modifying PPHFs with sorbents, they can be used for solid-phase microextraction, and the method is novel, efficient and economical. This article mainly reviews the modification of PPHFs using carbon nanotubes, graphene, ceramic metal oxides and self-synthesized polymers.
Co-reporter:Ying-pei Sun, Juan Chen, Huan-yang Qi, Yan-ping Shi
Journal of Chromatography B 2015 Volume 1004() pp:53-59
Publication Date(Web):1 November 2015
DOI:10.1016/j.jchromb.2015.09.025
•A simple strategy on preparing graphitic carbon nitrides modified hollow fiber (g-CNs-HF) was proposed.•This novel g-CNs-HF was applied to extract uric acid (UA) directly in biofluids in a solid phase microextraction (SPME) mode.•The solvent-free g-CNs-HF realized desorption and derivatization simultaneously.•An analytical method coupled g-CNs-HF with gas chromatography-mass spectrometry (GC/MS) is established to determine UA in water urine and serum.An elevated uric acid (UA) in urine or serum can affect renal function and blood pressure, which is an indicator of gout, cardiovascular and renal diseases, hypertension, etc. In this work, a new type of mixed matrix membrane (MMM), based on graphitic carbon nitrides (g-CNs) and hollow fiber (HF), was prepared and combined with solid phase microextraction (SPME) mode to determine UA in urine and serum followed by gas chromatography-mass spectrometry (GC/MS). The porous g-CNs were dispersed in ammonia, and then the exfoliated g-CNs nanosheets were held in the pores of HF by capillary forces and sonification. The prepared g-CNs modified HF (g-CNs-HF) was immersed in biofluid directly to extract UA with SPME mode and the solvent-free mode is convenient for further derivatization and analysis. To achieve the highest extraction efficiency (EF), main extraction and derivatization parameters, such as g-CNs-HF immobilizing time, sonification power and time of extraction, derivatization and desorption time, were optimized. Under the optimum extraction conditions, a favorable linearity of UA was obtained in the range 0.1–200 μg mL−1 with correlation coefficients higher than 0.9990, and the average recoveries at three spiked levels of UA in urine and serum ranged from 80.7% to 121.6%, from 84.7% to 101.1%, respectively. The obtained results demonstrated the developed g-CNs-HF-SPME is a simple, rapid, cost-effective, solvent-free method for the analysis of UA in biofluid.
Co-reporter:Na Li, Juan Chen, Yan-Ping Shi
Talanta 2015 Volume 141() pp:212-219
Publication Date(Web):15 August 2015
DOI:10.1016/j.talanta.2015.04.018
•G-MNPs consist of zero-valent iron, iron oxide–oxyhydroxide and graphene.•G-MNPs were prepared through a simple one-step synthesis method.•G-MNPs were applied to MSPE for the determination of carbamates in tomatoes.•G-MNPs were not only employed as magnetic carrier, but also as adsorbents.•This novel method was proved to be simple, effective, sensitive and green.Graphene-based magnetic nanoparticles, comprising zero-valent iron, iron oxide–oxyhydroxide and graphene, were prepared through a simple one-step synthesis method, and subsequently applied to magnetic solid-phase extraction for the determination of trace carbamate pesticides in tomatoes coupled with high performance liquid chromatography. The properties of the nanocomposites were confirmed by using Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and vibrating sample magnetometer. The components within the nanocomposites endowed the material with high extraction performance and manipulative convenience. Compared with reduced graphene oxide, the as-prepared G-MNPs showed the better extraction efficiencies for the carbamate pesticides thanks to the contribution of the iron-containing magnetic nanoparticles to the adsorption capacity of the nanocomposites. Various experimental parameters affecting the extraction efficiency had been investigated in detail. Under the optimal conditions, the method provided high enrichment factors ranging from 364 to 434, good linearities ranging from 5 to 200 ng g−1 for metolcarb, baygon and methiocarb and 10 to 200 ng g−1 for carbofuran and isoprocarb, low limits of detection ranging from 0.58 to 2.06 ng g−1, and satisfactory spiked recoveries (between 90.34% and 101.98% with the relative standard deviation values from 1.21% to 5.93%). It was confirmed that this novel method was an efficient pretreatment and enrichment procedure and could be successfully applied for extraction and determination of trace carbamate pesticides in complex matrices.Graphene-based magnetic nanoparticles were prepared through a simple one-step synthesis method, and subsequently applied to magnetic solid-phase extraction for the determination of trace carbamate pesticides in tomatoes coupled with high performance liquid chromatography.
Co-reporter:Run-Tian Ma, Yan-Ping Shi
Talanta 2015 Volume 134() pp:650-656
Publication Date(Web):1 March 2015
DOI:10.1016/j.talanta.2014.12.003
•Quercetagetin imprinted polymer shell layer were prepared by surface imprinting.•The obtained MMIPs served as sorbents were used to recognize quercetagetin in TCM.•The prepared MMIPs were investigated by FT-IR, XRD and VSM.•The MMIPs were proved to be highly selective, easy to collect and low cost.A new magnetic molecularly imprinted polymers (MMIPs) for quercetagetin was prepared by surface molecular imprinting method using super paramagnetic core-shell nanoparticle as the supporter. Acrylamide as the functional monomer, ethyleneglycol dimethacrylate as the crosslinker and acetonitrile as the porogen were applied in the preparation process. Fourier transform infrared spectrometer (FT-IR), X-ray diffraction (XRD) and Vibrating sample magnetometer (VSM) were applied to characterize the MMIPs, and High performance liquid chromatography (HPLC) was utilized to analyze the target analytes. The selectivity of quercetagetin MMIPs was evaluated according to their recognition to template and its analogues. Excellent binding for quercetagetin was observed in MMIPs adsorption experiment, and the adsorption isotherm models analysis showed that the homogeneous binding sites were distributed on the surface of the MMIPs. The MMIPs were employed as adsorbents in solid phase extraction for the determination of quercetagetin in Calendula officinalis extracts. Furthermore, this method is fast, simple and could fulfill the determination and extraction of quercetagetin from herbal extract.Quercetagetin imprinted polymer shell layer were coated on the surface of the super-paramagnetic Fe3O4 nanoparticles through surface imprinting method, so novel magnetic molecularly imprinted polymers (MMIPs) for quercetagetin were prepared. The MMIPs were applied in the determination and extraction of quercetagein in Calendula officinalis extracts followed by high-performance liquid chromatography.
Co-reporter:Jing Yu, Wei Ha, Jian-nan Sun, and Yan-ping Shi
ACS Applied Materials & Interfaces 2014 Volume 6(Issue 22) pp:19544
Publication Date(Web):November 5, 2014
DOI:10.1021/am505649q
In this work, we developed a simple, novel method for constructing gold nanocomposite supramolecular hybrid hydrogels for drug delivery, in which gold nanocrystals were utilized as building blocks. First, methoxypoly(ethylene glycol) thiol (mPEG-SH, molecular weight (MW) = 5 K) capped gold nanocrystals (nanospheres and nanorods) were prepared via a facile one-step ligand-exchange procedure. Then, the homogeneous supramolecular hybrid hydrogels were formed, after adding α-cyclodextrin (α-CD) into PEG-modified gold nanocrystal solutions, due to the host–guest inclusion. Both gold nanoparticles and inclusion complexes formed between α-CD and PEG chain provided the supra-cross-links, which are beneficial to the gelation formation. The resulting hybrid hydrogels were fully characterized by a combination of techniques including X-ray diffraction, rheology studies, and scanning electron microscopy. Meanwhile, the hybrid hydrogel systems demonstrated unique reversible gel–sol transition properties at a certain temperature caused by the temperature-responsive reversible supramolecular assembly. The drug delivery applications of such hybrid hydrogels were further investigated in which doxorubicin was selected as a model drug for in vitro release, cytotoxicity, and intracellular release studies. We believe that the development of such hybrid hydrogels will provide new and therapeutically useful means for medical applications.Keywords: drug delivery; gold nanoparticles; host−guest inclusion; supramolecular hybrid hydrogel
Co-reporter:Jian-Nan Sun, Juan Chen, Yan-Ping Shi
Journal of Chromatography A 2014 Volume 1352() pp:1-7
Publication Date(Web):25 July 2014
DOI:10.1016/j.chroma.2014.05.037
•Ionic liquid based electromembrane extraction (IL-EME) was first established.•The extraction performance of IL-EME compared with ENB based EME was carried.•The simultaneous extraction for multiple samples was achieved by parallel extraction setup.•The method was applied to the determination of strychnine and brucine in human urine samples.An ionic liquid-based electromembrane extraction (IL-EME) method was presented, and its performance was compared with 2-ethylnitrobenzene (ENB) based EME for the determination of strychnine and brucine in human urine. For the two methods, the fundamental extraction parameters such as supported liquid membrane, voltage, extraction time, pH values of sample solution and acceptor solution, temperature and salting-out effect were separately optimized. IL-EME provided 96- and 122-fold enrichment factors for strychnine and brucine, respectively, which were better than those obtained in EME (83- and 86-fold, respectively). The calibration curves were linear over the ranges of 20–720 μg L−1 for strychnine and 20–640 μg L−1 for brucine with the correlation coefficients higher than 0.9950. The repeatability of EME and IL-EME were evaluated by five parallel experiments giving the relative standard deviations of 5.12–6.98%. As the results indicated, compared with ENB based EME, the proposed IL-EME is more reliable and could provide better extraction performance for the determination of strychnine and brucine in human urine.
Co-reporter:Xin-Yue Song, Wei Ha, Juan Chen, Yan-Ping Shi
