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目的建立生食水产品中7种磺胺类药物残留的液相色谱-串联质谱(LC-MS/MS)检测方法,包括磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲嘧啶、磺胺间甲氧嘧啶、磺胺对甲氧嘧啶、磺胺噻唑、磺胺多辛。方法试样中加入C18填料后研磨均匀,磺胺类药物用乙腈-水在微波辐照辅助下进行提取,用乙腈饱和的正己烷液分配净化,用LC-MS/MS法测定。使用电喷雾离子化源(ESI),在正离子条件下以选择离子监测(SRM)方式进行扫描,外标法定量。结果该法线性范围为10～100μg/kg,以加标样品计算,在各浓度水平下各被测物的方法回收率均为70%～100%,各被测物的检出限为3μg/kg。结论该法灵敏、快速、准确,可用于生食水产品中磺胺类药物残留的检测。
Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of seven sulfonamides residues in raw aquatic products, including sulfadiazine, sulfamerazine, sulfamethazine, sulfamonomethoxine, Methoxypyrimidine, sulfathiazole, sulfadoxine. Methods The samples were homogenized by adding C18 filler. The sulfonamides were extracted with acetonitrile-water with the aid of microwave irradiation. The sulfonamides were purified by acetonitrile-saturated n-hexane solution and determined by LC-MS / MS. Electrospray ionization (ESI) was used to scan in positive ion selective ion monitoring (SRM) mode and quantified by external standard method. Results The linear range of this method was 10 ~ 100μg / kg. The spiked samples were calculated by spiked samples. The recoveries were 70% -100% at all concentration levels. The detection limit of each test substance was 3μg / kg. Conclusion The method is sensitive, rapid and accurate and can be used for the detection of sulfonamides residues in raw aquatic products.