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Impurity analysis of gentamicin bulk samples by improved liquid chromatography-ion trap mass spectrometry

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Science China Chemistry 2011年第9期54卷 1518-1528页

作者： ZHENG Chao WANG BoChu WANG MingJuan HOOGMARTENS Jos SCHEPDAEL Ann Van ADAMS Erwin Bioengineering College of Chongqing University Chongqing 400030 China Katholieke Universiteit Leuven Faculteit Farmaceutische Wetenschappen Laboratorium voor Farmaceutische Analyse O&N2 PB 923 Herestraat 49 B-3000 Leuven Belgium National Institute for Control of Pharmaceutical and Biological Products Beijing 100050 China

Several gentamicin bulk samples from different origins were investigated using an LC/MS *** equipped with ion trap MS with positive ionization was performed on a Capcell Pak C18(AQ) column with the mobile phase containing 50 mM trifluoroacetic(TFA) and *** present in batches of gentamicin bulk samples were elucidated and compared according to their fragmentation *** total seventeen impurities present in samples,five impurities were not elucidated and two compounds were identified *** was observed that the impurity profiles were different in samples from different origins which indicate necessity in the quality control of gentamicin.

关键词： gentamicin liquid chromatography LC/MS impurity analysis

A serum metabonomic study on the difference between alcoholand HBV-induced liver cirrhosis by ultraperformance liquid chromatography coupled to mass spectrometry plus quadrupole time-of-flight mass spectrometry

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Chinese Medical Journal 2011年第9期124卷 1367-1373页

作者： LIAN Jiang-shan LIU Wei HAO Shao-rui GUO Yong-zheng HUANG Hai-jun CHEN De-ying XIE Qing PAN Xiao-ping XU Wei YUAN Wen-xia LI Lan-juan HUANG Jian-rong Department of Infectious Disease State Key Laboratory for Diagnosis and Treatment of Infectious Disease the First Affiliated Hospital College of Medicine Zhejiang University Hangzhou Zhejiang 310003 China

Background Liver cirrhosis is the fatal consequence of chronic hepatitis, making early diagnosis of liver cirrhosis critical. Liver biopsy is still the standard diagnostic method for liver cirrhosis, although its use in a broad population with alcoholism or hepatitis B virus （HBV） infection remains difficult. In this study, we used a metabonomic approach to detect potential biomarkers for early diagnosis of liver *** Serum specimens were collected prospectively from normal control subjects （n=22） and patients with alcoholic cirrhosis （n=18） or HBV-induced cirrhosis （n=19）. The serum metabonome was analyzed using ultraperformance liquid chromatography （LC）Rime-of-flight mass spectrometry （MS） integrated with chemometrics. The acquired LC-MS data were normalized and processed using principal component analysis （PCA） and partial least squares discrimination analysis （PLS-DA）.Results Significant differences in the metabonomics among the three groups were observed. Lysophosphatidyl cholines （LPCs）（LPC C16：0, LPC C18：0, LPC C18：2, LPC C18：3, LPC C20：3, LPC C20：5） were decreased in the serum of patients with hepatic cirrhosis, whereas bile acids （glycocholic acid, glycochenodeoxycholic acid）, hypoxanthine, and stearamide were increased in the serum of patients with hepatic cirrhosis. These metabolites are considered ＂common＂biomarkers for hepatic cirrhosis. Oleamide and myristamide were increased in the serum of patients with alcoholic cirrhosis but decreased in those with HBV-induced cirrhosis. These could be specific biomarkers for differential diagnosis between alcohol- and HBV-induced hepatic *** There are significant metabonomic differences between alcohol- and HBV-induced liver *** is a top-down systems biology tool for conducting research on clinical problems.

关键词： metabonomics liquid chromatography liver cirrhosis multivariate analysis

High-performance isotope-labeling liquid chromatography mass spectrometry for investigating the effect of drinking Goji tea on urine metabolome profiling

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Science China Chemistry 2014年第5期57卷 678-685页

作者： TSENG Chiao-Li LI Liang Department of Chemistry University of Alberta

Urine is a human biofluid that is widely used for metabolomics research on disease biomarker ***,the metabolome profiles generated from comparative groups of individuals should mainly consist of the endogenous human metabolites that reflect the healthy states of the ***,external factors,such as diet,may alter the urine metabolome profile by either introducing a significant amount or variety of exogenous metabolites to urine or inducing changes of the metabolome ***,strict control of the external factors during the sample collection process is critical for urine metabolomics aimed at discovery of disease *** this work,we describe a study to determine the effect of drinking Goji tea,which is considered a nutritional supplement drink in some regions of the world,on urine metabolome *** purpose of this work is not to determine the nutritional values of Goji tea,but to investigate whether drinking a moderate amount of Goji tea 1-3 h(short-term effect)or 12 h(longer-term effect)before urine collection can cause significant variations of urine metabolome profiles.A highly sensitive dansylation isotope labeling liquid chromatography mass spectrometry(LC-MS)method was used to determine the urine metabolomes before and after drinking Goji *** the studies of the short term(<3 h)and longer term(12 h)effects of drinking Goji tea,it is clear that the consumption of a moderate amount of Goji tea does not affect the urine metabolome *** for 12 h should be sufficient to remove any potential interference of Goji metabolites from the human urine metabolome profile.

