动物源性食品中磺胺类药物增效剂残留的高效液相色谱-串联质谱法测定

利用高效液相色谱-电喷雾串联质谱测定了蜂蜜、蜂王浆、鮰鱼、鳗鱼、猪肉、猪肾、猪肝、鸡肉、牛肉和牛奶中的三甲氧苄氨嘧啶、二甲氧苄氨嘧啶和奥美普林3种磺胺类药物增效剂.除蜂王浆基质直接用10%三氯乙酸溶液提取外,其余基质均用10%三氯乙酸-乙腈(体积比7 : 3)混合溶液提取,提取溶液过阳离子交换固相萃取柱进行富集和净化.采用C18色谱柱,流动相为甲醇和0.1%甲酸溶液.选择1个母离子和2个子离子进行反应监测,对3种磺胺类药物增效剂残留进行定性,选择信号最强的子离子进行定量.在2 ～100 μg/L范围内,分析物的线性相关系数r>0.992.通过实际样品添加回收实验,所有基质定量下限为5.0 μg/kg,3个添加水平的回收率为63% ～89%,相对标准偏差为3.2% ～6.9%.

Determination of Sulfonamides Potentiator Residues in Animal Origin Foods by High Performance Liquid Chromatography-Tandem Mass Spectrometry

A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was developed for determination of three potentiators,e.g.trimethoprim(TMP),diaveridine(DVD) and ormetoprim(OMP) in honey,royal jelly,catfish,eel,pork,porcine kidney,porcine liver,chicken,beef and milk samples.Except that the royal jelly samples was directly extracted by 10%trichloroacetic acid solution,other matrices samples were extracted by 10%trichloroacetic acid-acetonitrile(7 : 3,by volume).The extracts were concentrated and purified by cation-exchange solid phase extraction cartridge.The separation of analytes was performed on C18 analytical chromatographic column with a gradient elution using methanol(A) and 0.1%formic acid(B) solution as mobile phase.The analysis of three potentiators were performed under selective reaction monitoring(SRM) mode by selecting one parent ion and two daughter ions as qualitative ions,and the most abundant daughter ion as a quantitative ion.The calibration curves of three potentiators were linear in the concentration range of 2-100 μg/L with correlation coefficients more than 0.992.The quantitative limits of the method were 5 μg/kg for all matrices,and the spiked recoveries were in the range of 63%-89%with RSDs of 3.2%-6.9%.