液质联用法测定牛乳中阿苯达唑残留标志物残留量

Determination of AlbendazoleResidual Marker in milk by UPLC-MS/MS

建立超高效液相色谱-串联质谱法测定牛乳中阿苯达唑、阿苯达唑亚砜、阿苯达唑砜和阿苯达唑-2-氨基砜残留量的方法。样品经过乙酸及乙腈溶液提取,以PCX固相萃取柱净化,采用Waters X Bridge BEH C18色谱柱分离,流动相以乙腈和0.1%甲酸水溶液梯度洗脱,并使用电喷雾离子源,正负离子切换扫描模式进行检测,外标法定量。结果表明, 4种兽药残留物在2.0~200 ng/mL范围内呈现良好线性关系,相关系数(R)均大于0.998。4种兽药残留物方法的检出限为0.5μg/kg,方法的定量限为2.0μg/kg。在添加量2.0, 6.0和20μg/kg的加标(n=6)回收试验下, 4种兽药加标回收率为82.5%~112.5%, RSD范围为0.49%~2.02%,日内及日间变异系数为1.72%和2.15%。试验方法前处理操作简便、分析速度快、灵敏度高,填补牛奶中阿苯达唑及其代谢物检测方法的空白,实现牛奶中4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理论和技术支撑。

An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was developed for the determination of albendazole, albendazolesulfoxide, albendazolesulfone and albendazole-2-amino sulfone residues in milk. The samples were extracted with acetic acid and acetonitrile solution, cleaned up by a PCX solid phase extraction column, separated on a Waters X Bridge BEH C18 column with gradient elution of acetonitrile and 0.1% formic acid aqueous solution as mobile phase, and detected by an electrospray ionization source in positive and negative ion switching scanning mode, and quantified by external standard method.Results showed thatthe four veterinary drug residues showed good linearity in the range of 2.0-200 ng/mL with the correlation coefficients(R) greater than 0.998. The limits of detection(LODs) of the method were 0.5 μg/kg and the limits of quantification(LOQs) of the method were 2.0 μg/kg. The recoveries of the four veterinary drug spiked at the spiked levels of 2.0, 6.0 and 20 μg/kg(n=6) were 82.5%-112.5% with the RSD range of 0.49%-2.02% and the intra-day and inter-day coefficients of variation of 1.72% and 2.15%. The method was simple, fast and sensitive.This study filled the gap of the method for the determination of ABZ and its metabolites in milk and achieves the accurate quantitative analysis of the four target compounds in milk, which provided theoretical and technical support for the quality monitoring of milk and its products.