Co-reporter:Da-Song Yang, Xi-Ying Ding, Hong-Ping Min, Bo Li, Meng-Xiang Su, Miao-Miao Niu, Bin Di, Fang Yan
Journal of Chromatography A 2017 Volume 1505(Volume 1505) pp:
Publication Date(Web):7 July 2017
DOI:10.1016/j.chroma.2017.05.025
•A novel IMAC and MOAC hybrid material was synthesized for enlarging phosphopeptide enrichment coverage.•This material showed excellent enrichment sensitivity and capability towards phosphopeptides.•The designed hybrid material enriched more phosphopeptides than single IMAC or MOAC strategy from complex sample.•This work opens up a strategy which combined various methods in one material for effective enrich phosphopeptide.Reversible phosphorylation of proteins is one of the most important post-translational modifications, while the detection of phosphopeptides is difficult due to their low abundance and the signal suppression of nonphosphorylated peptides. Therefore, selective enrichment of phosphopeptides from highly complicated mixtures is vital for MS-based phosphoproteome analysis. Despite various strategies have been developed, there is no single method that is capable of providing full coverage of the whole phosphoproteome. Metal oxide affinity chromatography (MOAC) enrichment preferably singly phosphopeptides, whereas immobilized metal affinity chromatography (IMAC) enrichment bias towards multiply phosphopeptides. In this study, first example of IMAC and MOAC hybrid material, Fe3O4@nSiO2@mSiO2/TiO2-Ti4+ nanoparticles were successfully synthesized for the enrichment of phosphopeptides with the aim to combining their advantages for enrich both mono- and multi-phosphorylated species. The TiO2 was firstly coated on the surface of mesoporous silica and then grafted with 3-(trihydroxysilyl)propyl methylphosphonate (THPMP) to chelate Ti4+ ions. This novel type of hybird material with high surface areas (179.3 m2/g) exhibited good adsorption capacity (133 mg/g) towards standard tryptic digest of β-casein and the method based on this material also showed good sensitivity (4 pmol). The synthesized Fe3O4@nSiO2@mSiO2/TiO2-Ti4+ microspheres were further used to selectively enrich phosphopeptides from complex biosamples, seven mono-phosphopeptides and eight multi-phosphopeptides were successfully enriched from nonfat milk which is much better than single IMAC or MOAC strategy. Those results indicated that Fe3O4@nSiO2@mSiO2/TiO2-Ti4+ microspheres have potential applications in MS-based phosphoproteomics to enlarge phosphoproteomics coverage and this work was expected to open up a promising strategy which combined the advantages of various methods in one material for effective enrich phosphorylated peptides.
Co-reporter:Fang Yan, Zhong-Ying Liu, Jin-Long Chen, Xiao-Yan Sun, Xiao-Juan Li, Meng-Xiang Su, Bo Li and Bin Di
RSC Advances 2014 vol. 4(Issue 62) pp:33047-33054
Publication Date(Web):14 Jul 2014
DOI:10.1039/C4RA05293E
In this work, we firstly explored zeolitic imidazolate framework-8 (ZIF-8) as a novel adsorbent for selective adsorption of theophylline (TPE) over its structure-related analogs involving caffeine (CFE) and diprophylline (DPE) in aqueous solution in view of sole and mixed adsorption, desorption, and solid phase extraction. The adsorption kinetics of TPE on ZIF-8 obeyed pseudo-second-order kinetics. Analysis of the intraparticle diffusion plots revealed that more than one process affected the adsorption, and film (boundary layer) diffusion controlled the adsorption rate at the beginning. The adsorption isotherms of TPE on ZIF-8 followed the Freundlich model, and enthalpy rather than entropy controlled its adsorption. Evidence from FT-IR and X-ray photoelectron spectroscopic data showed that the adsorption of TPE was also driven by coordination of unsaturated zinc species in ZIF-8 with the carbonyl groups in TPE besides π–π interaction and molecular size. All these interactions made the ZIF-8 a promising candidate for the selective adsorption and extraction of structure-related analogs.
