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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。
OBJECTIVE To establish a QuECh ERS pretreatment system for the rapid determination of 41 pesticides in fruits and vegetables by on-line gel permeation chromatography-gas chromatography-tandem mass spectrometry (GPC-GC-MS / MS) by comparing different extraction solvents and extraction and purification methods method. Methods The samples were homogenized with acetonitrile-sodium acetate buffer, cleaned-up with mixed solid-phase dispersant, and analyzed by gel permeation chromatography-gas chromatography-tandem mass spectrometry and MRM. Results The linear correlation coefficients of 41 pesticides were all greater than 0.995 in the range of 2 ~ 200 ng / m L. 41 pesticides were added into the matrixes of celery and apple, and the mixed standards of 5, 10 and 50 μg / kg The average recoveries of 41 pesticides ranged from 71.0% to 125.4% with relative standard deviations ranging from 0.34% to 15.00%. The limit of quantification at the addition level of 5μg / kg was 0.107 ~ 10.100μg / kg. Conclusion This method is simple and rapid sample processing, compared with other multi-residue analysis of the purification effect is good, the sensitivity and selectivity increased significantly.