超高效液相色谱-串联质谱法结合固相萃取净化测定牛奶中阿苯达唑及其主要代谢物残留量

Determination of Albendazole and Its Main Metabolites in Milk by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry Combined with Solid Phase Extraction Purification

本研究基于超高效液相色谱-串联质谱(UPLC-MS/MS)结合固相萃取净化技术,建立了阿苯达唑(ABZ)、阿苯达唑砜(ABZSN)、阿苯达唑亚砜(ABZSX)的定量分析方法,用以监控牛奶及其制品的质量安全。牛奶样品经过1%乙酸乙腈溶液提取后,提取液经氮气吹干,用碳酸盐缓冲溶液溶解后,使用C_(18)固相萃取柱净化。将净化液注入超高效液相色谱系统,经C18反向色谱柱分离,以可加热电喷雾离子源(H-ESI)正离子扫描模式下多反应监测(MRM),以浓度和峰面积外标法定量。结果表明,3种目标化合物的线性关系良好,相关系数(R^(2))≥0.9987,检出限(LOD)为0.5μg/kg,定量限(LOQ)为2μg/kg,回收率在90.8%~101.2%之间,日内及日间变异系数均≤2.14%。本研究填补了牛奶中ABZ及其代谢物检测方法的空白,实现了牛奶中3种目标化合物的准确定量分析,为牛奶及其制品的质量监测提供了理论和技术支撑。

This study based on ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)combined with solid phase extraction purification technology,established quantitative analysis methods for albendazole(ABZ),albendazole sulfone(ABZSN),and albendazole sulfoxide(ABZSX).Used to monitor the quality and safety of milk and its products.The milk sample was extracted with 1%acetic acid and acetonitrile solution,the extract was blown dry with nitrogen,dissolved in carbonate buffer solution,and purified using a C18 solid phase extraction column.The purified solution was injected into the ultra-high performance liquid chromatography system and separated by C18 reverse chromatographic column,the heating electrospray ion source(H-ESI)is used for multiple reaction monitoring(MRM)in the positive ion scanning mode,and the concentration and peak area external standard method are used for quantification.The results show that the 3 target compounds have a good linear relationship,the correlation coefficient(R^(2))is greater than or equal to 0.9987,the limit of detection(LOD)is 0.5μg/kg,the limit of quantification(LOQ)is 2μg/kg,and the recoveries were between 90.8%~101.2%.The intraday and inter-day coefficient of variation are both no more than 2.14%.This research fills the gap in the detection method of ABZ and its metabolites in milk,and realizes the accurate quantitative analysis of three target compounds in milk,and provides theoretical and technical support for the quality monitoring of milk and its products.