分散固相萃取-气相色谱-串联质谱法测定输印尼大蒜中5种农药残留  

Determination of 5 pesticides residues in garlic exported to Indonesia by gas chromatography tandem mass spectrometry with dispersive solid-phase extraction

作　　者：陈君义 王毅谦[2] 孙慧宇 陆慧媛[2] 殷冉 高玲[2] 王伟 王云飞 CHEN Jun-yi1, WANG Yi-qian2, SUN Hui-yu1, LU Hui-yuan2, YIN Ran3, GAO Ling2, WANG Wei1, WANG Yun-fei1(1 .Xuzhou Entry-Exit Inspection and Quarantine Bureau, Xuzhou 221006; 2.Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001; 3.Changshu Entry-Exit Inspection and Quarantine Bureau, Changshu 21550)

机构地区：[1]徐州出入境检验检疫局,徐州221006 [2]江苏出入境检验检疫局,南京210001 [3]常熟出入境检验检疫局,常熟215500

出　　处：《食品科技》2018年第3期315-319,共5页Food Science and Technology

基　　金：江苏省自然科学基金青年基金项目(BK20150443);国家质检总局科技项目(2015IK141)

摘　　要：印尼颁发的农业部长4号令对我国大蒜出口造成了严重影响。利用改进的QuEChERS技术为前处理方法,优化了净化吸附剂的用量,建立了输印尼大蒜中5种农药残留的检测方法。样品中加入无水乙酸钠和正己烷饱和的乙腈(含0.1%乙酸)溶液,振荡后过滤,滤液经旋转蒸干,色谱纯乙腈洗脱、PSA-C18吸附剂组合净化,过滤膜后用气相色谱-串联质谱测定。结果表明,在(0.1~1500)μg/L范围内,5种农药的浓度与峰面积呈良好的线性关系,相关系数均大于0.99,仪器的检出限为(0.1~100)ng/m L,方法的定量限为(0.025~25)μg/kg。5种农药在各自3个添加水平下,在大蒜中的平均回收率在84.3%~111.3%,相对标准偏差RSD为1.9%~6.7%。结果表明利用该方法能快速准确地对输印尼大蒜进行分析,满足输入国的要求。Act 4 issued by minister of Indonesia agriculture seriously affected export of Chinese garlic. A method was set up to determine the residues of 5 pesticides in garlic exported to Indonesia with modified QuEChERS and optimized quantity of absorbents. The garlic was extracted with acetonitrile saturated by hexane containing 0.1% acetic acid （v/v）. The extract was evaporated and then redissolved by acetonitrile. The organic phase was transferred to a tube filled with combination of PSA and C18 with amounts of （50-50）mg, shaked and tilted through a membrane for the final determination by gas chromatography tandem mass spectrometry. The results revealed that the concentration of 5 pesticides and their peak area showed nice linear relation in range of （0.1-1500）pg/L with R~〉~0.99. The LOD of the method was （0.1-100）ng/mL and LOQ was （0.025-25）pg/kg. The recovery test was conducted at three different levels with the average recovery ranged from 84.3% to 111.3% and RSD ranged from 1.9% to 6.7%. The method could provide fast and accurate determination of the residues in garlic export to Indonesia.

关 键 词：大蒜 分散固相萃取 气相色谱-串联质谱 农药残留 

分 类 号：O657.63[理学—分析化学]