超高效液相色谱-串联质谱法测定草鱼肉中阿苯达唑及其代谢物残留

Determination of Albendzole and Its Metabolites in Grass Carp Meat by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了同时测定草鱼肉中阿苯达唑及其3种代谢物阿苯达唑亚砜、阿苯达唑砜、阿苯达唑-2-氨基砜的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。草鱼肉样品通过碱性乙酸乙酯提取,正己烷净化,超高效液相色谱分离,串联质谱检测,氘代同位素内标定量。本方法分析时间短,在4 min内即可完成4种被分析物的液质联用分析。本方法在0.1～10μg/kg范围内各物质线性良好,线性系数在0.9991～0.9996之间。阿苯达唑、阿苯达唑亚砜、阿苯达唑砜、阿苯达唑-2-氨基砜在0.5～5.0μg/kg添加水平下的平均回收率分别为98.4%～102.6%,97.1%～103.4%,98.8%～103.7%和101.1%～104.2%检出限分别为0.2,0.1,0.2和0.1μg/kg;日内精密度小于4.77%,日间精密度小于3.03%。本方法为阿苯达唑及其代谢物的检测及监控提供了一种快速、灵敏度高、重现性好的定量分析方法。

A method of ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） has been developed for the determination of albendzole（ABZ） and its metabolites,albendazole sulfoxide （ABZSO）,albendazole sulfone（ABZSO2） and albendazole aminosulfone（ABZ-2-NH2SO2） in grass carp meat.The samples were extracted with alkaline ethyl acetate and cleaned up by n-hexane.Chromatographic separation was achieved by UPLC and the detection was performed by tandem mass spectrometry using deuterated isotope internal standard.The UPLC-MS/MS analysis was rapid and can be achieved in less than 4 min. In the range of 0.1-10 μg/kg,the analytes were in good linearity,and the correlation coefficients were 0. 9991-0.9996.The recoveries of ABZ,ABZSO,ABZSO2 and ABZ-2-NH2SO2 spiked at levels of 0.5-5.0 μ g/kg,were 98.4%-102.6%,97.1%-103.4%,98.8%-103.7%,101.1%-104.2%,the limit of quantity（LOQ） were 0.2,0.1,0.2,0.1 μg/kg,respectively.The Intra-day RSD were less than 4.8%, and Inter-day RSD was less than 3.0%.The UHPLC-MS/MS method is rapid,sensitive,reproducible and suitable for the determination of ABZ and its metabolites