气相色谱-三重四级杆质谱法测定菜籽油中40种农药残留

李洁 梁艺馨 王兴宁

摘要 [目的]建立气相色谱-串联质谱法测定菜籽油中40种农药残留的检测方法。[方法]考察不同提取剂的提取效果，比较氟罗里柱和中性氧化铝C18小柱、Agela TPT-spe小柱和Agela PC/NH2-SPE小柱对样品的净化效果，优选出以乙腈提取、Agela TPT-spe柱净化的试验条件，GC-MS-MS采用多反应监测模式（MRM）。[结果]40种农药在0.05～0.40 mg/L满足线性关系， r> 0.99，检出限在0.000 1～0.008 0 mg/kg;在0.04～0.40 mg/kg进行了3个浓度水平的加标回收试验，回收率在78%～110%，相对偏差（RSD， n =6）小于10%。[结论]该方法灵敏度高、选择性好、抗干扰能力强，适合菜籽油中40种农药残留的准确定量和定性分析。

关键词 气相色谱-三重四级杆质谱法;菜籽油;农药残留

中图分类号 TS207.5+3 文献标识码 A

文章编号 0517-6611（2020）14-0187-05

doi：10.3969/j.issn.0517-6611.2020.14.053

Abstract [Objective]To establish a gas chromatography-tandem mass spectrometry method for the simultaneous determination of 40 pesticide residues in rapeseed oil.[Method]The extraction effects of different extraction regents were compared and the purifying effects of Flerpillar column，Neutral alumina column， cleanert C18 solid phase extraction column ，cleanert TPT solid phase extraction column and cleanert PC/NH2 solid phase extraction column were also investigated.The optimum pretreatment conditions for the rapeseed oil samples were determined as follows： extracting the rapeseed oil samples by n-hexane followed by cleanert TPT column purification.The purified samples were then analyzed by GC-MS/MS with MRM mode，and quantified by internal standard method.[Result]A good linear relationship was established in the 40 pesticide residues concentration range of 0.05-0.40 mg/L and the correlation coefficient was above 0.99.At the spiked levels of 0.04-0.40 mg/kg， the average recoveries of difenoconazole at three spiked concentration levels ranged from 78% to 110% with the relative standard deviation less than 10%（ n =6）.[Conclusion]The method has high sensitivity， good selectivity and strong anti-interference ability， and is suitable for accurate quantitative and qualitative analysis of 40 pesticide residues in rapeseed oil.

Key words Gas chromatography-triple quadrupole mass spectrometry;Rapeseed oil;Pesticide residues

菜籽油是我國主要的食用油之一，主产于长江流域及西南、西北等地，产量居世界首位。油菜在种植过程会使用有机磷、有机氯和拟除虫菊酯农药等进行病虫害的防治，菜籽油的农药残留安全问题也越来越受关注。近年来对食用植物油中农药残留检测的方法有凝胶渗透色谱（GPC）法[1]、分散固相萃取法[2-4]和固相萃取法等，GPC法处理繁杂、耗时长;分散固相萃取法对菜籽油中复杂的成分和色素不能有效的去除和净化。采用固相萃取法气相色谱法[5]、固相萃取法气相色谱质谱法[6-7]测定食用植物油中农药残留，对花生油、大豆油等色素含量低、基质相对简单的植物油有很好的去除效果，但对菜籽油提取净化效果不好，干扰大，基质效应高。笔者针对近几年来植物油中农药残留检测的方法进行优化，结合气相色谱-三重四级杆质谱仪进行检测。