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Chinese Chemical Letters 2010年第6期21卷 -页

作者： Tsuneaki Maeda Analytical Chemistry Division National Institute of Advanced Industrial Science and TechnologyTsukuba Central 51-1-1 HigashiTsukubaIbaraki 305-8565Japan

Triacontyl modified silica gel as a sorbent coupled with gas chromatography-mass spectrometry(GC-MS) was developed to determine EPA prior 16 polycyclic aromatic hydrocarbons(PAHs) in water *** parameters of solid-phase extraction such as organic modifier solvent,eluent,sample flow rate and volume were *** developed method was found to yield a linear calibration curve in the concentration range of 0.05-8μg/L with respect to naphthalene,acenaphthylene,acenaphthene and 0.01-8μg/L for dibenz[a,h]anthracene and 0.05-14μg/L for fluorene,phenanthrene,anthracene and 0.01-14μg/L for the rest of ***,the good accuracy and repeatability of the method made sure the requirements for achieving reliable analysis of PAHs in the environmental water samples,and the recoveries of optimal method were in the range of 80-120%except to higher volatility PAHs.C_(30)-bonded silica was proved to be an efficient sorbent for extraction of high molecular weight PAHs.

关键词： Polycyclic aromatic hydrocarbons C30-bonded silica Gas chromatography-mass spectrometry solid-phase extraction Water analysis

A Tailored High-Efficiency Sample Pretreatment Method for Simultaneous Quantification of 10 Classes of Known Endogenous Phytohormones

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Plant Communications 2020年第3期1卷 75-84页

作者： Peiyong Xin Qiuhuan Guo Bingbing Li Shujing Cheng Jijun Yan Jinfang Chu National Centre for Plant Gene Research(Beijing) Innovation Academy for Seed DesignInstitute of Genetics and Developmental BiologyChinese Academy of SciencesBeijing 100101P.R.China University of Chinese Academy of Sciences Beijing 100039P.R.China

One of the hottest topics in plant hormone biology is the crosstalk mechanisms,whereby multiple classes of phytohormones interplay with each other through signaling *** better understand the roles of hormonal crosstalks in their complex regulatory networks,it is of high significance to investigate the spatial and temporal distributions of multiple-phytohormones simultaneously from one plant tissue *** this study,we develop a high-sensitivity and high-throughput method for the simultaneous quantitative analysis of 44 phytohormone compounds,covering currently known 10 major classes of phytohormones(strigolactones,brassinosteroids,gibberellins,auxin,abscisic acid,jasmonic acid,salicylic acid,cytokinins,ethylene,and polypeptide hormones[e.g.,phytosulfokine])from only 100 mg of plant *** compounds were grouped and purified separately with a tailored solid-phase extraction procedure based on their physicochemical properties and then analyzed by LC–MS/*** recoveries of our method ranged from 49.6%to 99.9%and the matrix effects from 61.8%to 102.5%,indicating that the overall sample pretreatment design resulted in good *** limits of quantitation(LOQs)of our method ranged from 0.06 to 1.29 pg/100 mg fresh weight and its precision was less than 13.4%,indicating high sensitivity and good reproducibility of the *** of our method in different plant matrices demonstrated its wide ***,these advantages will make our method helpful in clarifying the crosstalk networks of phytohormones.

关键词： phytohormones quantitative analysis LC-MS/MS solid-phase extraction plant tissue

Determination of Chromium and Nickel in Water Samples by Zinc Oxide Nanoparticle-Chitosan:Equilibrium,Kinetic and Thermodynamic Studies

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Journal of Analysis and Testing 2018年第4期2卷 299-305页

作者： Mostafa Khajeh Tabandeh Karimi Nemch Department of Chemistry Faculty of ScienceUniversity of ZabolZabolIran

This study describes the preparation of zinc oxide nanoparticle-chitosan as a solid-phase adsorbent for separation and preconcentration of trace amount of chromium and nickel from environmental water samples and their determination by inductively coupled plasma optical emission *** factors including pH,amount of adsorbent,amount of 1-(2-pyridylazo)-2-naphthol,sample volume,eluent concentration and extraction time were investigated and *** equilibrium data according to the Freundlich’s and Langmuir models were *** results showed that the equi-librium data were well fitted with Langmuir isotherm *** best fit of adsorption kinetics was attained with a second-order *** the optimum conditions,the detection limits for chromium and nickel were 0.041 and 0.039μg L^(−1),respectively,and the relative standard deviations(RSD%)were 1.5%and 1.3%(n=10,c=50μg L^(−1))for chromium and nickel,*** procedure was then used for preconcentration and determination of target compounds from envi-ronmental water samples.

