Co-reporter:Jinhui Jiang, Yonghua Hu, Zhenfeng Tian, Kaibo Chen, Shaolin Ge, Yingbo Xu, Dong Tian, Jun Yang
Carbohydrate Polymers 2016 Volume 135() pp:121-127
Publication Date(Web):1 January 2016
DOI:10.1016/j.carbpol.2015.08.084
•A rapid method was developed to quantify cellulose content in tobacco using 13C CP/MAS NMR with spectral deconvolution.•A designed NMR rotor was used to eliminate the unfavorable impact of the instability and high-speed rotation for internal standard.•Spectral deconvolution technique eliminated the interference of overlapping peaks and excessive noise.•The method showed good agreement and small average deviations between standard chemical method and values by 13C CP/MAS NMR spectra.A method was developed for rapid quantitative determination of cellulose in tobacco by utilizing 13C cross polarization magic angle spinning NMR spectroscopy (13C CP/MAS NMR). Sample powder was loaded into NMR rotor, which was customized rotor containing a matched silicon tube as an intensity reference. 13C CP/MAS NMR spectra of tobacco samples were processed with spectral deconvolution to obtain the area of the C-1 resonance at 105.5 ppm and the internal standard at 0 ppm. The ratio between the area of 105.5 ppm and 0 ppm of a set of standard cellulose samples was used to construct a calibration curve. The cellulose content of a tobacco sample was determined by comparison of the ratio between the area of 105.5 ppm and 0 ppm to the calibration curve. Results of this developed method showed good agreement with those obtained from chemical analysis. The proposed method has such advantages of accuracy, quickness and efficiency, and could be an alternative to chemical analyses of cellulose.
Co-reporter:Le-Chen Chen, Shan Lei, Mo-Zhen Wang, Jun Yang, Xue-Wu Ge
Chinese Chemical Letters 2016 Volume 27(Issue 4) pp:511-517
Publication Date(Web):April 2016
DOI:10.1016/j.cclet.2016.01.057
Macroporous polystyrene microsphere/graphene oxide (PS/GO) composite monolith was first prepared using Pickering emulsion droplets as the soft template. The Pickering emulsion was stabilized by PS/GO composite particles in-situ formed in an acidic water phase. With the evaporation of water and the oil phase (octane), the Pickering emulsion droplets agglomerated and combined with each other, forming a three-dimensional macroporous PS/GO composite matrix with excellent mechanical strength. The size of the macrospores ranged from 4 μm to 20 μm. The macroporous PS/GO composite monolith exhibited high adsorption capacity for tetracycline (TC) in an aqueous solution at pH 4–6. The maximum adsorption capacity reached 197.9 mg g−1 at pH 6. The adsorption behaviour of TC fitted well with the Langmuir model and pseudo-second-order kinetic model. This work offers a simple and efficient approach to fabricate macroporous GO-based monolith with high strength and adsorption ability for organic pollutants.A macroporous polystyrene/graphene oxide composite monolith with high adsorption capability for tetracycline was fabricated via the aggregation of Pickering emulsion droplets stabilized by the PS/GO composite particles.
