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    QuEChERS净化-高效液相色谱-串联质谱法测定蜂蜜中农药及抗生素的含量

    Determination of Pesticides and Antibiotics in Honey by QuEChERS-HPLC-MS/MS

    • 摘要: 样品经pH 4.0的Na2EDTA-Mcllvaine缓冲溶液稀释后,用乙酸-乙腈(1+19)混合溶液提取样品中农药及抗生素后,提取液中加入盐析剂分层,上清液放入盛有磁性C18N-丙基乙二胺吸附剂的净化瓶中净化,采用Luna C18色谱柱,以不同体积比的0.1%(体积分数)甲酸溶液和乙腈组成的混合液为流动相进行梯度洗脱。以电喷雾正离子源和多反应监测模式进行质谱分析。30种化合物的质量分数在一定范围内与峰面积呈线性关系,检出限(3S/N)在0.3~4.1 μg·kg-1之间。按标准加入法进行回收试验,回收率在71.1%~116%之间,测定值的相对标准偏差(n=5)在0.80%~21%之间。

       

      Abstract: The sample was diluted with pH 4.0 of Na2EDTA-Mcllvaine buffer solution, and pesticides and antibiotics in the sample were extracted with a mixture of acetic acid-acetonitrile (1+19), and the extract was stratified by salting-out agents. The supernatant was cleaned up with purification pipe filled with magnetic C18 and PSA. Luna C18 column was used as stationary phase, and a mixture of 0.1% (φ) formic acid solution and acetonitrile in various ratios as mobile phase in gradient elution. ESI+ and MRM were adopted in MS. Linear relationships between values of peak area and mass concentration of 30 compounds were found in definite ranges, with detection limits (3S/N) in the range of 0.3-4.1 μg·kg-1. Test for recovery was made by standard addition method, giving results in the range of 71.1%-116%, with RSDs (n=5) ranged from 0.80% to 21%.

       

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