液相色谱-串联质谱法快速检测大米中的15种农药残留
液相色谱-串联质谱法快速检测大米中的15种农药残留
目的建立液相色谱-串联质谱法快速检测大米中15种代表性农药残留的分析方法。方法大米样品经水溶胀后以乙腈提取, 利用QuEChERS法进行净化。采用0.02%甲酸+2 mmol/L甲酸铵(A)和甲醇(B)作为流动相进行梯度洗脱, 采用多离子监测模式对农药多残留进行检测。结果在9.5 min内完成15种目标农药残留的分离分析。在0.010、0.10和0.50 mg/kg 3个添加水平的回收率为70.2%~110.0%, 相对标准偏差为1.3%~14.5%(n=3); 方法定量限为0.010 mg/kg、检出限为0.2~1.0 μg/kg。结论该方法简便、快速、准确、实用, 适合测定大米样品中的农药残留。
ObjectiveTo establish a method for rapid determination of 15 kinds of representative pesticide residues in rice by liquid chromatography-tandem mass spectrometry. MethodsThe rice sample was swollen with water and extracted with acetonitrile before purified by the QuEChERS method. The gradient elution was performed using 0.02% formic acid + 2 mmol/L ammonium formate (A) and methanol (B) as the mobile phase, and the multi-residue pesticide was detected by multi-ion monitoring mode. ResultsThe separation and analysis of 15 kinds of target pesticide residues were completed within 9.5 min. The recoveries at 3 spiked levels (0.010, 0.10 and 0.50 mg/kg) were 70.2%?110.0%, with the relative standard deviations of 1.3%?14.5% (n=3). The limits of quantitation were 0.010 mg/kg and the limits of detection were 0.2-1.0 μg/kg. ConclusionThe proposed method is simple, fast, accurate and practical, which is suitable for the determination of pesticide residues in rice samples.
标题：液相色谱-串联质谱法快速检测大米中的15种农药残留
英文标题：Rapid determination of 15 kinds of pesticide residues in rice by liquid chromatography-tandem mass spectrometry
作者：
黄健祥 广东省农业科学院农产品公共监测中心；国家农业检测基准实验室(农药残留)；农业农村部农产品质量安全检测与评价重点实验室
陈炎 广东省农业科学院农产品公共监测中心；国家农业检测基准实验室(农药残留)；农业农村部农产品质量安全检测与评价重点实验室
谢书越 广东省农业科学院农产品公共监测中心；国家农业检测基准实验室(农药残留)；农业农村部农产品质量安全检测与评价重点实验室
万凯 广东省农业科学院农产品公共监测中心；国家农业检测基准实验室(农药残留)；农业农村部农产品质量安全检测与评价重点实验室
中文关键词:液相色谱-串联质谱法,大米,农药残留,
英文关键词:liquid chromatography-tandem mass spectrometry,rice,pesticide residue,
发表日期：2019-04-15
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