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

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.