利用气液微萃取技术联用气相色谱-质谱法检测谷类中27种残留农药
利用气液微萃取技术联用气相色谱-质谱法检测谷类中27种残留农药
目的建立气液微萃取技术(gas-liquid microextraction, GLME)联用气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)快速检测谷类中的27种农药残留的方法。方法精确称量0.5 g谷类样品, 用0.5 mL二氯甲烷溶剂超声萃取15 min, 离心4 min后取上清液100 μL, 利用气液微萃取(GLME)对27种农残萃取、净化和浓缩, 结合内标法确保结果的准确性。结果27种农药在0.001~1.0 mg/kg浓度范围内线性良好, 相关系数在0.9990~0.9999, 检出限为0.002~0.026 mg/kg, 定量限为0.0007~0.086 mg/kg, 平均回收率为71.2%~124.4%(n=3), 相对标准偏差在0.2%~18.8%之间。结论本方法操作简便方便、准确度高、重现性好, 适用于食品安全现场检测和快速检测, 对于保障我国食品安全构建完整的食品安全检测体系具有重大意义。
ObjectiveTo establish a method for rapid detection of various pesticides in cereal grains by gas-liquid microextraction (GLME) and gas chromatography-mass spectrometry (GC-MS). MethodsThe 0.5 g cereal sample was accurately weighed and extracted with 0.5 mL dichloromethane solvent for 15 min, after 4 min centrifugation, 100 μL supernatant was taken and 27 kinds of residues were extracted, purified and concentrated by gas-liquid microextraction (GLME). The accuracy of the results was ensured by the internal standard method. ResultsThe 27 kinds of pesticide had good linear relationships in the range of 0.001?1.0 mg/kg, and the correlation coefficients were 0.9990?0.9999. The limits of detection were 0.002?0.026 mg/kg and the limits of quantitation were 0.0007?0.086 mg/kg. The average recoveries were 71.2%?124.4% (n=3) with relative standard deviations of 0.2%?18.8%. ConclusionThis method is simple and rapid, with high accuracy and good repeatability, which is suitable for rapid analysis or field-detection in the food safety industry. It is of great significance to build a complete food safety inspection system to ensure China's food safety.
标题：利用气液微萃取技术联用气相色谱-质谱法检测谷类中27种残留农药
英文标题：Determination of 27 pesticides residues in grains by gas-liquid microextraction combined with gas chromatography-mass spectrometry
作者：
郭子钰 延边大学化学系,长白山生物资源与功能分子教育部重点实验室
李婉莹 延边大学化学系,长白山生物资源与功能分子教育部重点实验室
高汉勇 延边大学化学系,长白山生物资源与功能分子教育部重点实验室
金香子 延边大学化学系,长白山生物资源与功能分子教育部重点实验室
蒋世翠 长白山生物资源与功能分子教育部重点实验室
李东浩 延边大学化学系,长白山生物资源与功能分子教育部重点实验室
中文关键词:农药残留,谷类,气液微萃取,气相色谱-质谱法,快速检测,
英文关键词:pesticide residue,grain,gas-liquid microextraction,gas chromatography-mass spectrometry,rapid determination,
发表日期：2019-04-14
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