GC Determination of Residual Amount of Pyrethroid Pesticides in Whitebait with Separation by Dispersive Solid Phase Extraction
摘 要
以冰乙酸-乙腈溶液为萃取溶剂,采用乙二胺-N-丙基硅烷(PSA)、C18和石墨化炭黑固相材料分散净化技术,以气相色谱-电子捕获检测器测定银鱼中6种拟除虫菊酯类农药(联苯菊酯、甲氰菊酯、高效氯氟氰菊酯、氯氰菊酯、氰戊菊酯和溴氰菊酯).该方法在0.05~1.0 mg·L-1范围内呈线性关系.方法的检出限(3S/N):氯氰菊酯为0.02 mg·kg-1,其余5种拟除虫菊酯均为0.01 mg·kg-1.以银鱼试样为基体,加入两种不同浓度的6种拟除虫菊酯标准溶液作回收试验,测得回收率在82.9%~106.1%之间,相对标准偏差(n=6)在2.9%~7.1%之间.
Abstract
Six pyrethroid pesticides,namely bifenthrin,fenpropathrin,cyhalothrin,cypermethrin,fenvalerate and deltamethrin,in whitebait were determined simultaneously by GC with ECD after separation by dispersive solid phase extraction (DSPE).Sample of whitebait was extracted homogeneously with glacial acetic acid-acetonitrile solution as dispersion agent.The extract obtained was purified by DSPE through cycle-shaking with ethylene diamine-N-propylsilane (PSA),C18 and graphitized carbon black.The supernatant was used for GC-ECD analysis.Linearity ranges found were in the same range of 0.05-1.0 mg·L-1 for the 6 pyrethroid pesticides.Detection limits (3S/N) of the method obtained were 0.01 mg·kg-1 for cypermethrin and 0.02 mg·kg-1 for the other 5 pyrethroid pesticides.Tests for recovery and precision were made by addition of standard solutions of the 6 pyrethroid pesticides with 2 different concentrations to whitebait sample which was then analyzed by the proposed method.Values of recovery obtained were in the range of 82.9%-106.1% and values of RSD′s (n=6) were in the range of 2.9%-7.1%.
中图分类号 O657.7
所属栏目 工作简报
基金项目 江苏出入境检验检疫局科研计划(2009KJ33)
收稿日期 2009/7/11
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备注曹军(1982-),男,安徽怀宁人,工程师,主要从事食品检验检疫.
引用该论文: CAO Jun,CHEN Yong,YANG Rui-zhang,XU Bang-xing,WANG Tai-quan,HUANG Yue-fang. GC Determination of Residual Amount of Pyrethroid Pesticides in Whitebait with Separation by Dispersive Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(10): 1176~1178
曹军,陈勇,杨瑞章,徐邦兴,王太全,黄月芳. 分散固相萃取分离-气相色谱法测定银鱼中拟除虫菊酯类农药残留量[J]. 理化检验-化学分册, 2010, 46(10): 1176~1178
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【8】李莉,江树人,潘灿平,等.分散固相萃取-气相色谱-质谱方法快速净化测定枸杞中12种农药残留[J].农药学学报,2006,8(4):371-374.
【9】胡西洲,程运斌,胡定金.QuEChERS法测定蔬菜中有机磷类农药多残留析[J].中国测试技术,2006,32(3):132-134.
【10】张秀尧,蔡欣欣,陈珞洛,等.缓冲QuEChERS法提取气相色谱火焰光度检测法快速测定水果蔬菜中39种有机磷农药残留[J].中国卫生检验杂志,2007,17(12):2133-2136.
【11】祁克宗,施祖灏,彭开松,等.基质固相分散萃取-高效液相色谱法检测鸡组织中均三嗪类药物残留[J].分析化学,2007,11(35):1601-1606.
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【13】THIERRY D,MARIA G,PAULA P,et al.Dispersive solid-phase extraction followed by liquid chromatography-tandem mass spectrometry for the multi-residue analysis of pesticidesin raw bovine milk[J].Journal of Chromatography A,2009,1216:3702-3706.
【14】刘敏,端裕树,宋苑苑,等.分散固相萃取-液相色谱-质谱检测蔬菜水果中氨基甲酸酯和有机磷农药[J].分析化学,2006,34(7):941-945.
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