关键词： Chromium Nickel Zinc oxide nanoparticle-chitosan solid-phase extraction Water samples

Preparation and Application of Polymerized High Internal phase Emulsion Monoliths for the Preconcentration and Determination of Malachite Green and Leucomalachite Green in Water Samples

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Journal of Analysis and Testing 2020年第4期4卷 264-272页

作者： Li-Ping Jiang Na Li Lin-Qi Liu Xian Zheng Fu-You Du Gui-Hua Ruan Guangxi Key Laboratory of Electrochemical and Magnetochemical Functional Materials College of Chemistry and BioengineeringGuilin University of TechnologyGuilin 541004China College of Biological and Environmental Engineering Changsha UniversityChangsha 410022China

Polymerized high internal phase emulsion(polyHIPE)monoliths were prepared and applied as adsorbent materials for solid-phase extraction(SPE)of malachite green(MG)and leucomalachite green(LMG)from water *** polyHIPE monoliths were prepared by post-functionalization of monolithic surface with 6-aminocaproic acid(ACA)via ring opening reaction of epoxy groups in glycidyl methacrylate(GMA)-based polyHIPEs,and then applied to the preconcentration and determination of trace MG and LMG in environmental water samples by combing with high-performance liquid chromatog-raphy(HPLC).Taking MG and LMG as targets,main factors affecting SPE performance of the polyHIPE monoliths were *** the optimized conditions,the ACA-functionalized polyHIPE monoliths could effectively preconcentrate MG and LMG from 150 mL of water samples,and the recoveries of MG and LMG at three spiked levels were ranged from 84.8 to 97.4%with the relative standard deviations(RSDs)lower than 6%.The proposed method exhibited good linearity in the range of 2-200 ng mL^(-1),with low limits of detection of 17.0 and 8.7 pg mL^(-1)for MG and LMG,*** addi-tion,the prepared ACA-modified polyHIPE monolith showed good durability and stability,and it could be reused for 200 cycles without obvious losing the extraction performance.

关键词： High internal phase emulsion solid-phase extraction High-performance liquid chromatography Malachite green Leucomalachite green

Ionic liquids functionalized β-cyclodextrin polymer for separation/analysis of magnolol

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Journal of Pharmaceutical Analysis 2014年第4期4卷 242-249页

作者： Nan Zhou Xia-Shi Zhu College of Chemistry & Chemical Engineering Yangzhou University

Ionic liquids functionalized β-cyclodextrin polymer, a mono-6-deoxy-6-（1,2-dimethylimida- zolium）-β-cyclodextrin iodide polymer （ILs-β-CDCP）, was synthesized as a solid-phase adsorbent coupled with high-performance liquid chromatography for separating or analyzing magnolol in drug samples. The results showed that magnolol was adsorbed rapidly on ILs-D-CDCP and eluted with methanol. Under the optimum conditions, preconcentration factor of the proposed method was 12. The linear range, limit of detection （LOD）, correlation coefficient （R） and relative standard deviation （RSD） were found to be 0.02-8.00 μg/mL, 1.9 ng/mL, 0.9992 and 2.76% （n=3, c=2.00 pg/mL）, respectively. The interaction between 1Ls-]）-CDCP and magnolol was studied through the inclusion constant, FTIR and TGA analysis. This proposed method has been successfully applied to the determination of magnolol in real samples.

关键词： Magnolol Ionic liquidsfunctionalized-β-cyclodextrin polymer solid-phase extraction High-performance liquidchromatography

Simultaneous determination of telmisartan and amlodipine in human plasma by LC-MS/MS and its application in a human pharmacokinetic study

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Journal of Pharmaceutical Analysis 2012年第5期2卷 319-326页

作者： Vasu Babu Ravi Jaswanth Kumar Inamadugu Nageswara Rao Pilli Vudagandla Sreenivasulu Venkateswarlu Ponneri Research Studies Rayalaseema UniversityKurnool 518002India Wellquest Clinical Research Laboratories RamanthapurHyderabad 500013India BioPolymer and Thermophysical Lab Department of ChemistrySri Venkateswara UniversityTirupati 517502India Analytical and Environmental Chemistry Division Department of ChemistrySri Venkateswara UniversityTirupati 517502India

A rapid and sensitive liquid chromatography-tandem mass spectrometric （LC-MS/MS） assay method has been developed and fully validated for the simultaneous quantification of telmisartan and amlodipine in human plasma. Carbamazepine was used as an internal standard. Analytes and the internal standard were extracted from human plasma by solid-phase extraction technique using Waters Oasis HLB 1 cm3 （30 mg） extraction cartridge. The reconstituted samples were chromatographed on a Hypurity advance C18 column （50mm × 4.6mm, 5 gm） using a mixture of acetonitrile -5 mM ammonium acetate buffer （pH-4.0）（50：50, v/v） as the mobile phase at a flow rate of 0.8mL/min. The calibration curve obtained was linear （r_〉0.99） over the concentration range of 2.01-400.06 ng/mL for telmisartan and 0.05 -10.01 ng/mL for amlodipine. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more than 400 human plasma samples per day. The proposed method was found to be applicable to clinical studies.