Co-reporter:Xiao Yan, Jin-Long Chen, Meng-Xiang Su, Fang Yan, Bo Li and Bin Di
RSC Advances 2014 vol. 4(Issue 43) pp:22318-22323
Publication Date(Web):11 Apr 2014
DOI:10.1039/C4RA02592J
While most research has focused on the development of carbon dot (CD) based fluorescence sensors, much less attention has been paid to the phosphorescence phenomenon and its potential applications to date. Herein, room temperature phosphorescence (RTP) of water soluble CDs free of deoxidants and other inducers was observed for the first time in pure aqueous solution. RTP of CDs could be significantly quenched when chelating with iron ions as well as aggregation of CDs, presumably resulting from the formation of non-luminescent chelate. Due to a high affinity of iron ions to phosphate ions through well-known Fe–O–P bonds, the quenched RTP of functionalized CDs by Fe3+ could be basically recovered in the presence of phosphate-containing molecules. For a proof-of-concept demonstration, adenosine-5′-triphosphate (ATP), as a common phosphate-containing metabolite was quantitatively detected by a phosphorescence “off-to-on” approach. The enhancement of RTP at 440 nm was linearly proportional to the concentrations of ATP ranging from 20 to 200 μM with a detection limit as low as 14 μM. Moreover, the iron ion engineered CDs based RTP probe was used to estimate ATP levels in human blood plasma.
Co-reporter:Meng-xiang Su, Zhong-ying Liu, Jin-long Chen, Li-fei Cheng, Bo Li, Fang Yan and Bin Di
RSC Advances 2014 vol. 4(Issue 98) pp:54998-55002
Publication Date(Web):20 Oct 2014
DOI:10.1039/C4RA11302K
L-Phenylalanine imprinting chiral ordered mesoporous silica (L-Phe-COMS) was facilely synthesized in the presence of phenylalanine amino acid by combining tetraethyl orthosilicate and quaternized aminosilane silica sources. The obtained COMS was comparable with a MCM-41-type structure, with narrow pore size distribution, and high specific surface area characterized by powder X-ray diffraction and N2 adsorption experiments. The imprinting chirality of COMS was disclosed by mixed and separate L- and D-phenylalanine adsorption on the L-Phe-COMS with a stereoselective adsorption capacity of up to 3.24. In addition, six racemic mixtures including amino acids and drugs were explored to test the stereoselective adsorption capacity of L-Phe-COMS. The imprinting chiral ordered mesoporous silica presents the advantages of straightforward synthesis approach and robust stereoselective adsorption capacity, making it a promising candidate for chiral adsorption and separation.
Co-reporter:Dian-Yun Qu, Jin-Long Chen and Bin Di
Analytical Methods 2014 vol. 6(Issue 13) pp:4705-4709
Publication Date(Web):28 Apr 2014
DOI:10.1039/C4AY00533C
A new fluorescent probe capable of reliable detection of hydrazine under environmentally friendly conditions with high specificity and sensitivity was developed. 3,6-Diacetoxyfluoran (FDA), a readily commercially available compound, is explored for fluorescence “switch-on” detection of hydrazine in this work. FDA can undergo hydrazinolysis and transform into fluorescein in aqueous solution at neutral pH, resulting in distinct optical changes from colorless to green and “switch-on” fluorescence which allows for establishing a new method for sensitive detection of hydrazine. Under optimum conditions described in this work, the enhancement of fluorescence at 515 nm was linearly proportional to the concentrations of hydrazine ranging from 1.25 to 25.00 μM with a correlation coefficient of R2 = 0.9959 and a detection limit as low as 31 nM. The relative standard deviation of twelve replicate measurement samples was 5.4% for 12.5 μM hydrazine. The proposed method is convenient, low cost and free of complex equipment, making it possible to successfully determine hydrazine in four real samples containing distilled water, tap water, isoniazid and plasma. Furthermore, the hydrazine probe would be a promising candidate capable of naked-eye visualization of gaseous hydrazine by simple operations.
