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固相萃取-GC-MS法测定饲料中的沙丁胺醇

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分析测试学报 2004年第Z1期23卷 244-248页

作者：范理王彤田静高生苏晓鸥郑君杰国家饲料质量监督检验中心北京100081 北京市饲料监察所北京100012

　　沙丁胺醇(salbutamol),化学名称1-(4-羟基-3-羟甲基苯基)-2-(叔丁氨基)乙醇(结构式如图1所示),俗称舒喘宁,属于β-兴奋剂类药物的一种,临床上用于治疗支气管哮喘.同时沙丁胺醇同克伦特罗(瘦肉精)一样还具有提高饲料的转化率,促进动... 详细信息

　　沙丁胺醇(salbutamol),化学名称1-(4-羟基-3-羟甲基苯基)-2-(叔丁氨基)乙醇(结构式如图1所示),俗称舒喘宁,属于β-兴奋剂类药物的一种,临床上用于治疗支气管哮喘.同时沙丁胺醇同克伦特罗(瘦肉精)一样还具有提高饲料的转化率,促进动物生长的作用.但是,这种药物容易在动物内脏、组织中蓄积残留,有很大的副作用.……

关键词： Salbutomal Feed solid-phase extraction Gas chromatography - mass spectrometry

Application of multiwalled carbon nanotubes treated by potassium permanganate for determination of trace cadmium prior to flame atomic absorption spectrometry

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Journal of Environmental Sciences 2007年第10期19卷 1266-1271页

作者： XIAO Jun-ping ZHOU Qing-xiang BAI Hua-hua Department of Chemistry University of Science and Technology Beijing Beijing 100083 China Henan Key Laboratory for Environmental Pollution Control School of Chemistry and Environmental Sciences Henan Normal University Xinxiang 453007 China

In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes （MWCNTs） and established a new method for the determination of trace cadmium in environment with flame atomic absorption spectrometry. The MWCNTs were oxidized by potassium permanganate under appropriate conditions before use as preconcentration packing. Parameters influencing the recoveries of target analytes were optimized. Under optimal conditions, the target analyte exhibited a good linearity （R^2=0.9992） over the concentration range 0.5-50 ng/ml. The detection limit and precision of the proposed method were 0.15 ng/ml and 2.06%, respectively. The proposed method was applied to the determination of cadmium in real-world environmental samples and the recoveries were in the range of 91.3%-108.0%. All these experimental results indicated that this new procedure could be applied to the determination of trace cadmium in environmental waters.

关键词： multiwalled carbon nanombes (MWCNTs) solid-phase extraction flame atomic absorption spectrometry

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多壁纳米碳管固相萃取测定水中的有机氯农药

分析测试学报 2004年第Z1期23卷 258-261页

作者：张玲金谢文明国家地质实验测试中心北京100037 吉林农业大学吉林长春130118

　　对于水样中的有机氯农药的净化方法主要是采用传统的液液分配的方法,缺点是溶剂使用量和前处理复杂.近年来固相萃取及固相微萃取等技术被应用到水样中的有机污染物的测定[1,2].如利用键合在硅胶上的非极性(C18,LC18等)或极性物质(LC... 详细信息

　　对于水样中的有机氯农药的净化方法主要是采用传统的液液分配的方法,缺点是溶剂使用量和前处理复杂.近年来固相萃取及固相微萃取等技术被应用到水样中的有机污染物的测定[1,2].如利用键合在硅胶上的非极性(C18,LC18等)或极性物质(LC-CN,LC-NH2)对水中有机物进行富集,用GDX或XAD自填的固相柱的报道也很多[3,4].……

关键词： Multiwalled carbon nanotubes solid-phase extraction Organochlorine pesticides

凝胶渗透色谱和气相色谱-质谱法测定动物食品中27种有机氯和15种拟除虫菊酯类农药残留量

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分析测试学报 2007年第Z1期26卷 253-255,258页

作者：王云凤常春艳陈其勇葛宝坤高健会宓捷波天津出入境检验检疫局天津300456

A GC-MS method for the determination of 27 organochlorine pesticides and 15 Pyrethroid pesticides in animal food is *** method was based on Gel Permeation chromatography combined with solid-phase extraction for sample *** qualitative and quantitative analyses was carried out by gas chromatography-mass spectrometry under the selective-ion monitoring *** experimental results showed that the correlation coefficients were better than 0.99,the recoveries for spiked standards were 70%-104%,the relative standard deviations were 2.1%-15.9%.

