HPLC-MS/MS法测定猪肉和鸡肉中12种磺胺残留

Determination of 12 Sulfonamides Residue in Pork and Chicken by HPLC-MS/MS

采用高效液相色谱串联质谱(HPLC-MS/MS)法同时测定猪肉、鸡肉中磺胺类药物残留。猪肉、鸡肉样品中的磺胺类药物残留用乙腈提取,均质离心后,上清液用旋转蒸发器蒸发浓缩至近干,残渣用流动相(乙腈和0.01mol/L的乙酸铵溶液, 12+88)溶解,并用正乙烷去脂,样品溶液供液相色谱串联质谱仪测定,以外标法定量,采用多反应监测方式和正离子扫描方式测定。结果表明:12种磺胺类药物在10~200 ng/mL范围内线性关系良好,相关系数r高于0.997 3,检出限为2μg/kg,定量限为10μg/kg;猪肉和鸡肉空白样品中12种磺胺药物3个加标水平(2, 8和20μg/kg)的平均回收率分别为94.2%~133.4%和89.1%~112.2%, RSD分别为2.07%~6.11%和2.46%~5.87%。猪肉和鸡肉中磺胺嘧啶易被检出,其次是磺胺甲氧哒嗪、磺胺对甲氧嘧啶、磺胺-6-甲氧嘧啶。该方法操作简便、灵敏度高,适用于猪肉、鸡肉中12种磺胺类药物残留的测定。

A method of simultaneous determination of sulfonamides residues in pork and chicken by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was adopted. Pork and chicken sulfonamides residues in the samples were extracted with acetonitrile and homogeneous after centrifugal supernatant fluid with a rotary evaporator to concentrate almost dry. The residue was dissolved with mobile phase(acetonitrile and 0.01 mol/L ammonium acetate solution, 12+88) and defatted by ethane. The sample solution was determined through high performance liquid chromatography-tandem mass spectrometry using external standard method, quantitative multiple reaction monitoring mode and positive ion scanning mode. The results showed that the 12 kinds of sulfa drugs exhibited good linear relationships in the range of 10-200 ng/mL with correlation coefficients(r) of more than 0.997 3. The limits of detection and quantification for 12 kinds of sulfa drugs were 2 μg/kg and 10 μg/kg, respectively. Pork and chicken spiked in 2, 8 and 20 μg/kg had recoveries of 94.2%-133.4% and 89.1%-112.2% with a relative standard deviation of 2.07%-6.11% and 2.46%-5.87%. Sulfonamides were detected easily in the 12 kinds of sulfa drugs from pork and chicken, followed by sulfamethoxypyridazine, sulfamethoxazine and sulfamethoxypyrimidine. The method was simple, easy, sensitive and suitable for determination of 12 kinds of sulfa drugs in pork and chicken.