QuEChERS-在线凝胶色谱-气相色谱-质谱法测定植物油中34种农药残留  

Simultaneous Determination of 34 Pesticide Residues in Vegetable Oil by QuEChERS-on-line Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry

作　　者：阮华[1,2] 荣维广[2] 宋宁慧[3] 吉文亮[2] 刘华良[2] 马永建[2] 

机构地区：[1]东南大学公共卫生学院,南京210009 [2]江苏省疾病预防控制中心,南京210009 [3]环境保护部南京环境科学研究所,南京210042

出　　处：《分析化学》2014年第8期1110-1116,共7页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.41101307);江苏省"十二-五"科教兴卫工程(No.ZX201109);江苏省疾病预防控制中心"科教兴业工程"项目(No.JKRC2011030)资助~~

摘　　要：建立了葵花油、大豆油和玉米油中34种中高毒农药的快速筛查方法。样品采用改进的QuEChERS方法进行提取净化,提取液采用在线GPC-GC-MS检测。结果表明,34种农药在0.01~0.2 mg/L范围内具有良好的线性关系,相关系数为0.9913~0.9997。除p,p＇-DDE,p,p＇-DDD,p,p＇-DDT外的31种农药在葵花油、大豆油和玉米油中的检出限分别为0.0692~2.28μg/kg,0.0559~2.01μg/kg,0.0584~2.14μg/kg;在0.05和0.1μg/g添加水平的平均回收率分别为70.3%~115.4%,69.5%~112.6%,70.2%~116.1%;相对标准偏差（RSD,n=6）分别为2.9%~13.3%,3.9%~13.5%,4.2%~12.1%。本方法具有操作便捷、快速等特点,适用于葵花油、大豆油和玉米油中34种农药残留的快速筛查与检测。A method for the simultaneous determination of 34 pesticides in sunflower oil, soybean oil and corn oil was developed. The samples were extracted and purified by a modified QuEChERS method, and then the supernatant was analyzed by on-line gel permeation chromatography-gas chromatography-mass spectrometry （ GPC-GC-MS ） . The linear range was from 0 . 01 to 0 . 2 mg/L with a good correlation coefficients （ r≥0. 9913）. The average recoveries of 31 pesticides （except p,p′-DDE, p,p′-DDD, p,p′-DDT. For detail, please reference to section 3 . 6 ） ranged from 70 . 3% to 115 . 4%, 69 . 5% to 112 . 6% and 70 . 2% to 116 . 1%spiked at 0. 05 μg/g and 0. 1 μg/g with the relative standard deviations （RSDs, n=6） less than 13. 3%, 13. 5% and 12. 1% in sunflower oil, soybean oil and corn oil samples, respectively. The LODs of this method ranged from 0. 0692 to 2. 28, 0. 0559 to 2. 01 and 0. 0584 to 2. 14μg/kg （S/N=3） in sunflower oil, soybean oil and corn oil samples respectively. The convenient operation and versatility of this method are suitable for the fast screening and detection of 34 pesticide residues in sunflower oil, soybean oil and corn oil.

关 键 词：QUECHERS 凝胶色谱-气相色谱-质谱 植物油 农药残留 快速筛查 

分 类 号：O657.63[理学—分析化学] TS227[理学—化学]