液相色谱-串联质谱法测定猪肉中咪唑类药物及其代谢物

建立了高效液相色谱-串联质谱同时测定猪肉中29种咪唑类药物及其代谢物残留的检测方法。样品采用乙酸乙酯提取,浓缩复溶后加入乙腈饱和正己烷净化除脂,以0.3%(体积分数)甲酸水溶液和乙腈为流动相,反相C_(18)色谱柱梯度洗脱分离,采用电喷雾正离子(ESI+)源多反应监测(MRM)模式进行检测。29种化合物在0.05~20.0μg/L范围内线性关系良好,相关系数r~20.99。在1.0~5.0μg/kg添加范围内,平均回收率为65.4%~103%,相对标准偏差(RSD)为1.3%~6.8%。方法检出限为0.02~0.3μg/kg,定量限为0.1~1μg/kg。该方法简便、快速、灵敏,适用于猪肉中咪唑类及其代谢物残留的检测。

Determination of imidazoles and their metabolites in pork by liquid chromatography-tandem mass spectrometry

A method for the determination of 29 imidazoles and their metabolites in pork by liquid chromatography-tandem mass spectrometry has been developed. The samples were extracted with ethyl acetate, and then defatted with n-hexane after concentration of the extracts. The analytes were separated on a C₁₈ reversed-phase column with 0.3% (v/v) formic acid aqueous solution and acetonitrile as mobile phases, and finally analyzed using electrospray ionization in positive ion mode (ESI⁺) with multiple reaction monitoring (MRM). The linear ranges of the 29 compounds were from 0.05 to 20.0 μg/L with the correlation coefficients (r²) more than 0.99. The average recoveries and relative standard deviations were 65.4%-103% and 1.3%-6.8% respectively in the spiked ranges of 1.0-5.0 μg/kg. The limits of detection and the limits of quantification were 0.02-0.3 μg/kg and 0.1-1 μg/kg respectively for the 29 imidazoles. The method is simple, rapid and sensitive. It is suitable for the detection of imidazoles and their metabolites in pork.