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    凝胶渗透色谱-超高效液相色谱-串联质谱法测定水产品中多种同化激素残留

    Determination of Anabolic Steroid Residue in Aquatic Products by GPC-UHPLC-MS/MS

    • 摘要: 结合凝胶渗透色谱净化技术,建立了超高效液相色谱-串联质谱法测定水产品中6种同化激素的残留。样品经叔丁基甲醚提取,以乙酸乙酯-环己烷(1+1)溶液为流动相进行凝胶渗透色谱净化,用C18固体吸附剂净化,以C18色谱柱分离,采用电喷雾正离子源、多反应监测模式检测,外标法定量。6种激素的线性范围均为0.5~50 μg·L-1,测定下限(10S/N)在0.20~1.50 μg·kg-1之间。对空白样品进行加标回收试验,回收率在81.7%~90.8%之间,日间精密度(n=5)在5.8%~7.9%之间。

       

      Abstract: A method for determination of anabolic steroid residues in aquatic products was developed using ultra performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) combined with gel permeation chromatography (GPC). The sample was extracted with tert-butyl methyl ether, then purified by GPC with ethyl acetate-cyclohexane (1+1) solution as mobile phase, and re-purified by C18 adsorbent. The supernatant was seperated by C18 column and determined by MS/MS. ESI+ and MRM were adopted in MS/MS. External standard method was used for quantification. Linearity ranges of 6 kinds of anabolic steroid were found in the same range of 0.5-50 μg·L-1, with lower limits of determination of 0.20-1.50 μg·kg-1. Recovery measured by standard addition method was in the range of 81.7%-90.8% with inter-day precision (n=5) in the range of 5.8%-7.9%.

       

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