动物组织与水产品中头孢氨苄残留量的液相色谱-串联质谱检测  

Determination of Cefalexin Residue in Animal Tissue and Aquatic Products by LC-MS/MS

作　　者：倪梅林[1] 崔晓美[1] 殷居易[1] 彭锦峰[1] 房科腾[1] 曹苏仙[1] 谢东华[1] 

机构地区：[1]宁波出入境检验检疫局,浙江宁波315012

出　　处：《分析测试学报》2009年第4期489-492,共4页Journal of Instrumental Analysis

基　　金：国家标准编制资助项目(20073809-T-424)

摘　　要：建立了牛肉、猪肉、肝脏、肾脏、脂肪、鱼肉、虾肉中头孢氨苄残留的Lc—MS／MS检测方法。组织样品中的头孢氨苄用甲醇-0．2％偏磷酸（体积比3：7）溶液提取，采用OasisHLB固相萃取小柱净化。分析样品以甲酸溶液（体积分数0．1％）-乙腈为流动相，经MG-ⅡC18色谱柱分离，在LC—MS／MS多反应监测模式下进行定性、定量分析，采用正离子扫描。头孢氨苄的定量下限为0．01mg／kg，动物组织和水产品样品在0．01、0．05、0．1、0．2mg／kg添加水平的回收率为75％～106％，相对标准偏差（n=10）为5．3％-12．1％。A liquid chromatography - tandam mass spectrometric （ LC - MS/MS） method was developed for the determination of cefalexin residue in beef, pork, liver, kidney, fat, fish and shrimp tissue sample. The sample was extracted by methanol -0. 2% metaphosphoric acid with volume ratio of 3 ： 7 and cleaned up by an Oasis HLB solid phase extraction （SPE） cartridge. The analyte was separated on an MG- Ⅱ C18 column using 0. 1% formic acid - acetonitrile as mobile phase, and determined qualitatively and quantitatively by LC -MS/MS under multi-reaction monitoring（MRM） mode using positive ion scaning mode. The limit of quatitation（ LOQ, S/N = 10） for cefalexin was 0. 01 mg/kg. The recoveries of cefalexin from animal tissue and aquatic products spiked with four levels at 0. 01, 0. 05, 0. 1, 0.2 mg/kg were in the range of 75% - 106% with the relative standard deviations of 5.3% - 12. 1% （n = 10）.

关 键 词：头孢氨苄 液相色谱-串联质谱 残留 动物组织 水产品 

分 类 号：O657.63[理学—分析化学] S859.84[理学—化学]