Co-reporter:Xiabing Wu, Linjun You, Bin Di, Weiqiang Hao, Mengxiang Su, Yu Gu, Lingling Shen
Journal of Chromatography A 2013 Volume 1299() pp:78-84
Publication Date(Web):19 July 2013
DOI:10.1016/j.chroma.2013.05.051
•Novel chiral core–shell silica spheres were synthesized and characterized.•The core–shell silica spheres were tested as chiral stationary phases (CSPs).•Rapid separations of several racemic binaphthyl derivatives were achieved.•Core–shell silica and periodic mesoporous organosilicas as CSPs were compared.Novel chiral core–shell silica microspheres with trans-(1R,2R)-diaminocyclohexane (DACH) moiety bridged in the mesoporous shell were synthesized using layer-by-layer method. The chiral mesoporous shell around the nonporous silica core was formed by the co-condensation of N,N′-bis-[(triethoxysilyl)propyl]-trans-(1R,2R)-bis-(ureido)-cyclohexane (DACH-BS) and tetraethoxysilane (TEOS) using octadecyltrimethylammonium chloride (C18TMACl) and triblock poly(ethylene oxide)-b-poly(propylene oxide)-b-poly(ethylene oxide) copolymer (P123) as the templates. The functionalized core–shell silica microspheres were characterized and tested as chiral stationary phases for high performance liquid chromatography (HPLC). R/S-1,1′-bi-2,2′-naphthol, R/S-6,6′-dibromo-1,1′-bi-2-naphthol and R/S-1,1′-bi-2,2′-phenanthrol were enantioseparated rapidly on the column packed with the DACH core–shell silica particles. Moreover, the column packed with core–shell particles exhibited better performance than the column packed with the DACH functionalized periodic mesoporous organosilicas.
Co-reporter:Bin Di, Lifei Cheng, Qiuling Jiang, Mengxiang Su and Weiqiang Hao
New Journal of Chemistry 2013 vol. 37(Issue 5) pp:1603-1609
Publication Date(Web):20 Mar 2013
DOI:10.1039/C3NJ00219E
Monodispersed chiral mesoporous spheres of nanometer size with high specific area and good thermal stability were synthesized using the chiral anionic surfactant (N-palmitoyl-L-phenylalanine) as a template according to the co-structure directing agent (CSDA) method. The resulting mesoporous nanospheres were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), small angle X-ray powder diffraction (XRD) and nitrogen sorption experiments. The particle distribution was 190–210 nm with pore diameters of 3–4 nm. The enantioselective ability of this chiral mesoporous silica, after extraction of the chiral surfactant, was investigated by the selective adsorption of enantiomers and racemic solutions of alanine. The chiral selective adsorbability of this material type was shown by the asymmetric preferential adsorption of alanine as observed using circular dichroism (CD) spectroscopy and was further verified in a racemic mixture of valine. It was found that the adsorption of L-alanine was higher than that of D-alanine on as-prepared chiral mesoporous materials with a chiral selectivity factor of 3.15, which generates new possibilities for enantiomeric separation and other enantioselective applications.
Co-reporter:Linjun You;Jie Qian;Xiabing Wu;Xiaoyang Sun;Mengxiang Su;Yingxiang Du;Baiyang Mao
Journal of Pharmaceutical Sciences 2013 Volume 102( Issue 7) pp:2371-2379
Publication Date(Web):
DOI:10.1002/jps.23557
Abstract
The ocular pharmacokinetic (PK) of azithromycin in rabbit eye tissues was evaluated following single-dose and multiple-dose administrations of azithromycin. Because of destructive sampling, only the average ocular tissue concentration–time curve could be captured and used to estimate the PK parameters failing to obtain their standard deviations. In the present study, formulas were explained in details to estimate the major PK parameter errors in destructive sampling. The PK parameters were obtained by analyzing average ocular tissue concentration–time curve and their standard deviations were calculated using the formula proposed in this paper. A case study was included to elucidate the potential application of the formulas. F-test for equality of variances and independent-samples t-test were carried out between test formulation and reference formulation in PK parameters. Thus, a new and simple method was proposed to compare PK behavior for these studies using destructive sampling, which can be potentially applied into other cases in the future. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 102:2371–2379, 2013
Co-reporter:Linjun You, Yu Gu, Lingling Shen, Xiabing Wu, Mengxiang Su, Weiqiang Hao, Bin Di, Yingxiang Du
Materials Letters 2013 Volume 113() pp:107-110
Publication Date(Web):15 December 2013
DOI:10.1016/j.matlet.2013.09.062
•New material with core–shell structure was synthesized and used as stationary phase.•New material combines the advantages of core–shell structure and PMOs.•New material showed high column efficiency and fast separation.•Rapid separation of aromatic compounds was achieved.Micrometer-size periodic mesoporous organosilicas (PMOs) with a uniform spherical core–shell structure were prepared, and their application as a stationary phase for chromatographic separation was demonstrated in this study. The structure and morphology of this new material was characterized by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and nitrogen sorption measurements. The results showed that the materials exhibited a spherical morphology, core–shell structure and mesostructure. This new material was tested as a potential stationary phase for HPLC because of its combination of a core–shell structure and PMOs. The new material showed high column efficiency for fast separation of aromatic hydrocarbon compounds.
