摘要
建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时测定水产品中喹诺酮类、大环内酯类、磺胺类、磺胺增效剂、林可胺类、硝基咪唑类、喹啉类和多肽类8类共38种限用兽药残留的检测方法。试样用1%乙酸乙腈溶液提取,经冷冻离心分离和正己烷净化后,HPLC-MS/MS进行测定,基质曲线外标法定量。在电喷雾正离子模式下,以多反应监测(MRM)方式采集数据进行定性与定量分析。38种兽药在水产品中的基质溶液标准曲线线性系数(r)均大于0.99;在4个不同浓度加标水平下,平均回收率为43%～123%;日内相对标准偏差(RSD)为1.0%～26.4%,日间RSD为1.6%～28.9%;定量下限(LOQ,S/N≥10)为5～20μg/kg。方法简单、快速、可靠,可用于水产品中兽药多残留的快速筛查。
A new approach was established for the simultaneous determination of eight classes of lim- ited using veterinary drug residues, including quinolones, macrolides, sulfoamides, trimethoprim, lincosamides, nitroimidazoles, quinoxalines and peptides, in aquatic products by high performance liquid chromatography - tandem mass spectrometry （ HPLC - MS/MS）. The analytes were extracted with 1% acetic acid in acetonitrile, then purified with refrigerated centrifuge and hexane. The sam- ple matrix-matched calibration was used to determine the residue contents by the external standard. Electrospray ionization mass spectrometry was operated in the positive mode using multiple reaction monitoring（MRM） for the qualitative and quantitative analyses of 38 analytes. The results indicated that correlation coefficients of the calibration curves were more than 0. 99. The average recoveries of 38 analytes at four spiked concentration levels ranged from 43% to 123%. The intra-day relative standard deviations （RSDs） were in the range of 1.0% - 26.4% , and the inter-day RSDs were 1.6% -28.9%. The limits of quantitation（ LOQs, S/N≥ 10） were in the range of 5 -20 μg/kg. The method is simple, rapid and reliable, and is suitable for the simultaneous determination of multi- residues of veterinary drugs in aquatic products.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第2期193-198,204,共7页
Journal of Instrumental Analysis
基金
国家质检总局科研项目(2011IK214)
江西省教育厅科研基金(GJJ12232)
江西农业大学创新发展基金(CX201110)
关键词
高效液相色谱-串联质谱法
水产品
限用兽药
多残留
快速筛查
high performance liquid chromatography -tandem mass spectrometry
aquatic prod- ucts
limited using veterinary drug
multiple residues
rapid screening
