分散液相微萃取/液相色谱串联质谱法快速测定猪尿中的盐酸克伦特罗与氯霉素

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 ngD9-盐酸克伦特罗和D5-氯霉素内标,调节pH至10.0,加入10％ NaC1,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...

Determination of Clenbuterol and Chloramphenicol in Pig Urine Using Dispersive Liquid-Liquid Microextraction with High Performance Liquid Chromatography-Tandem Mass Spectrometry

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.