Co-reporter:Li Li, Haiyan Ding, Bin Di, Weilin Li and Jian Chen
Analyst 2012 vol. 137(Issue 23) pp:5632-5638
Publication Date(Web):26 Sep 2012
DOI:10.1039/C2AN35523J
Here we present a validated rapid detection system for propofol, an anaesthetic with a narrow therapeutic window, in whole blood. This method utilises an on-line molecularly imprinted polymer solid-phase extraction, rather than the traditional C18 solid-phase extraction, coupled to fluorescence optical fibre detection. The linearity was assessed from 0.10–15 μg mL−1 of propofol in whole blood, and the coefficients were greater than 0.995. The absolute recoveries of propofol were 95.81, 97.56 and 97.93% at three different concentrations. The inter-batch precision ranged from 4.3% to 8.1%, and the accuracy value ranged from 102.5% to 104.4%. The developed method was successfully applied to measure propofol concentrations in simulated whole blood samples. The entire analysis procedure lasted only 5 minutes, and the results showed no statistical difference between the new on-line method and a validated high-performance liquid chromatography method. The new on-line method, however, is faster and more convenient for the clinical real-time detection of propofol than previously reported methods.
Co-reporter:Ruixue Ran;Linjun You;Weiqiang Hao;Mengxiang Su;Fang Yan;Lili Huang
Journal of Separation Science 2012 Volume 35( Issue 15) pp:1854-1862
Publication Date(Web):
DOI:10.1002/jssc.201200047
Mesoporous organosilicas with both R-(+)-1,1′-binaphthyl-2,2′-diamine and ethane moieties bridging in the framework were synthesized. This mesoporous material was prepared via the one-step co-condensation of N,N′-bis-[(triethoxysilyl)propyl]-(R)-bis-(ureido)-binaphthyl (Si-DABN) with 1,2-bis(triethoxysilyl)ethane (BTSE) using octadecyltrimethylammonium chloride (C18TMACl) as a structural directing agent with the aid of a co-solvent (ethanol) in basic medium. The morphology of these bifunctionalized mesoporous organosilicas is sensitive to the Si-DABN mole fraction and the base concentration. And the mesostructure becomes less ordered as the mole fraction of Si-DABN in the initial mixture increases from 10 to 40%. Elemental analysis and Fourier transform infrared (FT-IR) spectrometer indicate that the binaphthyl diamine was successfully introduced to the mesoporous organosilicas. Acidic conditions are more suitable than basic ones for the hydrolysis and condensation of (R)-2,2′-dicyanomethoxy-6,6′-di[(2-triethoxysilyl)ethenyl]-1,1′-binaphthyl, a chiral silane precursors with a short silane side chain on the binaphthyl group. A column packed with these bifunctionalized mesoporous organosilica spheres exhibits greater selectivity for R/S-1,1′-bi-2,2′-naphthol than one packed with commercial SiO2 grafted with N,N′-bis-[(triethoxysilyl)propyl]-(R)-bis-(ureido)–binaphthyl. Binaphthol and bromosubstituted binaphthol were fully resolved, but two ether derivatives were only partially enantioseparated and the other three ester derivatives were no fully resolved on the column via co-condensation method.
