液相色谱-串联质谱法同时测定水产品中三苯甲烷类、氯霉素类、磺胺类、氟喹诺酮类和四环素类渔药残留  

Simultaneous determination of five kinds of veterinary drug residues in aquatic products by liquid chromatography with tandem mass spectrometry

作　　者：郭萌萌[1,2] 谭志军[1,2] 孙晓杰[1,2] 吴海燕[1,2] 孙伟红[1,2] 邢丽红[1,2] 李兆新[1,2] 翟毓秀[1,2] 

机构地区：[1]农业部水产品质量安全检测与评价重点实验室,中国水产科学研究院黄海水产研究所 [2]国家水产品质量监督检验中心,山东青岛266071

出　　处：《中国渔业质量与标准》2013年第1期51-58,共8页Chinese Fishery Quality and Standards

基　　金：国家自然科学基金项目(41106109);中央级基本科研业务费项目(20603022011004)

摘　　要：建立了同时测定水产品中三苯甲烷类染料、氯霉素类、磺胺类、氟喹诺酮类和四环素类5类共23种渔用药物残留的液相色谱-串联质谱分析方法。样品经酸化乙腈提取,C18吸附剂分散固相萃取净化,正己烷进一步除脂,滤膜过滤后进行分析。采用AtlantisdC18色谱柱,以乙腈和5mmol/L乙酸铵(含0.05%甲酸)水溶液为流动相,梯度洗脱分离后,目标分析物在选择反应监测模式(SRM)、正负离子切换扫描方式下进行定性和定量分析。所选定的23种化合物在12min内实现良好分离。其中,4种三苯甲烷类染料和氯霉素的线性范围为0.5～20.0ng/mL,检出限均为0.3μg/kg;8种磺胺类化合物、4种氟喹诺酮类化合物、甲砜霉素和氟甲砜霉素的线性范围为5.0～100.0ng/mL,检出限均为2.0μg/kg;4种四环素类化合物线性范围为10.0～200.0ng/mL,检出限均为5.0μg/kg。23种化合物的平均添加回收率为50.4%～118.5%,相对标准偏差(RSD)为2.86%～17.2%之间。该方法操作简便,灵敏度较高,可用于水产品中5类渔用药物残留的快速筛查。A method for simultaneous determination of triphenylmethanes, chloramphenicols, sulfonamides, fluoro- quinolones and tetracyclines in aquatic products by using liquid chromatography - tandem mass spectrometry （ LC - MS/MS） was developed. The sample was extracted with acidified acetonitrile, cleaned -up by dispersive solid -phase extraction using C^s dispersant sorbent, then was degreased by hexane and detected by LC -MS/MS within 12 mi- nutes. The separation of 23 veterinary drugs were performed on a Atlantis dC^8 （2.1 mm x 150 mm,3 ~xm）column u- sing a mixture of 5 mmol/L ammonium acetate containing 0.05 % formic acid （A） and acetonitrile （ B ） as mobile phase. Qualitative and quantitative analysis were carried out by eleetrospray ionization（ESI） mass spectrometry in se-lective reaction monitoring （SRM） mode. Triphenylmethanes, sulfonamides, fluoroquinolones and tetracyclines were analyzed in positive ion mode, while chloramphenicols in negative ion mode. The calibration curves were linear in the range of 0.5 - 20.0 ng ~ mL for four triphenylmethanes and choramphnicol, with detection limits of 0.3 Ixg ＂ kg ; 5.0 - 100.0 ng ~ mL for eight sulfonamides, four fluoroquinolones, thiamphenicol and florfenicol, with detection limits of 2.0 ~g ~ kg ; and 10.0 - 200.0 ng/mL for four tetracyclines, with detection limits of 5.0 txg ~ kg. The average re- coveries for 23 veterinary drugs were between 50.4 % and 118.5 % with relative standard deviations （RSD） ranged from 2.86% to 17.2 %. The developed method was simple, sensitive, and suitable for rapid analysis of large quanti- ties of samples.

关 键 词：渔用药物 残留 液相色谱-串联质谱 水产品 

分 类 号：S948[农业科学—水产养殖]