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    全自动固相萃取-高效液相色谱-串联质谱法测定豆芽中15种喹诺酮类药物的残留量

    HPLC-MS/MS Determination of Residual Amounts of 15 Quinolones in Bean Sprouts with Automated Solid Phase Extraction

    • 摘要: 豆芽样品采用pH 4.0的乙二胺四乙酸二钠-Mcllvaine缓冲溶液提取,采用MCX固相萃取柱进行在线净化。采用高效液相色谱-串联质谱法测定样品溶液中15种喹诺酮类药物的残留量。以Waters BEH C18色谱柱为固定相,以不同体积比的0.2%(体积分数,下同)甲酸溶液和0.2%甲酸乙腈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电离源正离子模式和多反应监测模式。15种喹诺酮类药物的质量浓度均在5~120 μg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为2 μg·kg-1,测定下限(10S/N)为6 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62.0%~89.3%,测定值的相对标准偏差(n=6)为2.4%~11%。

       

      Abstract: The bean sprout sample was extracted with EDTA-mcllvaine buffer solution of pH 4.0. MCX solid phase extraction column was used as on-line purification. HPLC-MS/MS was applied to the determination of residual amounts of 15 quinolones in the sample solution. Waters BEH C18 chromatographic column was used as stationary phase, and the mixture of 0.2% (φ, the same below) formic acid solution and 0.2% formic acid acetonitrile solution 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 15 quinolones were kept in the same range of 5-120 μg·L-1, with detection limits (3S/N) of 2 μg·kg-1 and lower limits of determination (10S/N) of 6 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 62.0%-89.3%, with RSDs (n=6) of determined values in the range of 2.4%-11%.

       

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