Co-reporter:Lili Huang;Juan Lu;Fang Feng;Mengxiang Su;Fang Yan
Journal of Separation Science 2011 Volume 34( Issue 18) pp:2523-2527
Publication Date(Web):
DOI:10.1002/jssc.201100103
Abstract
Monodisperse spherical periodic mesoporous organosilicas (PMOs) with ethane integrated in the framework were synthesized and their application as stationary phase for chromatographic separation is demonstrated. The ethane-PMOs were prepared by condensation of 1,2-bis(triethoxysilyl)ethane (BTSE) in basic condition using octadecyltrimethylammonium chloride (C18TMACl) as template and ethanol as co-solvent. The morphology and mesoporous structure of ethane-PMOs were controlled under different concentrations of sodium hydroxide (NaOH) and EtOH. The results of scanning electron microscopy (SEM), transmission electron microscopy (TEM), powder X-ray diffraction (XRD), nitrogen sorption measurement, Fourier transform infrared spectroscopy (FT-IR) and elemental analysis showed that ethane-PMOs have spherical morphology, uniform particle distribution, highly ordered pore structure, high surface area and narrow pore-size distribution. The column packed with these materials exhibits good permeability, high chemical stability and good selectivity of mixtures of aromatic hydrocarbons in normal phase high-performance liquid chromatography (HPLC).
Co-reporter:Meng-xiang Su;Min-hong Liu
European Journal of Drug Metabolism and Pharmacokinetics 2011 Volume 36( Issue 4) pp:223-228
Publication Date(Web):2011 December
DOI:10.1007/s13318-011-0064-7
The pharmacokinetic behaviors of the epimers of cefotetan disodium (R-CTT, S-CTT) after a single intravenous injection dose in healthy Chinese volunteers were explored in this study. In an open-label, randomized, three-way, cross-over study, 12 volunteers (6 females and 6 males) received a cross-over fashion doses of 0.5, 1.0, and 2.0 g of cefotetan disodium, separated by washout periods of 7 days. The plasma concentrations of both epimers were measured by validated high-performance liquid chromatography assays. Pharmacokinetic parameters of R-CTT, S-CTT, and total-CTT (R + S mixture) were calculated using a noncompartmental analysis. Generally, the R and S epimers showed different pharmacokinetic behaviors. Following 0.5, 1.0, and 2.0 g doses of cefotetan disodium, values of the total area under the plasma concentration–time curve (AUC0–∞) were 124.23 ± 19.54, 231.34 ± 39.34, and 459.09 ± 80.65 for R-CTT; 100.95 ± 14.19, 193.80 ± 30.42, and 372.66 ± 67.32 for S-CTT, respectively. Total body clearance values were 4.13, 4.43, and 4.46 L/h for R-CTT and 5.05, 5.28, and 5.50 L/h for S-CTT, respectively. Mean plasma elimination half-life (t1/2) values of R-CTT were 4.16, 4.13, and 4.01 h for 0.5, 1.0, and 2.0 g doses, respectively, and those of S-CTT were 3.15, 3.25, and 3.21 h. There were significant differences in t1/2 between the two epimers (P < 0.05). The t1/2 of R-CTT was 28% longer than that of S-CTT, which indicated that the elimination of the S-CTT was greater than that of the R-CTT. All treatments were well tolerated.
