QuEChERS-气相色谱-串联质谱法测定蜂蜜中20种农药残留

Determination of 20 kinds of pesticide residues in honey by QuEChERS-gas chromatography-tandem mass spectrometry

目的建立QuEChERS法与气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)联用快速检测蜂蜜中20种农残的分析方法。方法样品用乙腈快速提取、无水硫酸镁与乙酸钠盐析,经无水硫酸镁、N-丙基乙二胺(N-propyl ethylenediamine,PSA)和C18净化后,用GC-MS/MS分析。质谱采用多反应监测模式(multiple reation monitoring, MRM),保留时间和特征离子定性,外标法定量。结果结果表明20种农药在10~400 ng/mL范围内线性良好,相关系数≥0.99,检出限为0.003~0.082μg/kg,相对标准差(n=6)为3.9%~10.6%,当样品的加标水平为40、100和200μg/kg时,除伏杀硫磷、高效氯氟氰菊酯和溴氰菊酯的回收率偏高,其他17种农药各浓度回收率为83.16%~119.88%。结论该方法操作简单,适用于蜂蜜中多种农药残留的快速检测。

Objective To establish a method for simultaneous determination of 20 kinds of pesticide residues in honey by QuEChERS-gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods Honey samples were extracted into acetonitrile and salted out by anhydrous MgSO4 and sodium acetate, then cleaned up using the mixture of anhydrous MgSO4, N-propyl ethylenediamine (PSA) and C18 powder as sorbents, and detected by GC-MS/MS using multiple reaction monitoring mode. And samples was qualitied by chromatographic retention time and characteristic parent ion, and then quantified with external standard. Results The 20 pesticides had good linear relationships in the range of 10-400 ng/mL, and the correlation coefficients were not less than 0.99, the limits of detection(RS/N=3) were in the range of 0.003-0.082 μg/kg, with the relative standard deviations of 3.9%-10.6%(n=6), the recoveries of the 17 pesticides at 3 spiked levels of 40, 100 and 200 μg/kg were 83.16%-119.88% except phosalone, lambda-cyhalothrin and deltamethrin. Conclusion This method is simple, which is suitable for rapid detection of pesticide residues in honey.