固相萃取串联高效液相色谱检测动物源性食品中甲巯咪唑残留

Detection of methimazole residue in animal-derived foods by combining solidphase extraction with high performance liquid chromatography

以动物源性食品中抗甲亢药物甲巯咪唑为研究对象,采用Cleanert S C18固相萃取柱对复杂动物源性食品进行基质净化,对上样溶剂、洗杂液、洗脱液等试验参数进行优化,建立固相萃取净化富集与高效液相色谱联用技术,实现对猪肾、猪肝、猪肉样品中的痕量甲巯咪唑准确、灵敏检测。在最优试验条件下,在3个添加浓度的猪肾、猪肝、猪肉样品中,分析物甲巯咪唑的回收率均大于85%,相对标准偏差(RSD,n=3)均小于5%,对3种样品中最低检出限(S/N=3)和最低定量限(S/N=10)分别为:猪肾0.59,1.97μg/kg;猪肝0.54,1.80μg/kg;猪肉0.49,1.63μg/kg。所建立的检测方法具有较高的准确度和灵敏度,可以满足对实际样品中甲巯咪唑的分析检测。

The residue of antithyroid drug-methimazole in animal-derived food products was studied.The complex matrix of food products was purified by using Cleanert S C18solid-phase extraction column and the experimental parameters including the loading solvent,washing solution and the eluent were optimized in detail.The method for the accurate and sensitive detection of trace methimazole in pig kidney,liver and muscle samples was successfully developed by combining solid-phase extraction with high performance liquid chromatography.Under the optimized experimental conditions,good recoveries（〉85%）were obtained at three spiked concentrations in chosen animal-derived samples with RSD less than 5%（n=3）.The limit of detection（S/N=3）and limit of quantitation（S/N=10）achieved to0.59μg/kg and 1.97μg/kg（kidney）,0.54μg/kg and 1.8μg/kg（liver）,0.49μg/kg and 1.63μg/kg（muscle）,respectively,which validated that the developed method with high accuracy and sensitivity could meet the requirement of methimazole detection in real samples.