Co-reporter:Meng-xiang Su;Lin-jun You;Lan-jin Qu;Tai-jun Hang
Chromatographia 2011 Volume 74( Issue 9-10) pp:
Publication Date(Web):2011 November
DOI:10.1007/s10337-011-2131-2
A simple and sensitive liquid chromatography with ultraviolet detection (LC–UV) method was developed for the determination of three impurities with a content over 0.1% (w/w) in technical triadimefon. A Gemini C18 column (5 μm, 250 mm × 4.6 mm i.d.) was used for the chromatographic separations. The samples were separated by gradient elution with water (solvent A) and methanol (solvent B) using the following conditions: 70% A isocratic for 12 min, linear to 0% A within 8 min, and isocratic for 10 min at 0% A with a flow rate of 1.0 mL min−1. Chromatograms were recorded at an absorption wavelength of 280 nm. The chromatographic resolutions between triadimefon and its potential impurities A, B, and C were greater than 3. The developed LC method was validated with respect to linearity, accuracy, precision, and robustness. This method was successfully applied to analyze the impurities in commercial technical triadimefon. In addition, the structures of the three impurities were identified to be (A) 4-chlorophenol, (B) 1-(2,4-dichlorophenoxy)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)-2-butanone, and (C) 1,1-bis(4-chlorophenoxy)-3,3-dimethyl-2-butanone.
Co-reporter:Hua-qing Liu, Meng-xiang Su, Bin Di, Tai-jun Hang, Ying Hu, Xiao-qin Tian, Yin-di Zhang, Jian-ping Shen
Journal of Chromatography B 2008 Volume 873(Issue 1) pp:20-26
Publication Date(Web):15 September 2008
DOI:10.1016/j.jchromb.2008.07.045
A sensitive, rapid liquid chromatographic–electrospray ionization mass spectrometric method for the determination of xanthinol in human plasma was developed and validated. Xanthinol nicotinate in plasma (0.5 mL) was pretreated with 20% trichloroacetic acid for protein precipitation. The samples were separated using a Lichrospher silica (5 μm, 250 mm × 4.6 mm i.d.). A mobile phase of methanol–water containing 0.1% formic acid (50: 50, v/v) was used isocratically eluting at a flow rate of 1 mL/min. Xanthinol and its internal standard (IS), acyclovir, were measured by electrospray ion source in positive selected reaction monitoring mode. The method demonstrated that good linearity ranged from 10.27 to 1642.8 ng/mL with r = 0.9956. The limit of quantification for xanthinol in plasma was 10.27 ng/mL with good accuracy and precision. The mean plasma extraction recovery of xanthinol was in the range of 90.9–100.2%. The intra- and inter-batch variability values were less than 4.8% and 7.9% (relative standard deviation, R.S.D.), respectively. The established method has been successfully applied to a bioequivalence study of two xanthinol nicotinate tablets for 20 healthy volunteers.
Co-reporter:Linjun You, Jie Qian, Xiabing Wu, Xiaoyang Sun, ... Baiyang Mao
Journal of Pharmaceutical Sciences (July 2013) Volume 102(Issue 7) pp:2371-2379
Publication Date(Web):1 July 2013
DOI:10.1002/jps.23557
The ocular pharmacokinetic (PK) of azithromycin in rabbit eye tissues was evaluated following single-dose and multiple-dose administrations of azithromycin. Because of destructive sampling, only the average ocular tissue concentration–time curve could be captured and used to estimate the PK parameters failing to obtain their standard deviations. In the present study, formulas were explained in details to estimate the major PK parameter errors in destructive sampling. The PK parameters were obtained by analyzing average ocular tissue concentration–time curve and their standard deviations were calculated using the formula proposed in this paper. A case study was included to elucidate the potential application of the formulas. F-test for equality of variances and independent-samples t-test were carried out between test formulation and reference formulation in PK parameters. Thus, a new and simple method was proposed to compare PK behavior for these studies using destructive sampling, which can be potentially applied into other cases in the future. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 102:2371–2379, 2013
Co-reporter:Xiao-Fei Gu, Yue Zhao, Kan Li, Meng-Xiang Su, Fang Yan, Bo Li, Ying-Xiang Du, Bin Di
Journal of Chromatography A (25 November 2016) Volume 1474() pp:
Publication Date(Web):25 November 2016
DOI:10.1016/j.chroma.2016.10.072
•Effective platform for differentiation of volatile aromatic isomers.•Reliable strategy for structural elucidation of volatile compounds in mixtures.•Direct X-ray crystallographic analysis of volatile and even oily compounds.•Only microgram amounts of sample was required.