关键词： Organochlorine pesticides Pyrethroid pesticides Gel Permeation chromatography solid-phase extraction Gas chromatography-mass spectrometry Animal food

Detection and quantitation of PS20, a phosphorothioate oligodeoxynucleotides in monkey plasma

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Acta Pharmacologica Sinica 2004年第6期25卷 99-104页

作者： Ming-mei SHANG, Hai-feng SONG2, Xiu-wen LIU, Zhong-ming TANG Department of Pharmacology and Toxicology, the Institute of Radiation Medicine, Academy of Military Medical Sciences, Beijing 100850, China Department of Pharmacology and Toxicology the Institute of Radiation Medicine Academy of Military Medical Sciences 北京 100850

AIM: To establish the method for quantitation of the phosphorothioate oligodeoxynucleotides (S-ODNs) in plasma. METHODS: Two solid-phase extraction columns combined with a strong anion-exchange column were utilized to remove proteins and lipids in plasma, and the salts were removed by a reverse-phase column followed by dialysis with a 2500 Da-cutoff membrane. The concentration of the tested S-ODNs, PS20, and its metabolites extracted from the plasma were determined by the method of non-gel sieving capillary electrophoresis (NGCE) with diode array detection in the presence of internal standard (IS). RESULTS: The method was with good base number specificity. Relative standard deviation % of both intra and inter assay were all less than 10 %, and the total mean recovery was about 91 %. The methodology was successfully used to determine the PK behavior of an anti-tumor antisense S-ODNs in monkeys and identify the metabolites with single base difference. CONCLUSION: The combined method of solid-phase extraction and NGCE could be used to study the pharmacokinetics of S-ODNs, and the main parameters of the methodology met the requirement of PK study.

关键词： antisense oligodeoxyribonucleotides thionucleotides rhesus monkey plasma solid-phase extraction capillary electrophoresis non-gel sieving internal standard

Optimization of enrichment processes of pentachlorophenol (PCP) from water samples

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Journal of Environmental Sciences 2004年第1期16卷 17-20页

作者： LIPing LIUJun-xin ResearchCenterforEco-EnvironmentalSciences.ChineseAcademyofSciences Beijing100085

The method of enriching PCP(pentachlorophenol) from aquatic environment by solid phase extraction(SPE) was studied. Several factors affecting the recoveries of PCP, including sample pH, eluting solvent, eluting volume and flow rate of water sample, were optimized by orthogonal array design(OAD). The optimized results were sample pH 4; eluting solvent, 100% methanol; eluting solvent volume, 2 ml and flow rate of water sample, 4 ml/min. A comparison is made between SPE and liquid-liquid extraction(LLE) method. The recoveries of PCP were in the range of 87.6%—133.6% and 79%—120.3% for SPE and LLE, respectively. Important advantages of the SPE compared with the LLE include the short extraction time and reduced consumption of organic solvents. SPE can replace LLE for isolating and concentrating PCP from water samples.

关键词： pentachlorophenol(PCP) solid-phase extraction liquid-liquid extraction

Biosynthesis of imipramine glucuronide and characterization of imipramine glucuronidation catalyzed by recombinant UGTIA4

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Acta Pharmacologica Sinica 2006年第5期27卷 623-628页

作者： Ming-rong QIAN Su ZENG~2 Department of Pharmaceutical Analysis and Drug Metabolism,College of Pharmaceutical Sciences,Zhejiang University,Hangzhou 310031,China Department of Pharmaceutical Analysis and Drug Metabolism College of Pharmaceutical Sciences Zhejiang University Hangzhou China