关键词： metabolomics urine metabolites mass spectrometry liquid chromatography isotope labeling Goji diet

Development of Ultranarrow-Bore Open Tubular High Efficiency liquid chromatography

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Chinese Journal of Chemistry 2022年第1期40卷 137-152页

作者： Yingyan Zhou Guangsheng Guo Xiayan Wang Center of Excellence for Environmental Safety and Biological Effects Beijing Key Laboratory for Green Catalysis and SeparationDepartment of Chemistry and BiologyBeijing University of TechnologyBeijing 100124China

chromatography theory shows that when the inner diameter of the chromatography column is very narrow(e.g.,1—2μm),the maximum efficiency will be produced in liquid *** addition,the increasing demand for ultrasmall volume sample analysis has produced the trend of narrowing the diameter of the liquid chromatography *** have verified that ultranarrow-bore open tubular liquid chromatography(i.d.≤2μm)has the advantages of small sample requirement and high separation ***,there also exist huge challenges along with such obvious *** review summarizes the efforts made by our research group and other research groups to develop this *** hope that in the near future,ultranarrow bore open-tube liquid chromatography can be successfully and maturely applied to the application of analytes with ultrasmall size and volume such as single-cell and even subcellular organelles omics research.

关键词： Ultra narrow-bore liquid chromatography Ultrahigh separation efficiency Pico-PLOT column Analytical methods

New lysine-acetylated proteins screened by immunoaffinity and liquid chromatography-mass spectrometry

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Science China Chemistry 2010年第1期53卷 238-244页

作者： ZHANG Bing ZHAO Chao LUO KaiXuan YAN GuoQuan YAO Jun WANG YingYin LU HaoJie FAN HuiZhi YANG PengYuan Department of Chemistry Fudan UniversityShanghai 200433China Institutes of Biomedical Sciences Fudan UniversityShanghai 200032China

The lack of selective extraction specific for lysine-acetylated proteins has been a major problem in the field of acetylation biology,though acetylation plays a key role in many biological *** this paper,we report for the first time the proteomic screening of lysine-acetylated proteins from a mouse liver tissue,by a new approach of immunoaffinity purification of lysine-acetylated peptides combined with nano-HPLC/MS/MS *** have found 20 lysine-acetylated proteins with 21 lysine-acetylated sites,among which 12 lysine-acetylated proteins and 16 lysine-acetylated sites have never been reported ***,three acetyltransferases harboring in mitochondrion are newly discovered acetyltransferases responsible for the acetylation of nonhistone *** have explored the significant patterns of residue preference by the hierarchical clustering analysis of amino acid residues surrounding acetylation sites,which could be helpful to the prediction of new sites of lysine *** findings provide more candidates for studying the important roles played by acetylation in diverse cellular pathways and related human diseases.

关键词： lysine acetylation immunoaffinity purification liquid chromatography mass spectrometry

Two-dimensional MOF Cu-BDC nanosheets/ILs@silica core-shell composites as mixed-mode stationary phase for high performance liquid chromatography

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Chinese Chemical Letters 2022年第8期33卷 3869-3872页

作者： Tiantian Si Xiaofeng Lu Haixia Zhang Shuai Wang Xiaojing Liang Yong Guo CAS Key Laboratory of Chemistry of Northwestern Plant Resources and Key Laboratory for Natural Medicine of Gansu Province Lanzhou Institute of Chemical PhysicsChinese Academy of SciencesLanzhou 730000China State Key Laboratory of Applied Organic Chemistry and College of Chemistry and Chemical Engineering Lanzhou UniversityLanzhou 730000China University of Chinese Academy of Sciences Beijing 100049China

Here,silica microspheres were decorated with two-dimensional metal-organic frameworks(2 D MOFs)nanosheets and ionic liquids,and evaluated as the mixed-mode stationary phase for chromatographic *** ionic liquids were used to assist the synthesis of 2 D MOFs nanosheets,and also acted as adhesives among the nanosheets and *** contrast with the 2 D MOFs-based column without ionic liquids and commercial columns,the prepared column exhibited enhanced chromatographic separation performance for partially hydrophilic compounds such as alkaloids,sulfonamides and antibiotics,*** addition to excellent chromatographic repeatability and stability,it has also been verified that the composites could be easily and repeatedly *** relative standard deviation of the retention time of the same type of analyte between the three batches of materials was ranging from 0.21%to 1.7%.In short,these results indicated that the synthesized composites were promising separation material for liquid chromatography,which made it possible to broaden the application of 2 D MOFs in the field of chromatography.