Journal of Chromatography A 2014 Volume 1374() pp:23-30
Publication Date(Web):29 December 2014
DOI:10.1016/j.chroma.2014.11.029
•CNTs-β-CD nanocomposite was prepared by modifying the surface of CNTs with β-CD.•Reinforced fibers were obtained by immobilizing the nanocomposite in their wall pores.•The fiber was applied in SPME of plant hormones to study its extraction performance in real samples.•This new extraction fiber had merits of simplicity, high sensitivity, and selectivity.A new, efficient, and environmental friendly solid-phase microextraction (SPME) medium based on β-cyclodextrin (β-CD)-modified carbon nanotubes (CNTs) and a hollow fiber (HF) was prepared. Functionalized β-CD was covalently linked to the surface of the carboxylic CNTs and then the obtained nanocomposite was immobilized into the wall pores of HFs under ultrasonic-assisted effect. The scanning electron microscope was used to inspect surface characteristics of fibers, demonstrating the presence of nanocomposites in their wall pores. The reinforced HF was employed in SPME, and its extraction performance was evaluated by analyzing 1-naphthaleneacetic acid (NAA) and 2-naphthoxyacetic acid (2-NOA) in vegetables. Without any tedious clean-up procedure, analytes were extracted from the sample to the adsorbent and organic solvent immobilized in HFs and then desorbed in acetonitrile prior to chromatographic analysis. Under the optimized extraction conditions, the method provided 275- and 283-fold enrichment factors of NAA and 2-NOA, low limits of detection and quantification (at an ng g−1 level), satisfactory spiked recoveries, good inter-fiber repeatability, and batch-to-batch reproducibility. The selectivity of the developed fiber was investigated to three structurally similar compounds and two reference compounds with recognition coefficients up to 3.18. The obtained results indicate that the newly developed fiber is a feasible, selective, green, and cost-effective microextraction medium and could be successfully applied for extraction and determination of naphthalene-derived plant hormones in complex matrices.
Co-reporter:Jing Yu, Wei Ha, Juan Chen and Yan-ping Shi  
RSC Advances 2014 vol. 4(Issue 103) pp:58982-58989
Publication Date(Web):03 Nov 2014
DOI:10.1039/C4RA11311J
Codelivery of multiple drugs with one kind of drug carrier provides a promising strategy to suppress the drug resistance and achieve the enhanced therapeutic effect in cancer treatment. In this work, we successfully developed multifunctional supramolecular hydrogels based on in situ host–guest inclusion between polymer-drug conjugates and α-cyclodextrin to codeliver hydrophobic and hydrophilic anticancer drugs with pH-trigged release properties. Taking advantage of the strong hydrophobicity of 4β-aminopodophyllotoxin (NPOD), a derivative of podophyllotoxin (POD), the NPOD molecule was conjugated to low-molecular-weight methoxypoly (ethylene glycol) (mPEG) chain via a pH-responsive imine bond, forming an amphiphilic polymer-drug conjugates (NPOD-PEG). After adding α-cyclodextrin (α-CD) into the NPOD-PEG solutions, the stable supramolecular hydrogels were formed based on a combination of the partial inclusion complexation between one end of the mPEG blocks and α-CD and the hydrophobic aggregation of NPOD groups. The formed hydrogels could further efficiently load another hydrophilic anticancer drug doxorubicin (DOX) for combination therapy purposes. The hydrogel demonstrated unique gel–sol transition properties and pH-dependent dual drug release behavior due to the hydrolysis of imine bond at acidic environments. Furthermore, the cytotoxicity results suggested that the DOX loaded NPOD-PEG/α-CD hydrogels showed an enhanced cytotoxicity in cancer cells in comparison with single modality treatment and the resulting hydrogels are characterized by producing an additive cytotoxicity to cancer cells. In fact, the codelivery of two anticancer drugs with different physicochemical properties and anticancer mechanisms was a key to opening the door to their controlled drug delivery and enhanced anticancer effect. Therefore, DOX loaded NPOD-PEG/α-CD hydrogels as pH-trigged drug codelivery systems might have important potential for combination cancer chemotherapy.
Co-reporter:Rui Wang, Ying-Qian Liu, Wei Ha, Yan-Ping Shi, Tsong-Long Hwang, Guan-Jhong Huang, Tian-Shung Wu, Kuo-Hsiung Lee
Bioorganic & Medicinal Chemistry Letters 2014 Volume 24(Issue 16) pp:3944-3947
Publication Date(Web):15 August 2014
DOI:10.1016/j.bmcl.2014.06.039
Oxidative stress imposed by reactive oxygen species plays a crucial role in pathophysiology of inflammatory diseases. In the present study, sesquiterpenoids and diterpenoids isolated from Siegesbeckia pubescens  , a Chinese traditional medicine used to treat arthritis, were evaluated for inhibition of NO production in activated RAW 264.7 macrophages and FMLP/CB induced O2·- generation and elastase release in human neutrophils. In the former assay, sesquiterpenoids were more potent than diterpenoids. The C-4 carbonyl group in the carabrane-type sesquiterpenoid 3 and the C-9 ether linkage in the germacrane sesquiterpene 7 were associated with the enhanced potency. Also, for the active ent  -kaurane type diterpenoids, esterification of 17-OH with isobutyric acid and acetylation of 18-OH affected the inhibition of O2·- generation and elastase release. This report is the first to describe the inhibitory effects on oxidative stress of secondary metabolites from S. pubescens. Its findings suggest that active terpenoids from the herb could be used as lead anti-inflammatory agents.
Co-reporter:Wei Ha, Jing Yu, Rui Wang, Juan Chen and Yan-ping Shi  
Analytical Methods 2014 vol. 6(Issue 15) pp:5720-5726
Publication Date(Web):27 May 2014
DOI:10.1039/C4AY00976B
The colorimetric detection of heavy metal ions based on gold nanoparticles (GNPs) with a functionalized surface layer has received much attention due to their unique size and the dependence of their optical and electronic properties on the degree of aggregation. We developed a simple, environmentally friendly detection technique which uses GNPs functionalized with Xanthoceras sorbifolia tannin (XT) as a colorimetric probe for the selective detection of Cr3+ based on the aggregation-induced color change in the GNPs. In the synthesis of the XT-functionalized GNPs, XT simultaneously acts as a reducing and a stabilizing agent without requiring additional reagents or treatment. The XT-stabilized GNPs obtained are almost spherical, stable and water-soluble. The XT-stabilized GNPs can be used as a high-selectivity template to chelate with Cr3+; this chelation induces the aggregation of the GNPs, resulting in a color change from red to gray/purple within a few seconds. The proposed colorimetric sensor has been successfully applied to the detection of Cr3+ in tap water and river water. Compared with the current materials and methods for Cr3+ detection based on GNPs, this approach opens up a novel and environmentally friendly technique for the efficient detection of Cr3+.
Co-reporter:Rui-Lan Xu, Rui Wang, Wei Ha, Yan-Ping Shi
Phytochemistry Letters 2014 Volume 7() pp:111-113
Publication Date(Web):February 2014
DOI:10.1016/j.phytol.2013.10.010
•Two new cyclohexylethanoids were isolated and elucidated by extensive NMR experiments.•This series cyclohexylethanoids are characteristic of the Clerodendrum genus.•The new cyclohexylethanoids were evaluated for cytotoxicity against the A549 human tumor cell line.A series of cyclohexylethanoids, including two new compounds, 1-hydroxy-1-(8-palmitoyloxyethyl) cyclohexanone (1) and 5-O-butyl cleroindin D (2), together with five known ones, rengyolone (3), cleroindin C (4), cleroindin B (5), rengyol (6) and isorengyol (7), were isolated from the leaves of Clerodendrum trichotomum. Their structures were elucidated on the basis of spectroscopic analyses and by comparison of their NMR data with those in the literatures. Compounds 1 and 2 were evaluated for their cytotoxicity against A549 human tumor cell line.Two new (1–2) and five known (3–7) cyclohexylethanoids were isolated from the leaves of Clerodendrum trichotomum. Cyclohexylethanoids (1–2) were evaluated for their cytotoxicity against A549 human tumor cell line.
Co-reporter:Jian-Nan Sun, Juan Chen, Yan-Ping Shi
Talanta 2014 Volume 125() pp:329-335
Publication Date(Web):1 July 2014
DOI:10.1016/j.talanta.2014.03.013
•Multiple functional ILs [BSO3HMIm][OTf] and [EMIm][BF4] were first used in DLLME.•The acidic compounds were directly extracted from water without pH adjustment.•The whole extraction procedure was green without any consumption of organic solvent.A new mode of ionic liquid based dispersive liquid–liquid microextraction (IL-DLLME) is developed. In this work, [C6MIm][PF6] was chosen as the extraction solvent, and two kinds of hydrophilic ionic liquids, [EMIm][BF4] and [BSO3HMIm][OTf], functioned as the dispersive solvent. So in the whole extraction procedure, no organic solvent was used. With the aid of SO3H group, the acidic compound was extracted from the sample solution without pH adjustment. Two phenolic compounds, namely, 2-naphthol and 4-nitrophenol were chosen as the target analytes. Important parameters affecting the extraction efficiency, such as the type of hydrophilic ionic liquids, the volume ratio of [EMIm][BF4] to [BSO3HMIm][OTf], type and volume of extraction solvent, pH value of sample solution, sonication time, extraction time and centrifugation time were investigated and optimized. Under the optimized extraction conditions, the method exhibited good sensitivity with the limits of detection (LODs) at 5.5 μg L−1and 10.0 μg L−1 for 4-nitrophenol and 2-naphthol, respectively. Good linearity over the concentration ranges of 24–384 μg L−1 for 4-nitrophenol and 28–336 μg L−1 for 2-naphthol was obtained with correlation coefficients of 0.9998 and 0.9961, respectively. The proposed method can directly extract acidic compound from environmental sample or even more complex sample matrix without any pH adjustment procedure.Multiple functional ionic liquids [BSO3HMIm][OTf] and [EMIm][BF4] serving as dispersive solvent were first used in DLLME. With the aid of acidic ionic liquids, the phenolic compounds were directly extracted from environmental water samples without pH adjustment.