Co-reporter:Jinxing Chen, Shan Lei, Yunyun Xie, Mozhen Wang, Jun Yang, and Xuewu Ge
ACS Applied Materials & Interfaces 2015 Volume 7(Issue 51) pp:28606
Publication Date(Web):December 7, 2015
DOI:10.1021/acsami.5b10126
The preparation of efficient and practical biomacromolecules imprinted polymer materials is still a challenging task because of the spatial hindrance caused by the large size of template and target molecules in the imprinting and recognition process. Herein, we provided a novel pathway to coat a NIR-light responsive lysozyme-imprinted polydopamine (PDA) layer on a fibrous SiO2 (F-SiO2) microsphere grown up from a magnetic Fe3O4 core nanoparticle. The magnetic core–shell structured lysozyme-imprinted Fe3O4@F-SiO2@PDA microspheres (MIP-lysozyme) can be easily separated by a magnet and have a high saturation adsorption capacity of lysozyme of 700 mg/g within 30 min because of the high surface area of 570 m2/g and the mesopore size of 12 nm of the Fe3O4@F-SiO2 support. The MIP-lysozyme microspheres also show an excellent selective adsorption of lysozyme (IF > 4). The binding thermodynamic parameters studied by ITC proves that the lysozyme should be restricted by the well-defined 3D structure of MIP-lysozyme microspheres. The MIP-lysozyme can extract lysozyme efficiently from real egg white. Owing to the efficient NIR light photothermal effect of PDA layer, the MIP-lysozyme microspheres show the controlled release property triggered by NIR laser. The released lysozyme molecules still maintain good bioactivity, which can efficiently decompose E. coli. Therefore, this work provides a novel strategy to build practical NIR-light-responsive MIPs for the extraction and application of biomacromolecules.Keywords: controlled release; Fe3O4 nanoparticles; fibrous SiO2; lysozyme; NIR-light; polydopamine; protein imprinting
Co-reporter:Li Yao, Jun Yang, Baizhan Liu, Saijing Zheng, Weimiao Wang, Xiaolan Zhu and Xiaobo Qian
Analytical Methods 2014 vol. 6(Issue 16) pp:6488-6493
Publication Date(Web):17 Jun 2014
DOI:10.1039/C4AY00867G
Analysis of the urinary metabolite of benzo[a]pyrene (BaP), 3-hydroxybenzo[a]pyrene (3-OHBaP), is useful for the biomonitoring of carcinogenic polycyclic aromatic hydrocarbons (PAHs) exposure. The determination of 3-OHBaP by liquid chromatography tandem mass spectrometry (LC-MS/MS) suffers from the poor sensitivity of detection in commonly used electrospray ionization (ESI) sources. In this study, a sensitive and selective LC-MS/MS method was developed for the determination of urinary 3-OHBaP. Following enzymatic hydrolysis of the glucuronide and sulfate conjugates, the metabolite was enriched and cleaned up by solid-phase extraction and then derivatized with dansyl chloride. The derivative was analyzed by LC-MS/MS with ESI in the positive ion mode. The derivatization of 3-OHBaP by the introduction of a dansyl group into the molecule greatly enhanced the detection sensitivity by improving both the efficiency of ESI in the positive ion mode and collision-induced dissociation in the collision cell. Good linearity was obtained in the range of 0.25–40.0 pg mL−1 with a correlation coefficient (r2) of 0.9924. The limit of detection (LOD) and lower limit of quantification (LLOQ) were 0.1 pg mL−1 and 0.25 pg mL−1, respectively. Accuracy ranged from 87.7% to 107.5%. Intra- and inter-day relative standard deviations varied from 4.6% to 8.4% and 7.2% to 10.6%, respectively. Finally, this developed method was successfully applied for the analysis of urine samples from smokers and non-smokers to measure human exposure to PAHs.
Co-reporter:Bo You, Lili Wang, Li Yao and Jun Yang
Chemical Communications 2013 vol. 49(Issue 44) pp:5016-5018
Publication Date(Web):17 Apr 2013
DOI:10.1039/C3CC41949E
3D N-doped graphene–CNT networks (NGCs) can be obtained by hydrothermal treatment, freeze-drying and subsequent carbonization of graphene oxide-dispersed pristine CNTs in the presence of pyrrole. The resulting NCGs used as a supercapacitor show high specific capacitance, good rate capability and still retain ∼96% of the initial capacitance even after 3000 cycles.