关键词： 2D MOF composites Chromatographic separation liquid chromatography Mixed-mode Stationary phase

Simultaneous determination of 20 food additives by high performance liquid chromatography with photo-diode array detector

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Chinese Chemical Letters 2012年第4期23卷 492-495页

作者： Kang Ma Ya Nan Yang Xiao Xiong Jiang Min Zhao Ye Qiang Cai Division of Chemical Metrology and Analytical Science National Institute of Metrology of ChinaBeijing 100013China Division of Chemical Metrology Jiangsu Institute of MetrologyNanjing 210007China State Ke.v lztbotzltory of Bioactive Substances and Functions of Natural Medicines lnstitute of Materia MedicaChinese Academy of Medical Sciences and Peking Union Medical CollegeBeijing 100050China

An efficient and accurate analytical method was developed for the simultaneous determination of 20 synthetic food additives, including three sweeteners,seven food colorants,nine synthetic preservatives and caffeine,by high performance liquid chromatography （HPLC） with photodiode array detector（PDA）.This method permits the detection of food additives at very low concentrations（0.005-0.150μg/mL）.The applicability was verified by the determination of food additives present in various foodstuffs.

关键词： Food additives liquid chromatography Photodiode array detector Drinks

Quantification of theophylline or paracetamol in milk matrices by high-performance liquid chromatography

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Journal of Pharmaceutical Analysis 2017年第6期7卷 401-405页

作者： Tania A.P.Fernandes Joao P.Aguiara Ana I.Fernandes Joao F.Pinto CiiEM-Centro de Investigacao Interdisciplinar Egas Moniz Instituto Superior de Cinncias da Saude Egas MonizCampus Universitario-Quinta da GranjaMonte de Caparica2829-511 CaparicaPortugal iMed.UL-Dep.Tecnologia Farmaceutica Faeuldade de FarmdciaUniversidade de LisboaAv.Prof.Gama Pinto1649-003 LisboaPortugal

A simple, accurate and sensitive high-performance liquid chromatography （HPLC） method was developed, validated and applied to the determination of either theophylline or paracetamol in milk-based samples. The method allowed drug quantification in fresh and powdered milk with a relatively short run time of analysis and it was also successfully applied to the quantification of the drugs in solid dosage forms intended for pediatric use. Moreover, the main significant advantages over other published works are the simplicity of the sample preparation, reduced assay time and sample loss. The method meets the International Conference on Harmonization guideline for analytical methods validation regarding specificity, linearity, accuracy, precision, specificity and robustness as required by health authorities and applied by industry while designing and marketing new drug products. The technique encompasses the separation of the analytes with a reverse phase C18 column under isocrafic conditions and UV detection at 272 nm and 243 nm, respectively, for theophylline and paraeetamol. The lower limit of quantification for both drugs was determined as 0.2 μg/mL and the between-batch accuracy was 99.7%. This HPLC method allows quantification of theophylline and paracetamol in milk matrices and it can be applied in the design, development and production of milk-based pediatric dosage forms.

关键词： liquid chromatography Fresh milk Powdered milk Paracetamol Theophylline

Determination of Stereoisomers of Epalrestat by liquid chromatography

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Journal of Beijing Institute of Technology 2004年第4期13卷 445-448页

作者：齐美玲王鹏杨建军 School of Science Beijing Institute of Technology Beijing100081 China School of Pharmaceutical Engineering Shenyang Pharmaceutical University ShenyangLiaoning110015 China Jinxing Pharmaceuticals Ltd Xingtai Hebei 054000 China

An isocratic reversed-phase liquid chromatographic (LC) method is described for the determination of epalrestat and its three stereoisomers (degradation impurities) in drug substance. The LC separation system consisted of a Hypersil C18 column (250 mm×4.6 mm, 5 μm) with a mobile phase comprising methanol, acetonitrile and water (volume ratio 60∶1∶50, pH 4.5) delivered at a flow rate of 1.6 mL/min and UV detection at 280 nm. The proposed LC method is simple and selective for the determination of the stereoisomers of epalrestat in the drug substance with a limit of detection and quantification of 3.9 μg/mL and 4.9 μg/mL, respectively. The stereoisomers were identified by liquid chromatography-mass spectrometry (LC-MS).

关键词： liquid chromatography epalrestat stereoisomers