Co-reporter:Wei Ha, Jing Yu, Xin-yue Song, Zhi-jun Zhang, Ying-qian Liu and Yan-ping Shi  
Journal of Materials Chemistry A 2013 vol. 1(Issue 41) pp:5532-5538
Publication Date(Web):22 Aug 2013
DOI:10.1039/C3TB20956C
Here we report a multifunctional supramolecular hydrogel based on host–guest inclusion for loading two different anticancer drugs with different controlled release profiles. The resulting hydrogels are characterized by possessing dual phase drug release behavior and producing a dose and cell type dependent synergetic cytotoxicity to cancer cells, which can be used for cancer combination therapy.
Co-reporter:Juan Chen, Ling Jin, Ying-Dong Li and Yan-Ping Shi  
Analytical Methods 2013 vol. 5(Issue 24) pp:7058-7065
Publication Date(Web):15 Oct 2013
DOI:10.1039/C3AY40861B
The newly proposed strategy, namely, holistic analysis of multiple constituents from every constituent herb in a single run, was applied for the quality control of traditional Chinese medicine preparation Wuhu powder. Seven bioactive components, i.e., ferulic acid, hydroxysafflor yellow A, prim-O-glucosylcimifugin, 4′-O-β-D-glucosyl-5-O-methylvisamminol, imperatorin, isoimperatorin, and linoleic acid, from 5 medicinal herbs composing Wuhu powder were selected as evaluation markers, and then their quantitative information was obtained in a single run by an UPLC method coupled with photodiode array detection. Optimum separation was achieved on a C18 column (50 × 2.1 mm i.d., 1.7 μm particle) through a gradient delivery of a mixture of acetonitrile and 0.1% aqueous phosphoric acid at a flow rate of 0.3 mL min−1 at 30 °C. The corresponding maximum absorption wavelengths were selected as the detection wavelengths for each analyte. For all of the analytes, a good linear relationship (r of >0.999) was obtained between peak area and concentration. The method was validated for repeatability, precision, stability, accuracy, and selectivity. The RSD values of retention time and peak area were 0–0.6% and 0.7–1.0% for intra-assay, and 0.1–1.0% and 1.6–1.8% for inter-assay precision. Analysis repeatability and stability (24 h) were all lower than 5.0%. The recovery of the method was 96.1–97.7% with a RSD of 2.4–4.0%. The validated method was applied to quality control of Wuhu powder from different production batches.
Co-reporter:Fang-Fang Chen, Xiao-Yu Xie, Yan-Ping Shi
Journal of Chromatography A 2013 1300() pp: 112-118
Publication Date(Web):
DOI:10.1016/j.chroma.2013.02.018
Co-reporter:Fang-Fang Chen, Xiao-Yu Xie, Yan-Ping Shi
Talanta 2013 Volume 115() pp:482-489
Publication Date(Web):15 October 2013
DOI:10.1016/j.talanta.2013.06.009
•The prepared MMIPs were investigated by TEM, FTIR, XRD and VSM.•The MMIPs were used as a sorbent to recognize PDE-5 inhibitors in herbal medicines.•Good recoveries and low detection limits were obtained.The successfully developed magnetic molecularly imprinted polymers (MMIPs) toward six synthetic phosphodiesterase type-5 (PDE-5) inhibitors were described. Sildenafil was used as template for the preparation of MMIPs using superparamagnetic core–shell nanoparticle as supporter. The obtained MMIPs were characterized using transmission electron microscope, Fourier transform infrared, X-ray diffraction, and vibrating sample magnetometer. High performance liquid chromatography (HPLC) with diode array detector (DAD) was used for the analysis of target analytes. The application of MMIPs as selective sorbent in the cleanup of herbal medicine samples prior to HPLC offered simple sample preparation. The adsorption capacity and selectivity of prepared MMIPs and magnetic non-molecularly imprinted polymers were investigated. The binding isotherms were obtained for sildenafil and fitted by Freundlich isotherm model. Structurally similar compound of sildenafil and a reference compound protocatechuic acid were used for investing the selective recognition of MMIPs.The successfully developed magnetic molecularly imprinted polymer toward eight synthetic PDE-5 inhibitors was described with a superparamagnetic core–shell nanoparticle as the supporter.
Co-reporter:Hong-Fei Zhang, Yan-Ping Shi
Analytica Chimica Acta 2012 Volume 724() pp:54-60
Publication Date(Web):29 April 2012
DOI:10.1016/j.aca.2012.02.039
A magnetic carbon nanomaterial for Fe3O4 enclosure hydroxylated multi-walled carbon nanotubes (Fe3O4-EC-MWCNTs-OH) was prepared by the aggregating effect of Fe3O4 nanoparticle on MWCNTs-OH, and combined with high-performance liquid chromatography (HPLC)/diode array detection (DAD) to determine the aconitines (aconitine, hypaconitine and mesaconitine) in human serum samples. Compared with other extraction modes investigated in experiment, Fe3O4-EC-MWCNTs-OH sorbents showed a good affinity to target analytes. Some important parameters that could influence extraction efficiency of aconitines, including the extraction mode, amounts of Fe3O4-EC-MWCNTs-OH, pH of sample solution, extraction time, desorption solvent and desorption time, were optimized. Under optimal conditions, the recoveries of spiked serum samples were between 98.0% and 103.0%; relative standard deviations (RSDs) ranged from 0.9% to 6.2%. The correlation coefficients varied from 0.9996 to 0.9998. The limits of detection ranged from 3.1 ng mL−1 to 4.1 ng mL−1 at a signal-to-noise ratio of 3. The experimental results showed that the proposed method was feasible for the analysis of aconitines in serum samples.Graphical abstractA magnetic carbon nanomaterial of Fe3O4 enclosure hydroxylated multi-walled carbon nanotubes (Fe3O4-EC-MWCNTs-OH) was prepared by the aggregated effect of Fe3O4 nanoparticles on MWCNTs (multi-walled carbon nanotubes)-OH, and combined with high-performance liquid chromatography-diode array detection to determine the aconitines (aconitine, hypaconitine and mesaconitine) in human serum samples. Compared with other extraction modes investigated in experiment, Fe3O4-EC-MWCNTs-OH sorbents showed a good affinity to target analytes. Some important parameters that could influence extraction efficiency of aconitines, including the extraction mode, amounts of Fe3O4-EC-MWCNTs-OH, pH of sample solution, extraction time, desorption solvent and desorption time, were optimized. Under optimal conditions, the recoveries of spiked serum samples were between 98.0% and 103.0%; relative standard deviations ranged from 0.9% to 6.2%. The correlation coefficients varied from 0.9996 to 0.9998. The limits of detection (LOD) ranged from 3.1 ng mL−1 to 4.1 ng mL−1 at a signal-to-noise ratio of 3. The experimental results showed that the proposed method was feasible for the analysis of aconitines in serum samples.Highlights► The material of Fe3O4-enlosure MWCNTs-OH was prepared with chemical co-precipitation method. ► The material synthesized was used as sorbents to extract aconitines from human serum samples. ► Results exhibited the developed method is feasible for analysis in complex matrix.
Co-reporter:Fang-Fang Chen, Xiao-Yu Xie, Yan-Ping Shi
Journal of Chromatography A 2012 Volume 1252() pp:8-14
Publication Date(Web):24 August 2012
DOI:10.1016/j.chroma.2012.06.071
The magnetic molecularly imprinted polymers (MMIPs) had been synthesized for the selective extraction and clean-up of rhaponticin in Chinese patent medicines (CPM). The MMIPs were prepared via suspension polymerization, using Fe3O4 as magnetically component, rhaponticin as template molecule, acrylamide (AM) as functional monomers, styrene (St) as copolymer monomer and ethylene glycol dimethacrylate (EGDMA) as a cross-linker in dimethyl sulfoxide porogen. The obtained MMIPs were characterized using scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM). High performance liquid chromatography (HPLC) was used for analysis the target analytes. The polymers were evaluated further by batch rebinding experiments. From the derived Freundlich isotherm (FI) equation their binding capacity and binding strength were determined. Structurally similar compound resveratrol and a reference compound kirenol were used for investing the selective recognition capability of MMIPs. The MMIPs were used as sorbents for selective pre-concentration of rhaponticin from CPM samples. The contents of rhaponticin for the four CPM samples were found to be 11.84, 3.35, 4.47, and 7.57 μg g−1, respectively, and the recoveries of spiked samples ranged from 77.82% to 91.00%. The prepared MMIPs could be applied to selectively pre-concentrate and determine rhaponticin in CPM samples.Highlights► The prepared MMIPs were investigated by SEM, FTIR, XRD and VSM. ► The MMIPs were used as a sorbent to determine rhaponticin in CPMs. ► Good recoveries with low detection limit were obtained.
Co-reporter:Hong-Fei Zhang and Yan-Ping Shi  
Analyst 2012 vol. 137(Issue 4) pp:910-916
Publication Date(Web):13 Dec 2011
DOI:10.1039/C1AN15873B
A new solid-phase extraction mode for magnetic retrieval of chitosan combined with high-performance liquid chromatography-diode array detection was proposed for the pre-concentration and determination of flavonoids in green tea beverage samples. In the experiment, chitosan was used as sorbents for the extraction of target analytes; after completion of the extraction process, Fe3O4 nanoparticles acted as carrier to retrieve chitosan from the sample solution. Some important parameters influenced extraction efficiency of flavonoids, including the extraction mode, amounts of chitosan, pH of sample solution, extraction time, salt addition, amounts of Fe3O4 nanoparticles, desorption solvent and desroption time, were optimized. Under the optimum conditions, the recoveries of analytes done on samples spiked with the target analytes were between 96.4% and 108.6%; relative standard deviations ranged from 0.6% to 8.7%. The correlation coefficients varied from 0.9917 to 0.9988. The limits of detection ranged from 5.4 to 16.8 ng mL−1 at a signal-to-noise ratio of 3. All four different brands of green tea beverage samples were successfully analyzed by the proposed method.
Co-reporter:Leilei Liu;Rui Wang;Junli Yang;Yanping Shi
Chinese Journal of Chemistry 2012 Volume 30( Issue 6) pp:1255-1260
Publication Date(Web):
DOI:10.1002/cjoc.201200184

