液相色谱-串联质谱法同时测定畜禽肉中8种磺胺类药物残留量  

LC-MS/MS for the determination of sulfonamide residues in animal meat

作　　者：陆川[1] 张鲁南[2] 吴亚利[1] 秦峰[3] 马又娥[4] 杜玥[3] 贾晶莹[1] 刘罡一[1] 余琛[1] 

机构地区：[1]上海市徐汇区中心医院,上海200031 [2]上海市徐汇区疾病预防控制中心,上海200031 [3]上海市食品药品检验所,上海201203 [4]上海市农药研究所,上海200032

出　　处：《药物分析杂志》2009年第9期1479-1484,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立液相色谱-串联质谱法(LC-MS/MS)同时测定家禽和家畜肉中8种磺胺类药物(磺胺二甲氧基嘧啶、磺胺二甲嘧啶、磺胺甲基嘧啶、磺胺甲氧嘧啶、磺胺甲基异噁唑、磺胺吡啶、磺胺二甲异嘧啶、磺胺异噁唑)残留量。方法:以依普沙坦为内标,肉类样品匀浆后经乙腈沉淀提取,提取液加水稀释后,采用反相色谱法分离、电喷雾正离子模式下多反应监测定量分析。结果:线性范围为10～300ng·g-1(r>0.99),最低定量限为10ng·g-1(S/N≥10),准确度为86.0%～108.9%;批内和批间精密度均小于10%。结论:本方法操作简便,特异性强,灵敏度高,取样量少,符合生物样品的分析要求,可以用于肉类食品中的磺胺类药物多残留分析。Objective：To establish an LC -MS/MS method to simultaneously determine 8 sulfonamides （sulfadim- ethoxin, sulfadimidin, sulfamerazin, sulfameter, suifamethoxazole, sulfapyridine, sulfasomidin, sulfisoxazole） residues in meat. Methods：By adding eprosartan as internal standard, homogenized meat sample was deproteinated with ace- tonitrile. The analysis was performed in reverse phase liquid chromatography and detected in multiple reaction monitoring mode. Results：In this method, the determination was not effected by endogenous compounds; RSDs of intra - and inter- assay were lower than 10%, LLOQ was 10 ng · g-1（S/N≥ 10）; Relative recovery of sulfonamide was 86. 0% -108.9%; Calibrations between 10 -300 ng · g-1 exhibited consistent linearity and reproducibility. Conclusion：With a simple sample pretreatment, specific and cost - effective assay, the proposed LC - MS/MS method is suitable for sulfonamide residues analysis in meat.

关 键 词：液相色谱/串联质谱法 磺胺类 肉 残留量 

分 类 号：R917[医药卫生—药物分析学]