Determination of Clenbuterol and Chloramphenicol in Pig Urine Using Dispersive Liquid-Liquid Microextraction with High Performance Liquid Chromatography-Tandem Mass Spectrometry
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Determination of Clenbuterol and Chloramphenicol in Pig Urine Using Dispersive Liquid-Liquid Microextraction with High Performance Liquid Chromatography-Tandem Mass Spectrometry
Vol. 30, Issue 9, Pages: 1018-1022(2011)
作者机构:
1. 浙江省农业科学院农产品质量标准研究所
2. 赛默飞世尔科技(上海)有限公司色谱质谱部, 3.长沙环境保护职业技术学院环境科学系
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Determination of Clenbuterol and Chloramphenicol in Pig Urine Using Dispersive Liquid-Liquid Microextraction with High Performance Liquid Chromatography-Tandem Mass Spectrometry. [J]. 30(9):1018-1022(2011)
DOI:
Determination of Clenbuterol and Chloramphenicol in Pig Urine Using Dispersive Liquid-Liquid Microextraction with High Performance Liquid Chromatography-Tandem Mass Spectrometry. [J]. 30(9):1018-1022(2011)DOI:
Determination of Clenbuterol and Chloramphenicol in Pig Urine Using Dispersive Liquid-Liquid Microextraction with High Performance Liquid Chromatography-Tandem Mass Spectrometry
采用分散液相微萃取净化技术,建立了快速测定猪尿中盐酸克伦特罗和氯霉素残留的高效液相色谱-串联质谱分析方法。取5 mL猪尿样品,分别加入5 ng D9-盐酸克伦特罗和D5-氯霉素内标,调节pH至10.0,加入10% NaCl,经250 μL三氯甲烷和750 μL异丙醇分散萃取后离心,转移下层沉淀,氮吹后以甲醇水溶液定容,采用电喷雾正负离子切换扫描模式同时分析盐酸克伦特罗和氯霉素,内标法定量。结果表明,盐酸克伦特罗的加标质量浓度为0.05~2 μg/L,氯霉素的加标质量浓度为0.1~2 μg/L时,两者的回收率为82%~97%,相对标准偏差(RSD)为6.8%~9.6%,盐酸克伦特罗和氯霉素的定量下限(S/N=10)分别为0.05、0.1 μg/L。方法简单、灵敏,回收率和重复性良好,可用于猪尿中盐酸克伦特罗和氯霉素的测定。
Abstract
A quick and simple analytical method was developed for the determination of clenbuterol and chloramphenicol residues in pig urine using dispersive liquid-liquid microextraction combined with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).5 mL pig urine with pH adjusted to 10.0 was added with 5 ng clenbuterol-D9,5 ng chloramphenicol-D5 and 10% NaCl before extraction.Then the urine sample was added with the mixture of 250 μL chloroform and 750 μL isopropanol for dispersive liquid-liquid microextraction.After centrifugation,the sediment was transferred and dried under a gentle nitrogen flow,then redissolved with methanol-water solution.The clenbuterol and chloramphenicol in pig urine was simultaneously determined by HPLC-MS/MS under positive and negative transferring mode with the internal standard method.The spiked recoveries ranged from 82% to 97% at fortification levels of 0.05-2 μg/L for clenbuterol and 0.1-2 μg/L for chloramphenicol,with relative standard deviations of 6.8%-9.6%.The limits of quantitation(LOQs) were 0.05 μg/L for clenbuterol and 0.1 μg/L for chloramphenicol,respectively.With the advantages of convinience,sensitivity,good recoveries and repeatability,the method was suitable for the detection of clenbuterol and chloramphenicol residues in pig urine.
关键词
分散液相微萃取液相色谱-串联质谱猪尿盐酸克伦特罗氯霉素
Keywords
dispersive liquid-liquid microextractionhigh performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)pig urineclenbuterolchloramphenicol
Aptamer Electrochemiluminescence Sensor for Sensitive Detection of Chloramphenicol
Synthesis of a Carboxyl-functionalized Magnetic Carbon Nanotube and Its Extraction for Clenbuterol in Pork Samples
Determination of Residual Cyromazine and Its Metabolite Melamine in Pig Urine Samples Using Ultrahigh Performance Liquid Chromatography Coupled with Quadrupole-Orbitrap Mass Spectrometry
Preparation and Application of a Chloramphenicol Electrochemical Sensor Based on Molecularly Imprinted Polymer
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Department of Environmental Science,Beijing University of Technology
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