Co-reporter:Li Yao, Saijing Zheng, Yafeng Guan, Jun Yang, Baizhan Liu, Weimiao Wang, Xiaolan Zhu
Analytica Chimica Acta 2013 Volume 788() pp:61-67
Publication Date(Web):25 July 2013
DOI:10.1016/j.aca.2013.06.034
•No need to treat with glucuronidase or base to analyze NNAL-N-Gluc and NNAL-O-Gluc.•Good separation was achieved on a Phenomenex Kinetex PFP column within 6 min.•Streamlined extraction procedure was developed for purification.•Sensitive detection was performed by LC–MS/MS.Determination of the tobacco-specific nitrosamine metabolite 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) and its N- and O-glucuronides (NNAL-N-Gluc and NNAL-O-Gluc) is important for toxicology analysis of tobacco smoke induced carcinogenicity and the understanding of detoxification mechanisms of the carcinogenic nitrosamine in humans. But previously reported indirect measurement methods involving enzymolysis and base treatment steps were tedious and time-consuming. In this work, a direct measurement method for simultaneous determination of urinary NNAL, NNAL-N-Gluc and NNAL-O-Gluc by liquid chromatography–tandem mass spectrometry (LC–MS/MS) in a single run was developed for the first time without the need to perform enzymatic or base hydrolysis. Urine samples were purified using dichloromethane and further extracted by solid-phase extraction. Then they were analyzed by LC–MS/MS operated in electrospray positive ionization mode. Chromatographic separation was achieved on a Phenomenex Kinetex PFP column within 6 min. The proposed method was validated and the results demonstrated that the method can produce satisfactory recoveries and reproducibility for the analytes. The applicability of this newly developed method was investigated for the simultaneous analysis of the three metabolites in smokers’ urine and the obtained results were comparable to those detected using the conventional enzymolysis method.A simple method for the simultaneous separation and determination of 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol and its N- and O-glucuronides in human urine by liquid chromatography–tandem mass spectrometry on a pentafluorophenyl column was developed.
Co-reporter:Hongying Zhu;Yonggang Feng;Wenjie Pan;Zhanghai Li;Yonggao Tu;Xiaolan Zhu;Guangming Huang
Journal of Separation Science 2013 Volume 36( Issue 15) pp:2486-2495
Publication Date(Web):
DOI:10.1002/jssc.201300294
Sucrose esters (SEs) were successfully extracted from Oriental tobacco leaves using a new methodology based on accelerated solvent extraction followed by hydrophilic–lipophilic balanced cartridge cleanup step. The SEs were detected by HPLC with ion-trap MS detection using an electrospray interface operated in the positive ion mode. This methodology combines the high efficiency of extraction provided by a pressurized fluid and the highly sensitive characterization offered by ion-trap MS. Under the optimized conditions, 14 SEs were first identified among a total of 23 SEs found in Oriental tobacco leaves. Under the same conditions, only four new SEs were extracted by using traditional ultrasound-assisted extraction and liquid–solid extraction methods. The present method might be potentially useful in high-efficiency extraction and sensitive characterization of SEs from complex matrices such as tobacco leaves.
Co-reporter:Dr. Bo You;Na Li;Hongying Zhu;Xiaolan Zhu ; Jun Yang
ChemSusChem 2013 Volume 6( Issue 3) pp:474-480
Publication Date(Web):
DOI:10.1002/cssc.201200709
Abstract
A MnO2–CNT–graphene oxide (MCGO) nanocomposite is fabricated using graphene oxide (GO) as a surfactant to directly disperse pristine carbon nanotubes (CNTs) for the subsequent deposition of MnO2 nanorods. The resulting MCGO nanocomposite is used as a supercapacitor electrode that shows ideal capacitive behavior (i.e., rectangular-shaped cyclic voltammograms), large specific capacitance (4.7 times higher than that of free MnO2) even at high mass loading (3.0 mg cm−2), high energy density (30.4–14.2 Wh kg−1), large power density (2.6–50.5 kW kg−1), and still retains approximately 94 % of the initial specific capacitance after 1000 cycles. The advanced capacity, rate capability, and cycling stability may be attributed to the unique architecture, excellent ion wettability of GO with enriched oxygen-containing functional groups, high conductivity of CNTs, and their synergistic effects when combined with the other components. The results suggest that the MnO2–CNT–GO hybrid nanocomposite architecture is very promising for next generation high-performance energy storage devices.
Co-reporter:Bo You, Zhidan Zhang, Lili Zhang, Jun Yang, Xiaolan Zhu and Qingde Su
RSC Advances 2012 vol. 2(Issue 12) pp:5071-5074
Publication Date(Web):03 May 2012
DOI:10.1039/C2RA01243J
A new effect of aging time (AT) on the shrinkage of ordered mesoporous carbon (OMC) prepared by an evaporation-induced triconstituent co-assembly method has been reported. Increasing AT from 0.5 to 2.0 h can gradually reduce framework shrinkage of the OMC during carbonization. This novel effect is effective and simple for preparing the OMC with large mesopore sizes, high pore volumes and surface area.
