气相色谱-三重四极杆质谱法测定黄芪中42种农药残留

Determination of 42 kinds of pesticide residues in Astragalus membranaceus by gas chromatography-triple quadrupole mass spectrometry

中文关键词:  PTV  三重四级杆气质联用仪  农药残留  黄芪

英文关键词:gas chromatography-triple quadrupole mass spectrometry  pesticide residues  Astragalus membranaceus

中文摘要:

      目的 建立气相色谱-三重四极杆质谱法测定黄芪中42种农药的方法。方法 黄芪中的多组分农药采用乙腈提取, 上清液经N-丙基乙二胺、十八烷基硅烷键合硅胶、硅胶净化, 采用程序升温进样口上机测定, 基质匹配曲线外标法定量。结果 42种农药在0.01~1.00 μg/mL范围内线性关系良好, 相关系数为0.9954~0.9999, 在空白基质中添加低(0.02 mg/kg)、中(0.40 mg/kg)、高(2.00 mg/kg)3个不同浓度的混合标准品各6份, 加标回收率为72.5%~109.3%, 相对标准偏差为1.25%~6.07%, 检出限为0.002~0.010 mg/kg, 定量限为0.005~0.030 mg/kg。在100批次黄芪样本中检出6种农药, 分别是α-硫丹、对硫磷、甲基对硫磷、硫环磷、氯氰菊酯、氰戊菊酯, 样品检出率6.0%, 样品超标率1.0%, 超标农药为氯氰菊酯。结论 本方法灵敏度高、准确性好, 适用于黄芪中42种农药的同时测定。

英文摘要:

      Objective To establish a gas chromatography-triple quadrupole mass spectrometry method for the determination of 42 kinds of pesticides in Astragalus membranaceus. Methods The multi-component pesticides in Astragalus membranaceus were extracted by acetonitrile. and the supernatant was purified by N-propyl ethylenediamine, octadecylsilane bonded silica gel and silica gel. The samples were determined by temperature program injection nozzle, and quantified by matrix matching curve external standard method. Results The 42 pesticides had a good linear relationship in the range of 0.01-1.00 μg/mL, and the correlation coefficient was 0.9954-0.9999. Three mixed standards of low (0.02 mg/kg), medium (0.40 mg/kg) and high (2.00 mg/kg) concentrations were added to the blank matrix, each with 6 samples, the recovery was 72.5%-109.3%, the relative standard deviation was 1.25%-6.07%, the detection limit was 0.002~0.010 mg/kg and the quantitation limit of the method was 0.005-0.030 mg/kg. In 100 batches of radix astragali, six kinds of pesticides were detected, namely α-endosulfan, parathion, methyl parathion, cyclophosphamide, cypermethrin, fenvalerate, with a detection rate of 6.0%. The sample exceeded the standard rate was 1.0%, and the excessive pesticide was cypermethrin. Conclusion The method has high sensitivity and accuracy, and is suitable for the simultaneous determination of 42 kinds of pesticides in Astragalus membranaceus.