【摘要】 目的通过比较不同的提取溶剂和提取净化方法,建立了Qu ECh ERS前处理,在线凝胶色谱-气相色谱-串联质谱法(GPC-GC-MS/MS)快速测定蔬菜水果中41种农药的检测方法。方法样品经乙腈-乙酸乙酸钠缓冲液均质提取,混合型固相分散萃取剂净化,凝胶渗透色谱气相色谱串联质谱,MRM模式检测。结果在2~200 ng/m L范围内,41种农药的线性相关系数均大于0.995,在芹菜和苹果两种样品基质中添加41种农药,添加水平为5、10和50μg/kg的混合标准溶液,41种农药的平均回收率范围为71.0%~125.4%,相对标准偏差范围为0.34%~15.00%。添加水平为5μg/kg时的定量限为0.107~10.100μg/kg。结论该方法样品处理简单快速,相比其他多残留分析方法净化效果好,其灵敏度和选择性明显提高。更多还原

【Abstract】 Objective A method for the determination of 41 pesticides including 26 organophosphorus pesticides,6 kinds of carbamate,7 pryethoids insecticides,1 kinds of organochlorine and fungicide in vegetables and fruits,was established based on optimized Qu ECh ERS with on line gel permeation chromatography-gas chromatography-mass spectrometry( GPC-GC-MS / MS). Methods The method obtained the optimized conditions by comparing different methods of extraction and purification. The analytes were extracted from the samples using acetonitrile-buffer of acetic acid and sodium acetate. Then the extracts were determined by GC-MS / MS in multireaction monitoring( MRM) mode after being cleaned up with mixed solid-phase dispersion. And the external standard method was applied to quantify. Results All the 41 pesticides had good linearity in the ranges of 2-200 ng / m L with the correlation coefficients higher than 0. 995. The average recoveries of the most of 41 pesticides in celery and apple were in the range of 71. 0%- 125. 4% at the spiked levels of 5,10 and 50 μg / kg,with relative standard deviations( RSDs) of 0. 34%-15. 0%. The limits of quantification( LOQs) of the method at the spiked levels of 5 μg / kg were 0. 107- 10. 100 μg / kg. Conclusion The method is simple,rapid,sensitive and specific.更多还原