Abstract

Two new germacranes, chrysanthemumins C (1) and D (2), and five eudesmanes, chrysanthemumols I–K (35) as new ones, eudesm-4(14)-ene-3α,11-diol (6) and canusesnol E (7), were isolated from the ethyl acetate soluble fraction of 95% EtOH extract of the flowers of Chrysanthemum indicum. The structures of isolated sesquiterpenoids were elucidated on basis of extensive spectroscopic evidences.

Co-reporter:Juan Chen, Jian-Nan Sun, Xin-Yue Song and Yan-Ping Shi  
Analytical Methods 2012 vol. 4(Issue 9) pp:2989-2995
Publication Date(Web):28 Jun 2012
DOI:10.1039/C2AY25425E
To enable effective quality control of the traditional Chinese medicine (TCM) preparation the Wuji pill, seven bioactive components, i.e. paeoniflorin, jatrorrhizine, coptisine, palmatine, berberine, evodiamine and rutaecarpine, from the three medicinal herbs composing Wuji pills have been selected as evaluation markers. Then an ultra-performance liquid chromatography (UPLC) method coupled with photodiode array (PDA) detection was developed and validated for simultaneous quantification of the 7 mark components in the Wuji pill. Optimum separation was achieved on a C18 column (50 × 2.1 mm i.d., 1.7 μm particle) through a 5.0 min gradient delivery of a mixture of A (acetonitrile) and B (0.1% aqueous phosphoric acid containing 1.38 mmol L−1 sodium dodecyl sulphonate (SDS) and 5% acetonitrile (v/v)) at a flow rate of 0.3 mL min−1 at 25 °C. Because of the different UV characteristics of these components, 3 detection wavelengths were used for quantitative analysis. All of the analytes showed good linearity (r of >0.999). The limit of detection and limit of quantitation for the analytes ranged from 0.005 to 0.15 μg mL−1 and from 0.01 to 0.50 μg mL−1, respectively. The method was validated for repeatability, precision, stability, accuracy, and selectivity. The RSD values of retention time and peak area were 0–0.3% and 0.1–0.9% for intra-assay, and 0.1–1.4% and 1.0–2.6% for inter-assay precision. Analysis repeatability and stability (24 h) were all lower than 2.0%. The recovery of the method was 96.1–97.5% with a RSD of 1.1–2.8%. The validated method was applied to the quality control of Wuji pills from different production batches.
Co-reporter:Hai-Qun Gong;Rui Wang
Helvetica Chimica Acta 2012 Volume 95( Issue 4) pp:618-625
Publication Date(Web):
DOI:10.1002/hlca.201100407

Abstract

Chemical investigation of the aerial part of Leonurus heterophyllus led to the isolation and characterization of the seven labdane-type diterpenoids 17, including six new ones, 16. Compounds 4 and 5 were isolated as a C(15) epimer pair. The determination of the structures and relative configurations of the new compounds were mainly based on 1D- and 2D-NMR spectroscopic methods, and comparison of their NMR data with related compounds. The structure of compound 7 was confirmed by X-ray crystallographic analysis.

