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    高效液相色谱-串联质谱法同时测定乳制品中莫奈太尔和莫奈太尔砜

    Simultaneous Determination of Monepantel and Monepantel Sulfone in Dairy Products by HPLC-MS/MS

    • 摘要: 采用高效液相色谱-串联质谱法同时测定乳制品(奶粉或液态奶)中莫奈太尔和莫奈太尔砜的含量。奶粉样品(约0.5 g)加2 mL水涡旋振荡至溶解完全,上述奶粉样品溶液或约2 mL的液态奶样品,经5 mL饱和氯化钠溶液、18 mL乙腈超声提取,提取液浓缩后经正己烷净化。以Inertsil C8-3色谱柱为分离柱,以不同体积比的0.5 mmol·L-1乙酸铵溶液和甲醇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负离子源和多反应监测模式。莫奈太尔和莫奈太尔砜的质量浓度均在5.0 μg·L-1以内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.008~0.018 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79.5%~104%,测定值的相对标准偏差(n=6)为2.8%~5.9%。

       

      Abstract: HPLC-MS/MS was applied to the simultaneous determination of monepantel and monepantel sulfone in dairy products (milk powder or liquid milk). The milk powder sample (about 0.5 g) was vortexed to dissolve completely in 2 mL of water. The above milk powder sample solution or about 2 mL of liquid milk sample was extracted ultrasonically with saturated sodium chloride solution (5 mL) and 18 mL of acetonitrile. After concentration, the extract was purified with n-hexane. Inertsil C8-3 chromatographic column was used as stationary phase, and the mixture of 0.5 mmol·L-1 ammonium acetate solution and methanol mixed in different ratios was used as mobile phase in gradient elution. ESI- and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of monepantel and monepantel sulfone were kept in the same range within 5.0 μg·L-1, with detection limits (3S/N) in the range of 0.008-0.018 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 79.5%-104%, with RSDs (n=6) in the range of 2.8%-5.9%.

       

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