关键词： Telmisartan Amlodipine Human plasma solid-phase extraction LC-MS/MS Pharmacokinetics

Simultaneous determination of pioglitazone and candesartan in human plasma by LC-MS/MS and its application to a human pharmacokinetic study

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Journal of Pharmaceutical Analysis 2012年第3期2卷 167-173页

作者： Vijaya Kumari Karra Nageswara Rao Pilli Jaswanth Kumar Inamadugu J.V.L.N.Seshagiri Rao University College of Pharmaceutical Sciences Jawaharlal Nehru Technological UniversityKukatpallyHyderabad-500085India Analytical and Environmental Chemistry Division Department of ChemistrySri Venkateswara UniversityTirupati-517502India College of Pharmaceutical Sciences Andhra UniversityVisakhapatnam-530003India

A simple and rapid liquid chromatography-tandem mass spectrometric(LC-MS/MS) assay method has been developed and fully validated for simultaneous quantification of pioglitazone and candesartan in human *** was used as an internal *** analytes were extracted from human plasma samples by solid-phase extraction technique using a Strata-X 33 mm polymeric *** reconstituted samples were chromatographed on a C18 column by using a 80:20(v/v) mixture of acetonitrile and 0.1% formic acid as the mobile phase at a flow rate of 0.8 mL/*** calibration curves obtained were linear(rZ0.99) over the concentration range of 15-3000 ng/mL for pioglitazone and 5-608 ng/mL for *** results of the intra-and inter-day precision and accuracy studies were well within the acceptable limits.A run time of 2.7 min for each sample made it possible to analyze more than 300 plasma samples per *** proposed method was found to be applicable to clinical studies.

关键词： Pioglitazone Candesartan Human plasma solid-phase extraction LC-MS/MS Pharmacokinetics

Cathodic adsorptive stripping voltammetry of an anti-emetic agent Granisetron in pharmaceutical formulation and biological matrix

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Journal of Pharmaceutical Analysis 2012年第6期2卷 443-449页

作者： Rajeev Jain Ramkishor Sharma School of Studies in Chemistry Jiwaji University

Granisetron showed one well-defined reduction peak at Hanging Mercury Drop Electrode （HMDE） in the potential range from -1.3 to -1.5 V due to reduction of C=N bond. solid-phase extraction technique was employed for extraction of Granisetron from spiked human plasma. Granisetron showed peak current enhancement of 4.45% at square-wave voltammetry and 5.33% at cyclic voltammetry as compared with the non stripping techniques. The proposed voltammetric method allowed quantification of Granisetron in pharmaceutical formulation over the target concentration range of 5-200 ng/mL with detection limit 13.63 ng/mL, whereas in human plasma 50-225 ng/mL with detection limit 11.75 ng/mL.

关键词： Granisetron Human plasma solid-phase extraction Pharmaceuticalformulation Voltammetry Hanging mercury dropelectrode

Voltammetric quantification of anti-hepatitis drug Adefovir in biological matrix and pharmaceutical formulation

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Journal of Pharmaceutical Analysis 2012年第2期2卷 98-104页

作者： Rajeev Jain Ramkishor Sharma School of Studies in Chemistry Jiwaji University

Electrochemical reduction behavior of Adefovir was studied using Hanging Mercury Drop Electrode (HMDE) in Britton-Robinson (BR) buffer *** study showed one well-defined reduction peak in the potential range -1.2 to -1.4 V (***/AgCl) due to reduction of C=N bond of the imidazole ***-phase extraction and protein-precipitation techniques were employed for extraction of Adefovir from human *** proposed method allows quantification of Adefovir in human plasma over the concentration range 0.50-5.00 μg/mL with the detection limit 0.17 μg/mL,whereas in pharmaceutical formulation 0.25-2.25 μg/mL with the detection limit 0.08 μg/mL.

关键词： Voltammetry Adefovir solid-phase extraction Protein-precipitation Human plasma Pharmaceutical formulation

Separation and enrichment of trace ractopamine in biological samples by uniformly-sized molecularly imprinted polymers

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Journal of Pharmaceutical Analysis 2012年第6期2卷 395-402页

作者： Ya Li Qiang Fu Meng Liu Yuan-Yuan Jiao Wei Du Chong Yu Jing Liu Chun Chang Jian Lu Faculty of Pharmacy School of Medicine Xi'an Jiaotong University Department of Pharmacy Northwest Hospital Department of Pharmacy The First Affiliated Hospital of Xinjiang Medical University Xian Yang Central Hospital

In order to prepare a high capacity packing material for solid-phase extraction with specific recognition ability of trace ractopamine in biological samples, uniformly-sized, molecularly imprinted polymers （MIPs） were prepared by a multi-step swelling and polymerization method using methacrylic acid as a functional monomer, ethylene glycol dimethacrylate as a cross-linker, and toluene as a porogen respectively. Scanning electron microscope and specific surface area were employed to identify the characteristics of MIPs. Ultraviolet spectroscopy, Fourier transform infrared spectroscopy, Scatchard analysis and kinetic study were performed to interpret the specific recognition ability and the binding process of MIPs. The results showed that, compared with other reports, MIPs synthetized in this study showed high adsorption capacity besides specific recognition ability. The adsorption capacity of MIPs was 0.063 mmol/g at 1 mmol/L ractopamine concentra- tion with the distribution coefficient 1.70. The resulting MIPs could be used as solid-phase extraction materials for separation and enrichment of trace ractopamine in biological samples.

关键词： Ractopamine Uniformly-sizedmolecularly imprintedpolymers solid-phase extraction Multi-step swelling andpolymerization Separation andenrichment