•Unambiguous identification of samples was realized without reference standards.Structure elucidation of volatile aromatic isomers at trace level has long been considered as an elusive task, due to their structural similarities and similar polarities, even with the aid of many spectroscopic techniques such as mass spectrometry and nuclear magnetic resonance (NMR) spectroscopy. Single-crystal X-ray diffraction (SCD) is recognized as one of the most powerful structural elucidation techniques. The recently developed crystalline sponge method overcomes the intrinsic limitation of SCD that the target molecules must be single crystals, being able to analyze non-crystalline and trace-amount compounds without any special treatment. In order to investigate whether the crystalline sponge method could be used for the structure elucidation of closely related isomers or other volatile and even oily compounds in complex mixtures at trace level, we combined HPLC separation with the crystalline sponge method for X-ray crystallographic analysis. In this paper, two pairs of volatile aromatic isomers including cis/trans isomers of asarone and positional isomers of carvacrol and thymol, as well as the main volatile component in essential oil extracted from Acorus Tatarinowii, were first isolated by HPLC and encapsulated into the crystalline sponge then elucidated by X-ray crystallographic analysis. Direct observation of these volatile compounds by X-ray crystallography was achieved using only microgram quantities without crystallization or derivatization. Unambiguous identification of these compounds was realized without reference standards. This strategy offers a promising platform capable of providing high-confidence detailed structural information of closely related isomers as well as other volatile and even oily compounds in complex mixtures in microgram quantities.
Co-reporter:Xiao-Fei Gu, Yue Zhao, Kan Li, Meng-Xiang Su, Fang Yan, Bo Li, Ying-Xiang Du, Bin Di
Journal of Chromatography A (25 November 2016) Volume 1474() pp:130-137
Publication Date(Web):25 November 2016
DOI:10.1016/j.chroma.2016.10.072
•Effective platform for differentiation of volatile aromatic isomers.•Reliable strategy for structural elucidation of volatile compounds in mixtures.•Direct X-ray crystallographic analysis of volatile and even oily compounds.•Only microgram amounts of sample was required.•Unambiguous identification of samples was realized without reference standards.Structure elucidation of volatile aromatic isomers at trace level has long been considered as an elusive task, due to their structural similarities and similar polarities, even with the aid of many spectroscopic techniques such as mass spectrometry and nuclear magnetic resonance (NMR) spectroscopy. Single-crystal X-ray diffraction (SCD) is recognized as one of the most powerful structural elucidation techniques. The recently developed crystalline sponge method overcomes the intrinsic limitation of SCD that the target molecules must be single crystals, being able to analyze non-crystalline and trace-amount compounds without any special treatment. In order to investigate whether the crystalline sponge method could be used for the structure elucidation of closely related isomers or other volatile and even oily compounds in complex mixtures at trace level, we combined HPLC separation with the crystalline sponge method for X-ray crystallographic analysis. In this paper, two pairs of volatile aromatic isomers including cis/trans isomers of asarone and positional isomers of carvacrol and thymol, as well as the main volatile component in essential oil extracted from Acorus Tatarinowii, were first isolated by HPLC and encapsulated into the crystalline sponge then elucidated by X-ray crystallographic analysis. Direct observation of these volatile compounds by X-ray crystallography was achieved using only microgram quantities without crystallization or derivatization. Unambiguous identification of these compounds was realized without reference standards. This strategy offers a promising platform capable of providing high-confidence detailed structural information of closely related isomers as well as other volatile and even oily compounds in complex mixtures in microgram quantities.
Co-reporter:
Analytical Methods (2009-Present) 2014 - vol. 6(Issue 13) pp:
Publication Date(Web):
DOI:10.1039/C4AY00533C
A new fluorescent probe capable of reliable detection of hydrazine under environmentally friendly conditions with high specificity and sensitivity was developed. 3,6-Diacetoxyfluoran (FDA), a readily commercially available compound, is explored for fluorescence “switch-on” detection of hydrazine in this work. FDA can undergo hydrazinolysis and transform into fluorescein in aqueous solution at neutral pH, resulting in distinct optical changes from colorless to green and “switch-on” fluorescence which allows for establishing a new method for sensitive detection of hydrazine. Under optimum conditions described in this work, the enhancement of fluorescence at 515 nm was linearly proportional to the concentrations of hydrazine ranging from 1.25 to 25.00 μM with a correlation coefficient of R2 = 0.9959 and a detection limit as low as 31 nM. The relative standard deviation of twelve replicate measurement samples was 5.4% for 12.5 μM hydrazine. The proposed method is convenient, low cost and free of complex equipment, making it possible to successfully determine hydrazine in four real samples containing distilled water, tap water, isoniazid and plasma. Furthermore, the hydrazine probe would be a promising candidate capable of naked-eye visualization of gaseous hydrazine by simple operations.