Co-reporter:Xiao-Yu Xie, Rui Wang, Yan-Ping Shi
Biochemical Systematics and Ecology 2012 Volume 45() pp:120-123
Publication Date(Web):December 2012
DOI:10.1016/j.bse.2012.07.025
A new sterol (1), five known flavonols (2–6), and four known iridoids (7–10) were isolated from the fruits of Cornus officinalis. The structure of compound 1 was elucidated using various spectroscopic methods. Compounds 3, 5, and 6 were reported for the first time from the species. The chemotaxonomic significance of these compounds was summarized.Highlights► A new sterol, five flavonols and four iridoids were purified from Cornus officinalis. ► Their structures were elucidated on the basis of spectroscopic evidences. ► Chemotaxonomic significance of these compounds were discussed.
Co-reporter:Yang Yang, Juan Chen, Yan-Ping Shi
Talanta 2012 Volume 97() pp:222-228
Publication Date(Web):15 August 2012
DOI:10.1016/j.talanta.2012.04.021
Carbon nanotube-reinforced hollow fiber solid-phase microextraction (CNTs-HF-SPME) combined with high-performance liquid chromatography (HPLC) was used to extract and determine diethylstilbestrol (DES) in milk products. Wall pores of the hollow fiber were filled with multi-walled carbon nanotubes (MWCNTs) using sol–gel technology. In the proposed method, DES was selectively extracted by MWCNTs, desorbed to methanol, and analyzed by HPLC. The parameters affecting the efficiency of CNTs-HFSPME, such as the length of the hollow fiber, extraction and desorption times, extraction temperature, stirring rate, pH of the sample solution, and the amount of organic solvent and salt in the sample solution, were investigated and optimized. Under the optimized extraction conditions, the method showed good linearity (24–960 μg L−1), a low method detection limit (MDL, 5.1 μg L−1), and good recoveries at four different concentrations. It was proven to be simple, rapid, sensitive, and solvent free for the analysis of DES in dairy products.Highlights► Multi-walled carbon nanotubes were filled into the wall pores of hollow fiber using sol–gel technology. ► CNTs-HF was developed and used extract diethylstilbestrol in milk. ► This method was proved to be simple, rapid, economical, and ecological.
Co-reporter:Fang-Fang Chen, Rui Wang, Yan-Ping Shi
Talanta 2012 Volume 89() pp:505-512
Publication Date(Web):30 January 2012
DOI:10.1016/j.talanta.2011.12.080
Molecular imprinted polymers (MIPs) were prepared by thermal polymerization using a non-covalent molecularly imprinting strategy with kirenol as the template, acrylamide (AM) as the functional monomer and ethylene glycol dimethacrylamide (EGDMA) as the cross-linker in the porogen of tetrahydrofuran (THF). The synthesized MIPs were characterized by scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR). Its molecular recognition property was investigated by UV spectrogram. High-pressure liquid chromatography (HPLC) was used for analysis of target analytes. The polymers were evaluated further by batch rebinding experiments, and from the derived isotherms their binding capacity and binding strength were determined. Then the selectivity of the MIPs was checked toward the selected structurally related compounds and the recognition coefficients for kirenol, darutigenol, and ent-2-oxo-15, 16, 19-trihydroxypimar-8(14)-ene (TD) were 2.47, 3.43 and 3.40, respectively. The properties of MIPs for SPE were also evaluated. The results obtained demonstrate that the good imprinting effect and the excellent selectivity of MIPs were obtained. The optimized molecular imprinted SPE procedure was applied to extract kirenol directly from the extracts of the aerial part of Siegesbeckia pubescens herb. A selective extraction of kirenol from traditional Chinese medicine (TCM) was achieved with extraction yield of 80.9%.Highlights► MIPs were prepared and then investigated by SEM, FTIR and UV spectrogram. ► The optimized MISPE procedure was applied to Siegesbeckia pubescens herb. ► The selective extraction yield of kirenol from TCM was achieved at 80.9%.
Co-reporter:Jun-Li Yang, Yan-Ping Shi
Phytochemistry 2012 Volume 76() pp:124-132
Publication Date(Web):April 2012
DOI:10.1016/j.phytochem.2012.01.004
Cycloartane-type triterpenoids (1–3), seven sesquiterpenoids (7–13), and five previously reported secondary metabolites, including three cycloartane-type triterpenoids (4–6) and two sesquiterpenoids (14 and 15), were isolated from the resinous exudates of Commiphora opobalsamum. Their structures were elucidated by extensive spectroscopic analysis, including UV, IR, NMR, and MS, and comparison with literature data. The structures of 1, 3, and 7 were confirmed by single-crystal X-ray diffraction analysis. The absolute configuration of 1 was interpreted by the incorporation of CHCl3 (crystallization solvent) in the crystal and that of 10 was determined by the CD exciton chirality method. Compound 12 represents the first example of a 12-norcadinane-type sesquiterpenoid. Furthermore, compounds 1, 3, 7, and 10–14 were evaluated for cytotoxicity against HeLa and HepG2 cell lines.Graphical abstractTen triterpenoids and sesquiterpenoids were isolated from Commiphora opobalsamum. Structures of 1, 3, and 7 were confirmed by single-crystal X-ray diffraction analysis, and the absolute configurations of 1 and 10 were also determined.Highlights► Ten new triterpenoids and sesquiterpenoids were isolated and identified. ► Three of their structures were confirmed by X-ray diffraction analysis. ► The absolute configurations of two were also determined. ► The cytotoxicity of selected isolates was evaluated.
Co-reporter:Jia Li, Hong-Fei Zhang, Yan-Ping Shi
Food Chemistry 2011 Volume 127(Issue 2) pp:784-790
Publication Date(Web):15 July 2011
DOI:10.1016/j.foodchem.2010.12.148
A fast and sensitive multi-residue analysis method is reported for simultaneous determination of 25 pesticides of chemical classes which are spiked into fresh grape. The sample pretreatment method involves extraction and clean-up in one step with SiO2 hollow fibre from 1.0 mL fresh grape slurry to minimise the matrix effects, and determination by gas chromatography–mass spectrometry with selective ion monitoring mode. The validation of the optimised method in terms of linearity, precision, recovery and repeatability showed that the proposed procedure is sensitive (the limits of detection were in the range of 0.0009–0.0084 μg mL−1 for 25 pesticides), precise and repeatable (average recoveries were between 61% and 108% with relative standard deviations from 4.0% to 12.4 %). The proposed method was also applied to the analysis of these groups of pesticides in fresh grape sample purchased from the local markets of Lanzhou (China), while no residues of the selected pesticides were detected in the sample.Research highlights► A fast and sensitive multi-residue analysis method in grapes is developed. ► SiO2 hollow fiber was applied in analysis of multi-pesticides in grape samples. ► A new pretreatment method involves extraction and clean-up in one step.
Co-reporter:Fang-Fang Chen;Guo-Ying Wang
Journal of Separation Science 2011 Volume 34( Issue 19) pp:2602-2610
Publication Date(Web):
DOI:10.1002/jssc.201100463

Abstract

Molecularly imprinted polymers (MIPs) had been prepared by precipitation polymerization method using acrylamide as the functional monomer, ethylene glycol dimethacrylate as the cross-linker, acetonitrile as the porogen solvent and protocatechuic acid (PA), one of phenolic acids, as the template molecule. The MIPs were characterized by scanning electron microscopy and Fourier transform infrared, and their performance relative to non-imprinted polymers was assessed by equilibrium binding experiments. Six structurally similar phenolic acids, including p-hydroxybenzoic acid, gallic acid, salicylic acid, syringic acid, vanillic acid, ferulic acid were selected to assess the selectivity and recognition capability of the MIPs. The MIPs were applied to extract PA from the traditional Chinese medicines as a solid-phase extraction sorbent. The resultant cartridge showed that the MIPs have a good extraction performance and were able to selectively extract almost 82% of PA from the extract of Rhizoma homalomenae. Thus, the proposed molecularly imprinted-solid phase extraction-high performance liquid chromatography method can be successfully used to extract and analyse PA in traditional Chinese medicines.

Co-reporter:Guo-Ying Wang;Fang-Fang Chen
Journal of Separation Science 2011 Volume 34( Issue 3) pp:268-277
Publication Date(Web):
DOI:10.1002/jssc.201000594

Abstract

A novel ultra-performance LC-photodiode array-eλ-ESI-MS/MS screening method was developed for the detection and identification of natural antioxidants from Radix et Rhizoma Rhei. Nine compounds were found to possess a potential antioxidant activity, and their free radical-scavenging capacities were investigated in detail. The nine compounds were identified as 1-O-galloyl-2-O-cinnamoylglucose, 6-hydroxymusizin-8-O-β-D-glucopyranoside, (+)-catechin, gallic acid 3-O-β-D-glucopyranoside, trans-3,5,4′-trihydroxystilbene-4′-O-β-D-(2″-O-galloyl)-glucopyranoside, sennoside A, 4-(4′-hydroxyphenyl)-2-butanone-4′-O-β-D-(2″-O-galloyl-6″-O-p-coumaroyl) glucopyranoside, emodin-8-O-(6′-O-malonyl) glucopyranoside, and physcion-8-O-β-D-glucopyranoside. The reactivity and SC50 values of those compounds were investigated, respectively. 1-O-Galloyl-2-O-cinnamoylglucose showed the strongest capability for scavenging 1,1-diphenyl-2-picrylhydrazyl-free radical; trans-3,5,4′-trihydroxystilbene-4′-O-β-D-(2″-O-galloyl) glucopyranoside showed the strongest capability for scavenging superoxide radical; 4-(4′-hydroxyphenyl)-2-butanone-4′-O-2-D-(2″-O-galloyl-6″-O-p-coumaroyl) glucopyranoside exhibited the highest reactivity in the lipid peroxidation processes. The use of the analytical screening method based on ultra-performance LC-photodiode array-eλ-ESI-MS/MS would provide a new way for rapid detection of radical-scavenging natural compounds from Radix et Rhizoma Rhei or complex matrices.

