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    超高效液相色谱-串联质谱法测定奶粉中16种苯并咪唑类药物残留量

    UHPLC-MS/MS Determination of Residual Amounts of 16 Benzimidazoles in Milk Powder

    • 摘要: 样品2.000 0 g经0.1 mol·L-1盐酸溶液8 mL、乙腈7 mL超声提取5 min。提取液经活化的MCX固相萃取柱净化。净化液经处理后进行超高效液相色谱分离。以Waters ACQUITY UPLC BEH色谱柱为固定相,以不同体积比的0.02%(体积分数)甲酸溶液和乙腈的混合液为流动相进行梯度洗脱。质谱分析中采用电喷雾正离子源和多反应监测模式。16种苯并咪唑类药物的质量分数在一定范围内与其峰面积呈线性关系,检出限(3S/N)在3.2~4.4 μg·kg-1之间。按标准加入法在3个浓度水平上进行回收试验,回收率在82.0%~108%之间,测定值的相对标准偏差(n=6)均小于9.0%。

       

      Abstract: The sample (2.000 0 g) was extracted ultrasonically for 5 min with 8 mL of 0.1 mol·L-1 hydrochloric acid solution and 7 mL of acetonitrile. The extract was purified on activated MCX solid phase extraction (SPE) column. The purified solution after treatment was separated by UHPLC using Waters ACQUITY UPLC BEH column as the stationary phase, and mixtures of 0.02% (φ) formic acid solution and acetonitrile, mixed in various volumic ratios, as mobile phase in gradient elution. ESI+ and MRM were adopted in MS. Linear relationships between values of peak area and mass fraction of 16 benzimidazoles were found in definite ranges, with detection limits (3S/N) in the range of 3.2-4.4 μg·kg-1. Test for recovery was made by standard addition at 3 concentration levels, giving results in the range of 82.0%-108%, with RSDs (n=6) all less than 9.0%.

       

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