![1-(3-TRIETHOXYSILYLPROPYL)-3-[(1R,2R)-2-(3-TRIETHOXYSILYLPROPYLCARBAMOYLAMINO)CYCLOHEXYL]UREA](http://img.cochemist.com/ccimg/331900/331850-56-7.png)
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![[1,1'-Biphenanthrene]-2,2'-diol](http://img.cochemist.com/ccimg/196900/196865-17-5_b.png)
![Bisoxireno[4b,5:8a,9]phenanthro[1,2-c]furan-4(2H)-one,1b,3,6,6b,7,7a,9,10,11,11a-decahydro-9,10,11-trihydroxy-1b-methyl-10-(1-methylethyl)-,(1aS,1bS,6bS,7aS,8aS,9R,10S,11S,11aS)- (9CI)](http://img.cochemist.com/ccimg/147900/147852-78-6.png)
![Bisoxireno[4b,5:8a,9]phenanthro[1,2-c]furan-4(2H)-one,1b,3,6,6b,7,7a,9,10,11,11a-decahydro-9,10,11-trihydroxy-1b-methyl-10-(1-methylethyl)-,(1aS,1bS,6bS,7aS,8aS,9R,10S,11S,11aS)- (9CI)](http://img.cochemist.com/ccimg/147900/147852-78-6_b.png)
![Glycine,N-[2-[(acetyloxy)methoxy]-2-oxoethyl]-N-[2-[2-[2-[bis(carboxymethyl)amino]phenoxy]ethoxy]phenyl]-](http://img.cochemist.com/ccimg/139900/139890-68-9.png)
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![(2s,4s)-1-[(2s)-3-benzoylsulfanyl-2-methylpropanoyl]-4-phenylsulfanylpyrrolidine-2-carboxylic Acid](http://img.cochemist.com/ccimg/81900/81872-10-8.png)
![(2s,4s)-1-[(2s)-3-benzoylsulfanyl-2-methylpropanoyl]-4-phenylsulfanylpyrrolidine-2-carboxylic Acid](http://img.cochemist.com/ccimg/81900/81872-10-8_b.png)
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![3-Furancarboxylic acid,(8R,9R,10R,11S,12R,13R,14R,15S,21S,22S,23R)-10,13,22,23-tetrakis(acetyloxy)-12-[(acetyloxy)methyl]-7,8,9,10,12,13,14,15,17,18,19,20-dodecahydro-18,21-dihydroxy-8,18,21-trimethyl-5,17-dioxo-8,11-epoxy-9,12-ethano-11,15-methano-5H,11H-[1,9]dioxacyclooctadecino[4,3-b]pyridin-14-ylester](http://img.cochemist.com/ccimg/37300/37239-48-8.png)
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![8,11-Epoxy-9,12-ethano-11,15-methano-5H,11H-[1,9]dioxacyclooctadecino[4,3-b]pyridine-5,17(18H)-dione,10,13,22,23-tetrakis(acetyloxy)-12-[(acetyloxy)methyl]-14-(benzoyloxy)-7,8,9,10,12,13,14,15,19,20-decahydro-21-hydroxy-8,18,21-trimethyl-,(8R,9R,10R,11S,12S,13R,14R,15S,18S,21S,22S,23R)-](http://img.cochemist.com/ccimg/11100/11088-09-8_b.png)
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![Dinaphtho[2,1-d:1',2'-f][1,3]dioxepin](http://img.cochemist.com/ccimg/200/188-35-2_b.png)
