超高效液相色谱-串联质谱法测定乳制品中苯并咪唑类药物及其代谢物的残留量

UHPLC-MS/MS Determination of Residual Amounts of Benzimidazoles and Its Metabolites in Dairy Products

乳制品样品中加入水、乙腈、氯化钠提取,采用乙腈饱和的正己烷脱脂净化。采用超高效液相色谱-串联质谱法测定样品溶液中苯并咪唑类药物及其代谢物的残留量。以Atlantis T3色谱柱为固定相,以不同体积比的0.1%(体积分数,下同)甲酸乙腈溶液和0.1%甲酸溶液的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾离子源(正离子扫描)和可编辑多反应监测模式。采用同位素内标法定量,苯并咪唑类药物及其代谢物的线性范围均为0.02~5.0μg·L^-1,检出限(3S/N)为0.010~1.0μg·kg^-1,测定下限(10S/N)为0.025~4.0μg·kg^-1。以空白样品为基体进行加标回收试验,所得回收率为81.4%~108%,测定值的相对标准偏差(n=6)为0.40%~9.3%。

The dairy product sample was extracted with water,acetonitrile and NaCl.n-Hexane saturated with acetonitrile was used for de-fat and purification.UHPLC-MS/MS was applied to the determination of residual amounts of benzimidazoles and its metabolites in the sample solution.Atlantis T3 chromatographic column was used as stationary phase,and the mixture of 0.1%(φ,the same below)formic acid acetonitrile solution and 0.1%formic acid solution mixed in different ratios was used as mobile phase in gradient elution.ESI+and scheduled multireactions monitor mode were adopted in MS/MS.Isotope was used as internal standard.Linearity ranges of benzimidazoles and its metabolites were found in the same range of 0.02-5.0μg·L^-1,with detection limits(3 S/N)in the range of 0.010-1.0μg·kg^-1 and lower limits of determination(10 S/N)in the range of 0.025-4.0μg·kg^-1.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 81.4%-108%,with RSDs(n=6)of determined values in the range of 0.40%-9.3%.