Co-reporter:Panpan Li, Xiaolan Zhu, Shenqiu Hong, Zhenfeng Tian and Jun Yang
Analytical Methods 2012 vol. 4(Issue 4) pp:995-1000
Publication Date(Web):13 Mar 2012
DOI:10.1039/C2AY05866A
A new ultrasound-assisted extraction (UAE) followed by dispersive liquid–liquid microextraction (DLLME) method has been developed for the simultaneous determination of flavoring compounds, including safrole, coumarin, 6-methylcoumarin, 7-metheoxycoumarin, estragole, methyleugenol, pulegone and thujone, in tobacco additives. In this method, the targets were extracted from tobacco additive sample using ethanol by UAE. Then, 0.5 mL of the extract were used for the DLLME. In the DLLME, the target analytes in the extraction solvent were rapidly extracted into a small volume of chloroform and analyzed by chromatography-mass spectrometry (GC-MS). The parameters affecting the DLLME, including type and volume of extraction and disperser solvents, salt effect and extraction time, were investigated and optimized. Under the optimum conditions, the enrichment factors (EFs) ranged from 140 to 208. The linear relationship was obtained in the range of 0.4–928 ng mL−1, which showed satisfactory linearity with correlation coefficients (r2) over 0.9989 for all the analytes. The limits of detection (LOD) were between 0.04 and 0.24 ng mL−1 and the average recoveries were between 89.9 and 99.7% with relative standard deviations (RSDs) ranging from 2.5 to 6.7% in all cases. The method was successfully applied to the preconcentration and determination of these target compounds in tobacco additives.
Co-reporter:Bo You, Jun Yang, Yingqiang Sun and Qingde Su
Chemical Communications 2011 vol. 47(Issue 45) pp:12364-12366
Publication Date(Web):20 Oct 2011
DOI:10.1039/C1CC15348J
Hollow core, mesoporous shell carbon nanospheres (HCMSs) with large bimodal mesopores (6.4 and 3.1 nm) and high surface area (1704 m2 g−1) have been synthesized by a triconstituent surface co-assembly of monodisperse silica nanospheres method. The resulted HCMS show a high specific capacity of 251 F g−1 at 50 mV s−1 in 2 M H2SO4 and long cyclic life.
Co-reporter:Yaping Zhang;Ronghua Shi;Qingde Su;Li Yao ;Panpan Li
Journal of Separation Science 2011 Volume 34( Issue 14) pp:1675-1682
Publication Date(Web):
DOI:10.1002/jssc.201100058
Abstract
A method was developed to determine eight acetanilide herbicides from cereal crops based on accelerated solvent extraction (ASE) and solid-phase extraction (SPE) followed by gas chromatography-electron capture detector (GC-ECD) analysis. During the ASE process, the effect of four parameters (temperature, static time, static cycles and solvent) on the extraction efficiency was considered and compared with shake-flask extraction method. After extraction with ASE, four SPE tubes (graphitic carbon black/primary secondary amine (GCB/PSA), GCB, Florisil and alumina-N) were assayed for comparison to obtain the best clean-up efficiency. The results show that GCB/PSA cartridge gave the best recoveries and cleanest chromatograms. The analytical process was validated by the analysis of spiked blank samples. Performance characteristics such as linearity, limit of detection (LOD), limit of quantitation (LOQ), precision and recovery were studied. At 0.05 mg/kg spiked level, recoveries and precision values for rice, wheat and maize were 82.3–115.8 and 1.1–13.6%, respectively. For all the herbicides, LOD and LOQ ranged from 0.8 to 1.7 μg/kg and from 2.4 to 5.3 μg/kg, respectively. The proposed analytical methodology was applied for the analysis of the targets in samples; only three herbicides, propyzamid, metolachlor and diflufenican, were detected in two samples.