Co-reporter:Hai-Qun Gong;Quan-Xiang Wu;Lei-Lei Liu;Jun-Li Yang;Rui Wang
Helvetica Chimica Acta 2011 Volume 94( Issue 7) pp:1269-1276
Publication Date(Web):
DOI:10.1002/hlca.201000417

Abstract

Fourteen sesquiterpenoids with an eudesmane C-atom skeleton, including four new ones, (1β,5α,7β,8β,11β)-5-hydroperoxy-1-hydroxyeudesm-4(15)-eno-12,8-lactone (1), (1β,5α,7β,8β)-8-(acetyloxy)-5-hydroperoxy-1-hydroxycostic acid methyl ester (12), and a mixture of (1β,3β,4β,7β,8β)-1,3-dihydroxyeudesma-5,11(13)-dieno-12,8-lactone (7) and (1β,3β,4β,7β,8β,11β)-1,3-dihydroxyeudesm-5-eno-12,8-lactone (8), were isolated from the aerial parts of Inula japonica (Asteraceae). Their structures were determined by extensive spectroscopic methods, and those of 7 and 12 confirmed by means of single-crystal X-ray diffraction analysis.

Co-reporter:Ya-Min Zhao
Chemistry & Biodiversity 2011 Volume 8( Issue 3) pp:414-430
Publication Date(Web):
DOI:10.1002/cbdv.201000022

Abstract

The plants of genus Dipsacus, with a wide distribution in Europe, Asia, and Africa, have been used as medicinal agents to treat several diseases, including lime disease, fibromyalgia, bone fracture, and abortion, and especially the Alzheimer's disease and cancer. A large number of studies on plants of genus Dipsacus has revealed cytoprotective properties, inhibition of HIV-1 reverse transcriptase, antinociceptive, and antimicrobial effects, etc. This review compiles all chemical constituents isolated, mainly triterpenoids, iridoids, phenolics, and alkaloids, from the genus Dipsacus over the past few decades together with their structural features, biological activities, and structureactivity relationships.

Co-reporter:Jun-Li Yang;Rui Wang
Natural Products and Bioprospecting 2011 Volume 1( Issue 1) pp:1-24
Publication Date(Web):2011 August
DOI:10.1007/s13659-011-0003-y
Ligularia, an important genus of the Compositae family, has captured the interest of natural product chemists for years. Phytochemical investigations on the title genus have led to isolation of hundreds of secondary metabolites with various skeletons. Herein, we summarized the chemical constituents of this genus and their biological activities over the past few decades. Open image in new window
Co-reporter:Wen-Hao Chen, Rui Wang and Yan-Ping Shi
Journal of Natural Products 2010 Volume 73(Issue 8) pp:1398-1403
Publication Date(Web):August 4, 2010
DOI:10.1021/np100339u
Three new flavonoids, oxytropisoflavans A (1) and B (2) and (6aR,11aR)-3,8-dihydroxy-9,10-dimethoxypterocarpan (3), together with 30 known flavonoids (4−33), were isolated from the aerial parts and roots of Oxytropis falcata. The absolute configurations of 3 and C-3 in 1 and 2 were deduced by circular dichroism. The structure of flavonoid 2 was confirmed by single-crystal X-ray diffraction analysis and that of flavonoid 3 by total synthesis of its racemate. Oxytropisoflavan A (1) is an unprecedented chalcan-isoflavan biflavonoid, whereas oxytropisoflavan B (2) possesses a rare modified A-ring. Pterocarpan 3 has good radical-scavenging activity in the 1,1-diphenyl-2-picrylhydrazyl (DPPH) assay.
Co-reporter:Guo-Ying Wang;Huan-Yang Qi
Journal of Separation Science 2010 Volume 33( Issue 12) pp:1730-1738
Publication Date(Web):
DOI:10.1002/jssc.200900861

Abstract

An ultrasonic cell grinder extraction (UCGE) method has been developed and applied to extract five anthraquinones (physcion, chrysophanol, emodin, rhein, and aloe-emodin) from Radix et Rhizoma Rhei. Several parameters of UCGE procedure, including ultrasonic cell grinder running mode, type and volume of extraction solvent and extraction time, were optimized. The determination was preformed on a Waters ultra-performance LC BEH C18 column using gradient elution system. A baseline separation could be achieved in less than 7.5 min with high resolution. Under the optimized conditions, contents of physcion, chrysophanol, emodin, rhein and aloe-emodin in Radix et Rhizoma Rhei collected from different cultivated areas were 0–4.22, 0.11–27.64, 0.09–3.49, 0.31–3.31 and 0.13–2.93 mg/g, respectively. Compared with reflux, maceration and ultrasonic bath extractions, the UCGE method was more efficient, faster and easier to be operated, and required lower extraction temperature and less solvent. The results indicated that UCGE was a novel and ideal method for extracting bioactive constituents from plant samples.

