目的 建立 QuEChERS 方法和气相色谱-三重四极杆串联质谱(gas chromatography-tandem mass spectrometry, GC-MS/MS)联用技术快速检测大米、韭菜、茶叶中51种不同农药残留量的方法.方法 利用乙腈提取样品, 分散固相萃取法净化样品, GC-MS/MS 检测采用选择多反应监测(multiple reaction monitoring, MRM), 灵敏度最高的离子对用作定量.结果 51种农药在20~1500 ng/mL范围内呈现良好的线性关系, 相关系数(r2)大于0.99, 各农药检出限(S/N≥3)为0.0005~0.02 mg/kg, 除双甲脒回收率在14.61%~35.56%外, 其他农残在3个浓度添加水平上的加标回收率范围为51.5%~129%, 相对标准偏差(relative standard deviation, RSD, n=6)范围为0.79%~15.23%.结论 该方法灵敏度高,准确性好,快速简便,适用于大米、韭菜、茶叶中51种农药残留量的快速测定和验证.%Objective To establish a method for rapid determination of 51 kinds of pesticides residues in rice, garlic chives and tea by QuEChERS coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The samples were extracted by acetonitrile, cleaned up with dispersive solid phase extraction method and detected by GC-MS/MS with multiple reaction monitoring (MRM) mode, and the most sensitive ion pairs were selected for quantification. Results The linear relationships between peak area ratio and concentration ratio of 51 kinds of pesticides and internal standard were good from 20 ng/mL to 1500 ng/mL (r2>0.99). The limits of detection (S/N≥3) of 51 kinds of pesticides in the spiked blank samples were 0.0005-0.02 mg/kg. The recovery rates of amitraz were from 14.61% to 35.56%, and recoveries of other pesticides at the 3 levels were ranged from 51.5% to 129%. The relative standard deviations (RSD, n=6) were 0.79%-15.23%. Conclusion The established method is sensitive, accurate, rapid and simple, which is suitable for simultaneous analysis of 51 kinds of pesticides in rice, garlic chives and tea.
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