气相色谱-质谱法检测植物油中腐霉利和氟硅唑含量
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摘要
采用QuEChERS快速净化小柱进行快速样品前处理,利用气相色谱-质谱法检测植物油中腐霉利和氟硅唑农残含量。结果显示:腐霉利和氟硅唑加标回收率分别为85. 0%～96. 0%和88. 3%～94. 1%;精密度实验腐霉利和氟硅唑实验室内变异系数分别为1. 5%～8. 9%和2. 1%～6. 8%;腐霉利和氟硅唑的检出限分别为0. 007 5 mg/kg和0. 022 5 mg/kg。该方法前处理简便,灵敏度高,重现性好。
Using Qu EChERS rapid purification column to pretreat sample,the procymidone and flusilazole pesticides residues in vegetable oil were determined by GC-MS. The results showed that the recoveries of procymidone and flusilazole were 85. 0%-96. 0% and 88. 3%-94. 1%,respectively; the intra-laboratory variation coefficients of procymidone and flusilazole were 1. 5%-8. 9% and 2. 1%-6. 8%,respectively; the detection limits of procymidone and flusilazole were 0. 007 5 mg/kg and 0. 022 5 mg/kg,respectively. The method had the advantages of simple pretreatment,high sensitivity and good reproducibility.
Using Qu EChERS rapid purification column to pretreat sample,the procymidone and flusilazole pesticides residues in vegetable oil were determined by GC-MS. The results showed that the recoveries of procymidone and flusilazole were 85. 0%-96. 0% and 88. 3%-94. 1%,respectively; the intra-laboratory variation coefficients of procymidone and flusilazole were 1. 5%-8. 9% and 2. 1%-6. 8%,respectively; the detection limits of procymidone and flusilazole were 0. 007 5 mg/kg and 0. 022 5 mg/kg,respectively. The method had the advantages of simple pretreatment,high sensitivity and good reproducibility.
引文
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[14]陈章明,杨石有,张蕊,等.氟硅唑·丙环唑混合药剂高效液相色谱分析[J].农药,2016(11):814-816.
[15]FULGNCIO A C D C,SACZK A A,OLIVEIRA M F D,et al.New voltammetry-based aanalytical method for indirect determination of procymidone in Brazilian apples[J].Food Anal Method,2014,7(1):31-38.
[16]ARAU'JO E A,LARA M C R,REIS M R D,et al.Determination of haloxyfop-methyl,linuron,and procymidone pesticides in carrot using SLE-LTP extraction and GC-MS[J].Food Anal Method,2016,9(5):1-9.
[17]KORBA K,PELIT L,PELIT F O,et al.Preparation and characterization of sodium dodecyl sulfate doped polypyrrole solid phase micro extraction fiber and its application to endocrine disruptor pesticide analysis[J].J Chromatogr B,2013,929(7):90-96.
[18]刘亚伟,董一威,孙宝利,等.Qu ECh ERS在食品中农药多残留检测的应用研究进展[J].食品科学,2009,30(9):285-289.
[2]张国军.八种常用杀菌剂“三致”作用及生殖毒性研究进展[J].中国预防医学杂志,2007,8(3):320-321.
[3]宋晰,肖露,林东,等.番茄灰霉病菌对腐霉利的抗药性检测及生物学性状研究[J].农药学学报,2013,15(4):398-404.
[4]林才华.山东主要草莓种植区草莓枯萎病菌抗药性及抗三唑酮菌系的生理生化研究[D].山东泰安:山东农业大学,2009.
[5]蒲金基,杨石有,张贺,等.芒果炭疽病菌对三唑酮的敏感性基线及抗药性评价[J].农药,2014(8):597-599.
[6]OH B Y.Pesticide residues for food safety and environment protection[M].Suwon:Food and Fertilizer Technology Center,2001.
[7]曾鑫年,黄柯程,黎卓莹,等.低剂量农药对人体健康的影响[C]//第五届广东省环境诱变剂学会暨第三届广东省预防医学会卫生毒理专业委员会学术交流会论文集.北京:中国诱变剂学会,2006.
[8]宋博才.气相色谱法测定草莓的农残含量[J].安徽农业科学,2016(10):133-135.
[9]ZHANG C,ZHOA H,WU M,et al.Simultaneous determination of procymidone,pyridaben and beta-cypermethrin residues in tea solution by GC-ECD[J].J Chromatogr Sci,2012,50(10):940-944.
[10]陈琼,喻芳,张惠,等.Qu ECh ERS法处理结合液质法测茶叶中多种农残[J].广州化工,2015(16):143-146.
[11]张群,吴南村,张月,等.气相色谱-串联质谱法测定韭菜中的三唑酮和腐霉利残留[J].农药学学报,2016,18(3):397-401.
[12]解魁,张伟,杨丽,等.气相色谱-质谱联用法测定人参中五氯苯胺和腐霉利的残留[J].中国卫生检验杂志,2015(21):3624-3625.
[13]SOARES A A,AMARAL E H,SOUSA L A F D,et al.In-house method validation and occurrence of alpha-,beta-endosulfan,endosulfan sulphate,lambda-cyhalothrin,procymidone and trifluralin residues in strawberry[J].Food Sci Technol,2013,33(4):765-775.
[14]陈章明,杨石有,张蕊,等.氟硅唑·丙环唑混合药剂高效液相色谱分析[J].农药,2016(11):814-816.
[15]FULGNCIO A C D C,SACZK A A,OLIVEIRA M F D,et al.New voltammetry-based aanalytical method for indirect determination of procymidone in Brazilian apples[J].Food Anal Method,2014,7(1):31-38.
[16]ARAU'JO E A,LARA M C R,REIS M R D,et al.Determination of haloxyfop-methyl,linuron,and procymidone pesticides in carrot using SLE-LTP extraction and GC-MS[J].Food Anal Method,2016,9(5):1-9.
[17]KORBA K,PELIT L,PELIT F O,et al.Preparation and characterization of sodium dodecyl sulfate doped polypyrrole solid phase micro extraction fiber and its application to endocrine disruptor pesticide analysis[J].J Chromatogr B,2013,929(7):90-96.
[18]刘亚伟,董一威,孙宝利,等.Qu ECh ERS在食品中农药多残留检测的应用研究进展[J].食品科学,2009,30(9):285-289.