Co-reporter:Jun-Li Yang, Lei-Lei Liu, Bin-Gui Wang, Yan-Ping Shi
Biochemical Systematics and Ecology 2010 Volume 38(Issue 4) pp:850-852
Publication Date(Web):August 2010
DOI:10.1016/j.bse.2010.07.015
Co-reporter:Yang Yang, Juan Chen, Yan-Ping Shi
Journal of Chromatography B 2010 Volume 878(Issue 28) pp:2811-2816
Publication Date(Web):15 October 2010
DOI:10.1016/j.jchromb.2010.08.032
Hollow fiber liquid-phase microextraction (HF-LPME) coupled with high-performance liquid chromatography was used to simultaneously determine three Aconitum alkaloids, including aconitine (AC), hypaconitine (HA) and mesaconitine (MA) in human urine sample. Analytes were extracted from 5 mL urine sample containing 1.0 mmol/L NaOH into 1-octanol membrane phase impregnated in the pores of hollow fiber wall, and then back extracted into acidified aqueous solution in the lumen of the hollow fiber. After extraction, 10 μL of the acceptor phase was analyzed directly by HPLC. In this method, some important extraction parameters, such as organic solvent, extraction time, stirring rate, pH of donor phase and acceptor phase, temperature, and the volume of acceptor phase were optimized. This method provided 98- to 288-fold enrichment factors within 60 min of extraction and good repeatability with RSDs of 0.99–7.22%. The calibration curves were linear over the ranges of 16.0–128.0 μg/L for AC, 11.0–88.0 μg/L for HA and 8.1–64.8 μg/L for MA in human urine sample, with correlation coefficients of 0.9949, 0.9969 and 0.9904, respectively. Limits of detection were from 0.7 to 1.5 μg/L, and recoveries from spiked urine sample varied from 84.4% to 106.2% for AC, 77.3% to 85.6% for HA and 90.1% to 100.8% for MA.
Co-reporter:Hong-Fei Zhang, Yan-Ping Shi
Talanta 2010 Volume 82(Issue 3) pp:1010-1016
Publication Date(Web):15 August 2010
DOI:10.1016/j.talanta.2010.06.008
In this article, a novel method termed as temperature-assisted ionic liquid dispersive liquid–liquid microextraction (TA IL-DLLME) combining high performance liquid chromatography with diode array detection (HPLC-DAD) was developed for the determination of anthraquinones in Radix et Rhizoma Rhei samples. The ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate) was used to replace volatile organic solvent as an extraction solvent for the extraction of anthraquinones (aloe-emodin, rhein, emodin, chrysophanol and physcion) from Radix et Rhizoma Rhei. Several important parameters influencing the extraction efficiency of TA IL-DLLME such as the type and volume of extraction solvent and disperser solvent, sample pH, extraction time, extraction temperature, centrifugation time as well as salting-out effects were optimized. Under the optimal conditions, the spiked recovery for each analyte was in the range of 95.2–108.5%. The precisions of the proposed method were varied from 1.1% to 4.4% (RSD). All the analytes exhibited good linearity with correlation coefficients (r2) ranging from 0.9986 to 0.9996. The limits of detection for all target analytes were ranged from 0.50 to 2.02 μg L−1 (S/N = 3). The experimental results indicated that the proposed method was successfully applied to the analysis of anthraquinones in Radix et Rhizoma Rhei.
Co-reporter:Rui-Lan Xu, Rui Wang, Lan Ding, Yan-Ping Shi
Steroids (July 2013) Volume 78(Issue 7) pp:711-716
Publication Date(Web):1 July 2013
DOI:10.1016/j.steroids.2013.03.002
•Five new steroids were isolated and elucidated by extensive NMR experiments.•Steroidal side chain with two double bonds at C-22 and C-25 are rare in nature.•The steroids were evaluated for cytotoxicity against HeLa cell line.•Steroids 2 and 5 exhibited moderate cytotoxicity.A phytochemical investigation of the leaves of Clerodendrum trichotomum led to the isolation of five new (2–6) and two known (1 and 7) steroids, whose structures and relative configurations were elucidated by comprehensive spectroscopic analysis and by comparison of their NMR data with those of related compounds. Steroids 2 and 5 exhibited moderate cytotoxicity in vitro against HeLa cell line.Five new (2–6) and two known (1 and 7) steroids were isolated from the leaves of Clerodendrum trichotomum. Steroids 2 and 5 exhibited moderate cytotoxicity in vitro against HeLa cell line.Download full-size image
Co-reporter:Dong-Mei Liu, Jun-Li Yang, Wei Ha, Juan Chen, Yan-Ping Shi
Analytical Biochemistry (15 May 2017) Volume 525() pp:
Publication Date(Web):15 May 2017
DOI:10.1016/j.ab.2017.02.020
In the present study, pressure mediated microanalysis (PMMA), a fast, convenient and efficient capillary electrophoresis (CE) method was developed for studying enzyme kinetics of tyrosinase and inhibition kinetics of kojic acid, a model inhibitor of tyrosinase. The enzymatic reaction conditions and CE conditions were optimized in order to obtain high enzyme activity and short analysis time. By PMMA, only the product could be detected at 475 nm, and no voltage was applied to separate the product from the reaction mixture thus greatly simplifying the optimization procedure. The spectrophotometric assay and electrophoretically mediated microanalysis (EMMA) were also performed to validate the developed method. With the present method, the Michaelis-Menten constant (Km) was calculated to be 1.347 mM for tyrosinase. The inhibition constant of kojic acid to free tyrosinase (KI) and kojic acid to tyrosinase/L-DOPA complex (KIS) were calculated to be 36.64 and 74.35 μM, respectively, and the half-maximal inhibitory concentration (IC50) was determined to be 46.64 μM for kojic acid. The developed method is fast and convenient for studying enzyme kinetics, inhibition kinetics and further screening enzyme inhibitors.
Co-reporter:Na Li, Juan Chen, Yan-Ping Shi
Analytica Chimica Acta (1 January 2017) Volume 949() pp:
Publication Date(Web):1 January 2017
DOI:10.1016/j.aca.2016.11.016
•A novel Fe3O4@PEI-RGO was synthesized and applied for the analysis of polar acidic herbicides.•PEI affected the surface property of RGO and changed the polarity of RGO.•Fe3O4@PEI-RGO showed good extraction efficiency towards polar acidic herbicides.•RSM was used to optimize parameters affecting the extraction efficiency.•The absorption mechanism was discussed in detail.A novel magnetic polyethyleneimine modified reduced graphene oxide (Fe3O4@PEI-RGO) had been fabricated based on a self-assemble approach between positive charged magnetic polyethyleneimine (Fe3O4@PEI) and negative charged GO sheets via electrostatic interaction followed by chemical reduction of GO to RGO. The as-prepared Fe3O4@PEI-RGO was characterized by transmission electron microscopy (TEM), Fourier transform infrared spectrometry (FT-IR), X-ray diffraction (XRD), thermal gravimetric analyzer (TGA), vibrating sample magnetometer (VSM) and zeta potential analysis, and then was successfully applied to determine four phenoxy acid herbicides and dicamba in rice coupled with high performance liquid chromatography (HPLC). As a surface modifier of RGO, PEI not only effectually affected the surface property of RGO (e.g. zeta potential), but also changed the polarity of RGO and offered anion exchange groups to polar acidic herbicides, which would directly influence the type of adsorbed analytes. Compared with Fe3O4@PEI, Fe3O4/RGO and Fe3O4@PEI-GO, the as-prepared Fe3O4@PEI-RGO, integrating the superiority of PEI and RGO, showed higher extraction efficiency for polar acidic herbicides. Besides, the adsorption mechanism was investigated as well. It turned out that electrostatic interaction and π-π interaction were considered to be two major driving force for the adsorption process. Response surface methodology (RSM), a multivariate experimental design technique, was used to optimize experimental parameters affecting the extraction efficiency in detail. Under the optimal conditions, a satisfactory performance was obtained. The calibration curves were linear over the concentration ranging from 2 to 300 ng g−1 with correlation coefficients (r) between 0.9985 and 0.9994. The limits of detection (LODs) were in the range of 0.67–2 ng g−1. The recoveries ranged from 87.41% to 102.52% with relative standard deviations (RSDs) less than 8.94%. Taken together, the proposed method was an efficient pretreatment and enrichment procedure and could be successfully applied for selective extraction and determination of polar acidic herbicides in complex matrices.
Co-reporter:Wei Ha ; Jing Yu ; Xin-yue Song ; Juan Chen
ACS Applied Materials & Interfaces () pp:
Publication Date(Web):
DOI:10.1021/am5022864
Taking advantage of the strong hydrophobicity of the anticancer drug camptothecin (CPT), the CPT molecule was conjugated to a class of low-molecular-weight (MW) poly(ethylene glycol) (PEG) chains (MW = 500, 1000, and 2000), forming an amphiphilic prodrug. The CPT-PEG prodrug formed stable hydrogels based on a combination of the partial inclusion complexation between one end of the PEG blocks and α-CD and the hydrophobic aggregation of CPT groups. Meanwhile, the formed hydrogels could be loaded with water-soluble drug 5-fluorouracil (5-FU), which is always combined with CPT drugs to enhance their anticancer activity. Moreover, the hydrogel systems demonstrate unique structure-related reversible gel–sol transition properties at a certain temperature due to the reversible supramolecular assembly, and the gel–sol transition temperature could be modulated by varying the length of the PEG chain and the concentrations of α-CD, demonstrating the possibility of achieving on-demand gel–sol transitions. The structure-related reversible gel–sol transition properties were proved by rheological property, XRD, DSC, and SEM measurements. The different controlled release profiles of two different anticancer drugs showed significant temperature-dependent properties. This easily prepared supramolecular hydrogel with excellent biocompatibility and tunable temperature responsiveness has significant potential for controlled drug release applications.
Co-reporter:
Analytical Methods (2009-Present) 2015 - vol. 7(Issue 16) pp:NaN6820-6820
Publication Date(Web):2015/07/10
DOI:10.1039/C5AY01093D
