液相色谱串联质谱法测定鸡肉中20种抗球虫药物多残留

建立了鸡肉中盐霉素、甲基盐霉素、莫能菌素、拉沙里菌素、马杜拉霉素、氯羟吡啶、氨丙啉、乙氧酰胺苯甲酯、4,4-二硝基均二苯脲、常山酮、克拉珠利、甲苄喹啉、癸氧喹酯、二硝托胺、地克珠利、硝米特、甲苯三嗪酮、甲苯三嗪酮砜、甲苯三嗪酮亚砜及阿克洛胺等20种抗球虫药物的定量测定方法.用乙腈萃取鸡肉中的抗球虫类药物残留,乙腈饱和正己烷脱脂,硅胶柱净化,浓缩,以Acquity BEH C18色谱柱为分离柱,液相色谱串联质谱仪测定,正/负离子分段扫描.测定限为0.005～0.05 mg/kg,在3个添加水平上进行回收实验,平均回收率为84.8％～105.0％；相对标准偏差为1.5％～10.6％.本方法简便、快速、准确,各项技术指标满足国内外法规的要求,可用于鸡肉样品中抗球虫类药物多残留的定量测定.

Simultaneous Determination of 20 Coccidiostat Residues in Chicken by Liquid Chromatography-Tandem Mass Spectrometry

A quantitative method was developed with high performance liquid chromatography tandem mass spectrometry(LC-MS/MS) to determine 20 residues of coccodiostats in chicken,which include salinomycin,narasin,monensin,lasalocid,maduramicin,clopidol,amprolium,ethopabate,dinitrocarbanilide,halofuginone,clazuril,nequinate,decoquinate,zoalene,diclazuril,nitromide,toltrazuril,toltrazuril sulfone,toltrazuril sulfoxide,and aklomide.In this method,the 20 coccidiostat residues were extracted with acetonitrile,after degreased by hexane which was saturated with acetonitrile,the extract was cleaned with silica SPE column.Then the condensed sample solution was analyzed by LC-MS/MS in positive/negative ion mode,with Aquity BEH C18 column as the separation column.The method was validated at three levels.The average recovery varies from 84.8% to 105%,and the relative standard deviation(RSD) is between 1.5% and 10.6%.The LOQ is between 0.005-0.05 mg/kg.The method is simple,rapid,and accurate,and its performance can meet the requirements of the domestic and international legislation.The described method was proved suitable for simultaneous determine coccidiostats residues in chicken.