Aim:To study the profile of imipramine N~+-glucuronidation using homogenatesof recombinant uridine-5′-diphosphoglucuronosyltransferase 1A4 (UGT1A4) frombaculovirus-infected sf9 ***:Recombinant UGT1A4 was obtainedfrom sf9 cells infected with recombinant *** N~+-glucuronidewas biosynthesized by incubating imipramine with recombinant UGT1A4 andthen purified with solid-phase cartridges.A reversed phase-high pressure liquidchromatography (RP-HPLC) assay method was used to directly measure the con-centration of imipramine and its metabolite,imipramine N~+-glucuronide,withp-nitrophenol as the internal *** validated method was used to charac-terize the activity of recombinant UGT1A4 and carry out kinetic studies on imi-pramine glucuronidation in ***:The high concentration of imipramineinhibited glucuronide conjugation,so the formula V=Vmax·S/(Km+S+S~2/Ki) was usedto calculate the parameters,using MATLAB *** values of apparentKm,Ki,and Vmaxfor imipramine glucuronidation via UGT1A4 were 1.39±0.09mmol/L,6.24±0.45 mmol/L and 453.81±32.12 pmol/min per mg cell homogenate (n=3),***:As a specific substrate of UGT1A4,imipramine wasused as a convenient method to characterize the activity of recombinant UGT1A4by using ***,the profile of imipramine glucuronidation was evalu-ated by using recombinant UGT1A4 in vitro.

关键词： imipramine glucuronide uridine-5’-diphosphoglucuronosyltransferase IA4 baculovirus solid-phase extraction

Study on the Preparation of Mercaptoacetic Acid-modified Heterophylla Shell and Its Application in Separation and Enrichment of Pb^2＋ in Environmental Samples

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Chemical Research in Chinese Universities 2018年第4期34卷 665-669页

作者： LYU Linlin JIANG Xlaojun JIA Lian AI Tian WU Hang School of Chemical Engineering University of Science and Technology Liaoning Anshan 114051 P. R. China School of Chemistry and Life Science Anshan Normal University Anshan 114005 P. R. China

To increase the adsorption capacity of the Corylus heterophylla Fisch（HS） for Pb2＋, HS was chemically modified using NaOH aqueous solution and 95% ethanol and was labeled as SHS; then SHS was chemically modified using mercaptoacetic acid. The SHS modified with mercaptoacetic acid（MHS） was characterized using FTIR, SEM, and XPS. The results indicated that the --SH group was present on MHS, and after Pb2＋ adsorption, the absorption value of the characteristic peak of the --SH group decreased. The adsorption and desorption properties of this func- tionalized material were investigated as well as the influences of parameters, such as pH value, type of desorption reagent, dosage, flow rate and maximum sample volume. The Pb2~ adsorption of MI-IS reached a maximum with pH〉5. The experimental data of Pb2＋ adsorption using MHS were fitted using the Langmuir isothermal adsorption model, and a maximum adsorption capacity of 61.54 mg/g was obtained. This was much higher than the adsorption capacity of SHS before modification with the thiol group. After adsorption, MHS was desorbed using a 0.2 mol/L HC1 solution, and the percent of desorption was higher than 99%. MHS was used as a solid-phase extractant in the analysis and determination of Pb2＋ content in food and water samples, and the enrichment times achieved 150-fold.

关键词： Corylus heterophylla Fisch Chemical modification Pb Adsorption solid-phase extraction

Determination of Sex Hormones in Antler Velvet by High Performance Liquid Chromatography Tandem Mass Spectrometry

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Chemical Research in Chinese Universities 2012年第2期28卷 191-194页

作者： LU Chun-mei WANG Ming-tai MU Jun BAI Yu-ping DU Jian-shi ZHANG Han-qi WANG Jian-wei College of Chemistry Jilin UniversityChangchun 130012P.R.China China-Japan Union Hospital of Jilin University Changchun 130021P.R.China Jilin Entry-exit Inspection and Quarantine Bureau Changehun 130061R R.China China FAW Group Corporation R&D Center Changchun 130011P.R.China Institute of Applied Chemistry Chinese Academy of SciencesChangchun 130022P.R.China

Eighteen sex hormones in antler velvet were determined by high performance liquid chromatography tandem mass *** solid phase extraction was applied to eliminating the matrix *** experimental conditions were examined and *** the optimal conditions,the proposed method provides the good linearities and determination limits（0.2―1.0 μg/kg） of the analytes *** recoveries ranging from 72.3% to 149.5% were obtained for the target analytes at two concentration *** method was applied to the determination of eighteen sex hormones in different kinds of antler velvet samples and the obtained results are *** results indicate that the proposed method is suitable for the determination of sex hormones in antler velvet samples.

关键词： Antler velvet Liquid chromatography tandem mass spectrometry Sex hormone solid-phase extraction