An efficient, accurate and reliable chromatographic fingerprint based on ultra-performance liquid chromatography coupled with photodiode array detection and electrospray ionization mass spectrometry (UPLC-PDA-ESI-MS) was developed for the identification and quality control of Oxytropis falcate Bunge. The method was validated for precision, repeatability, stability, and specificity. The RSD values of retention times and peak areas of the common peaks were 0–0.7% and 1.0–3.6% for within-day precision, while 0–0.5% and 1.5–6.1% for between-day precision. For repeatability, the values were lower than 0.5% and 2.6%, respectively, and for stability (24 h), the values were lower than 0.9% and 3.3%, respectively. Twenty-one batches of O. falcate obtained from different regions were analyzed by employing the developed method. Several multivariate statistical analysis including similarity analysis (SA), hierarchical clustering analysis (HCA) and principal component analysis (PCA) were applied to cluster and evaluate the O. falcate samples according to their collection sites. The results showed that the quality of O. falcate did not merely depend on the geographic origin. Thirty common peaks were found in the chromatographic fingerprints of O. falcate and eleven of them were identified by comparing the retention time, the ultraviolet spectrum and the molecular ion peaks (obtained from selective ion recording mode) with the reference compounds. This method with high precision, reliable stability and good repeatability can provide a reference for the quality evaluation of O. falcate.
Co-reporter:
Analytical Methods (2009-Present) 2013 - vol. 5(Issue 24) pp:
Publication Date(Web):
DOI:10.1039/C3AY40861B
The newly proposed strategy, namely, holistic analysis of multiple constituents from every constituent herb in a single run, was applied for the quality control of traditional Chinese medicine preparation Wuhu powder. Seven bioactive components, i.e., ferulic acid, hydroxysafflor yellow A, prim-O-glucosylcimifugin, 4′-O-β-D-glucosyl-5-O-methylvisamminol, imperatorin, isoimperatorin, and linoleic acid, from 5 medicinal herbs composing Wuhu powder were selected as evaluation markers, and then their quantitative information was obtained in a single run by an UPLC method coupled with photodiode array detection. Optimum separation was achieved on a C18 column (50 × 2.1 mm i.d., 1.7 μm particle) through a gradient delivery of a mixture of acetonitrile and 0.1% aqueous phosphoric acid at a flow rate of 0.3 mL min−1 at 30 °C. The corresponding maximum absorption wavelengths were selected as the detection wavelengths for each analyte. For all of the analytes, a good linear relationship (r of >0.999) was obtained between peak area and concentration. The method was validated for repeatability, precision, stability, accuracy, and selectivity. The RSD values of retention time and peak area were 0–0.6% and 0.7–1.0% for intra-assay, and 0.1–1.0% and 1.6–1.8% for inter-assay precision. Analysis repeatability and stability (24 h) were all lower than 5.0%. The recovery of the method was 96.1–97.7% with a RSD of 2.4–4.0%. The validated method was applied to quality control of Wuhu powder from different production batches.
Co-reporter:Juan Chen, Jian-Nan Sun, Xin-Yue Song and Yan-Ping Shi
Analytical Methods (2009-Present) 2012 - vol. 4(Issue 9) pp:NaN2995-2995
Publication Date(Web):2012/06/28
DOI:10.1039/C2AY25425E
To enable effective quality control of the traditional Chinese medicine (TCM) preparation the Wuji pill, seven bioactive components, i.e. paeoniflorin, jatrorrhizine, coptisine, palmatine, berberine, evodiamine and rutaecarpine, from the three medicinal herbs composing Wuji pills have been selected as evaluation markers. Then an ultra-performance liquid chromatography (UPLC) method coupled with photodiode array (PDA) detection was developed and validated for simultaneous quantification of the 7 mark components in the Wuji pill. Optimum separation was achieved on a C18 column (50 × 2.1 mm i.d., 1.7 μm particle) through a 5.0 min gradient delivery of a mixture of A (acetonitrile) and B (0.1% aqueous phosphoric acid containing 1.38 mmol L−1 sodium dodecyl sulphonate (SDS) and 5% acetonitrile (v/v)) at a flow rate of 0.3 mL min−1 at 25 °C. Because of the different UV characteristics of these components, 3 detection wavelengths were used for quantitative analysis. All of the analytes showed good linearity (r of >0.999). The limit of detection and limit of quantitation for the analytes ranged from 0.005 to 0.15 μg mL−1 and from 0.01 to 0.50 μg mL−1, respectively. The method was validated for repeatability, precision, stability, accuracy, and selectivity. The RSD values of retention time and peak area were 0–0.3% and 0.1–0.9% for intra-assay, and 0.1–1.4% and 1.0–2.6% for inter-assay precision. Analysis repeatability and stability (24 h) were all lower than 2.0%. The recovery of the method was 96.1–97.5% with a RSD of 1.1–2.8%. The validated method was applied to the quality control of Wuji pills from different production batches.
Co-reporter:Wei Ha, Xiao-Bo Zhao, Kan Jiang, Yang Kang, Juan Chen, Bang-Jing Li and Yan-Ping Shi
Chemical Communications 2016 - vol. 52(Issue 100) pp:NaN14387-14387
Publication Date(Web):2016/11/21
DOI:10.1039/C6CC08123A
A three dimensional supramolecular hydrogel consisting of prodrug-modified graphene oxide and α-cyclodextrin was developed. This hydrogel with a well-ordered interior microstructure integrated hydrophobic and hydrophilic anticancer drugs into a single multifunctional platform, and underwent a gel–sol transition leading to cascade release of two drugs in an on-demand fashion upon NIR light irradiation.
Co-reporter:Wei Ha, Jing Yu, Xin-yue Song, Zhi-jun Zhang, Ying-qian Liu and Yan-ping Shi
Journal of Materials Chemistry A 2013 - vol. 1(Issue 41) pp:NaN5538-5538
Publication Date(Web):2013/08/22
DOI:10.1039/C3TB20956C
Here we report a multifunctional supramolecular hydrogel based on host–guest inclusion for loading two different anticancer drugs with different controlled release profiles. The resulting hydrogels are characterized by possessing dual phase drug release behavior and producing a dose and cell type dependent synergetic cytotoxicity to cancer cells, which can be used for cancer combination therapy.
Co-reporter:Run-Tian Ma, Wei Ha, Juan Chen and Yan-Ping Shi
Journal of Materials Chemistry A 2016 - vol. 4(Issue 15) pp:NaN2627-2627
Publication Date(Web):2016/03/17
DOI:10.1039/C6TB00409A
Antibody-free analysis is a potential method for glycoprotein analysis, but the development of this method has been limited by its unfavorable selectivity in recent years. Magnetic molecular imprinting, which integrates the fast separation of magnetic materials with high selectivity towards templates in molecular imprinting, was expected to be an effective sample pretreatment in antibody-free analysis for glycoproteins. However, the aggregation of magnetic imprinted nanoparticles and thick molecularly imprinted polymer (MIP) shells on the surface of magnetic carriers caused an unfavorable adsorption capacity, and unsatisfactory rebinding and elution rates, and has limited its application in glycoprotein extraction. Thus, highly dispersed magnetic molecularly imprinted nanoparticles (MMINs) with a well-defined thin film for the selective extraction of glycoprotein HRP were developed in this work. A solvothermal method was used in this work to improve the dispersity of Fe3O4 NPs (nanoparticles) and the MMINs. The thickness of the MIP film was optimized to provide the optimum extraction efficiency. Thus the adsorption capacity of the MMINs, the rebinding rate and the elution rate of the templates were greatly improved. As a result, the prepared MMINs not only exhibited excellent selectivity and high adsorption capacity to HRP, and an outstanding tolerance for interference, but also showed excellent rebinding and elution rates for extraction application. Furthermore, this method provided a reliable way to improve conventional magnetic molecular imprinting, and showed great potential for the analysis of glycoprotein tumor biomarkers in clinics in the future.
Co-reporter:
Analytical Methods (2009-Present) 2014 - vol. 6(Issue 15) pp:
Publication Date(Web):
DOI:10.1039/C4AY00976B
The colorimetric detection of heavy metal ions based on gold nanoparticles (GNPs) with a functionalized surface layer has received much attention due to their unique size and the dependence of their optical and electronic properties on the degree of aggregation. We developed a simple, environmentally friendly detection technique which uses GNPs functionalized with Xanthoceras sorbifolia tannin (XT) as a colorimetric probe for the selective detection of Cr3+ based on the aggregation-induced color change in the GNPs. In the synthesis of the XT-functionalized GNPs, XT simultaneously acts as a reducing and a stabilizing agent without requiring additional reagents or treatment. The XT-stabilized GNPs obtained are almost spherical, stable and water-soluble. The XT-stabilized GNPs can be used as a high-selectivity template to chelate with Cr3+; this chelation induces the aggregation of the GNPs, resulting in a color change from red to gray/purple within a few seconds. The proposed colorimetric sensor has been successfully applied to the detection of Cr3+ in tap water and river water. Compared with the current materials and methods for Cr3+ detection based on GNPs, this approach opens up a novel and environmentally friendly technique for the efficient detection of Cr3+.
4(15),11(12),10(14)-germacratriene-1beta,3beta,9alpha-triol
4(15),11(12),10(14)-germacratriene-1alpha,3beta,9beta-triol
Propanoic acid, 2-methyl-, [(3S,4S,5S,5aS,6R,7S,9S,9aS,10R)-6,7-bis(acetyloxy)-5-(benzoyloxy)octahydro-9,10-dihydroxy-2,2,9-trimethyl-4-(2-methyl-
2(3H)-Naphthalenone,4,4a,5,6,7,8-hexahydro-4-hydroxy-1,4a-dimethyl-7-(1-methylethenyl)-,(4R,4aR,7R)-
8beta-angeloylmaximilianin
Isothymusin
Forsythin
1beta-6, 8-Cyclo-4(14)-eudesmen-1-ol
2',4',5,7-tetrahydroxy-5',6-dimethoxyflavone
(7S)-7-isopropyl-4,10-dimethylenecyclodec-5-enol