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    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

    • 摘要: 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0.02~5.0 μg·L-1,检出限(3S/N)为0.010~1.0 μg·kg-1,测定下限(10S/N)为0.025~4.0 μg·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%。

       

      Abstract: 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 multi-reactions 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 0.02-5.0 μg·L-1, with detection limits (3S/N) in the range of 0.010-1.0 μg·kg-1 and lower limits of determination (10S/N) in the range of 0.025-4.0 μg·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%.

       

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