Co-reporter:Bo You, Lili Wang, Li Yao and Jun Yang
Chemical Communications 2013 - vol. 49(Issue 44) pp:NaN5018-5018
Publication Date(Web):2013/04/17
DOI:10.1039/C3CC41949E
3D N-doped graphene–CNT networks (NGCs) can be obtained by hydrothermal treatment, freeze-drying and subsequent carbonization of graphene oxide-dispersed pristine CNTs in the presence of pyrrole. The resulting NCGs used as a supercapacitor show high specific capacitance, good rate capability and still retain ∼96% of the initial capacitance even after 3000 cycles.
Co-reporter:Bo You, Jun Yang, Yingqiang Sun and Qingde Su
Chemical Communications 2011 - vol. 47(Issue 45) pp:NaN12366-12366
Publication Date(Web):2011/10/20
DOI:10.1039/C1CC15348J
Hollow core, mesoporous shell carbon nanospheres (HCMSs) with large bimodal mesopores (6.4 and 3.1 nm) and high surface area (1704 m2 g−1) have been synthesized by a triconstituent surface co-assembly of monodisperse silica nanospheres method. The resulted HCMS show a high specific capacity of 251 F g−1 at 50 mV s−1 in 2 M H2SO4 and long cyclic life.
Co-reporter:
Analytical Methods (2009-Present) 2014 - vol. 6(Issue 16) pp:
Publication Date(Web):
DOI:10.1039/C4AY00867G
Analysis of the urinary metabolite of benzo[a]pyrene (BaP), 3-hydroxybenzo[a]pyrene (3-OHBaP), is useful for the biomonitoring of carcinogenic polycyclic aromatic hydrocarbons (PAHs) exposure. The determination of 3-OHBaP by liquid chromatography tandem mass spectrometry (LC-MS/MS) suffers from the poor sensitivity of detection in commonly used electrospray ionization (ESI) sources. In this study, a sensitive and selective LC-MS/MS method was developed for the determination of urinary 3-OHBaP. Following enzymatic hydrolysis of the glucuronide and sulfate conjugates, the metabolite was enriched and cleaned up by solid-phase extraction and then derivatized with dansyl chloride. The derivative was analyzed by LC-MS/MS with ESI in the positive ion mode. The derivatization of 3-OHBaP by the introduction of a dansyl group into the molecule greatly enhanced the detection sensitivity by improving both the efficiency of ESI in the positive ion mode and collision-induced dissociation in the collision cell. Good linearity was obtained in the range of 0.25–40.0 pg mL−1 with a correlation coefficient (r2) of 0.9924. The limit of detection (LOD) and lower limit of quantification (LLOQ) were 0.1 pg mL−1 and 0.25 pg mL−1, respectively. Accuracy ranged from 87.7% to 107.5%. Intra- and inter-day relative standard deviations varied from 4.6% to 8.4% and 7.2% to 10.6%, respectively. Finally, this developed method was successfully applied for the analysis of urine samples from smokers and non-smokers to measure human exposure to PAHs.
Co-reporter:
Analytical Methods (2009-Present) 2012 - vol. 4(Issue 4) pp:
Publication Date(Web):
DOI:10.1039/C2AY05866A
A new ultrasound-assisted extraction (UAE) followed by dispersive liquid–liquid microextraction (DLLME) method has been developed for the simultaneous determination of flavoring compounds, including safrole, coumarin, 6-methylcoumarin, 7-metheoxycoumarin, estragole, methyleugenol, pulegone and thujone, in tobacco additives. In this method, the targets were extracted from tobacco additive sample using ethanol by UAE. Then, 0.5 mL of the extract were used for the DLLME. In the DLLME, the target analytes in the extraction solvent were rapidly extracted into a small volume of chloroform and analyzed by chromatography-mass spectrometry (GC-MS). The parameters affecting the DLLME, including type and volume of extraction and disperser solvents, salt effect and extraction time, were investigated and optimized. Under the optimum conditions, the enrichment factors (EFs) ranged from 140 to 208. The linear relationship was obtained in the range of 0.4–928 ng mL−1, which showed satisfactory linearity with correlation coefficients (r2) over 0.9989 for all the analytes. The limits of detection (LOD) were between 0.04 and 0.24 ng mL−1 and the average recoveries were between 89.9 and 99.7% with relative standard deviations (RSDs) ranging from 2.5 to 6.7% in all cases. The method was successfully applied to the preconcentration and determination of these target compounds in tobacco additives.