Simultaneous Determination of Residual Amounts of 37 Pesticides in Rice by Gas Chromatography
摘 要
提出了分散固相萃取-气相色谱法同时测定大米中37种农药残留量的方法.采用C18、乙二胺-N-丙基硅烷(PSA)和无水硫酸镁固相材料分散净化技术,以丙酮-正己烷(25+75)溶液为萃取溶剂,用脉冲火焰光度检测器和电子捕获检测器同时测定37种农药.13种有机氯农药的线性范围为0.02~0.2 mg·L-1,16种有机磷农药和8种拟除虫菊酯农药的线性范围为0.1~1.0 mg·L-1,方法的检出限(3S/N)均小于0.02 mg·kg-1.以大米样品为基体,加入三种不同浓度的农药标准溶液作回收试验,测定回收率在71.8%~111.8%之间,相对标准偏差(n=3)在1.1%~14.0%之间.
Abstract
Thirty-seven pesticides in rice were determined simultaneously by GC with PFPD and ECD after separation by dispersive-solid phase extraction (DSPE).Sample of rice was extracted homogeneously with mixture of acetone-hexane(25+75) as dispersion agent.The extract obtained was purified by DSPE through shaking with mixture of C18,ethylene diamine-N-propylsilane (PSA) and anhydrous magnesium sulfate in the sample flask.The supernatant was used for GC analysis with PFPD and ECD.Linearity ranges of 13 organochlorine,16 organophosphorous and 8 pyrethroid pesticides were kept in the ranges of 0.02-0.2 mg·L-1,0.1-1.0 mg·L-1 and 0.1-1.0 mg·L-1 respectively.Detection limits (3S/N) found were less than 0.02 mg·kg-1.Tests for recovery and precision were made by addition of standard solutions of the 37 pesticides at 3 different concentration levels to rice sample which was then analyzed by the proposed method.Values of recovery obtained were in the range of 71.8%-111.8% and values of RSD′s (n=3) were in the range of 1.1%-14.0%.
中图分类号 O657.7
所属栏目 工作简报
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收稿日期 2009/8/14
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备注张潜(1977-),女,四川内江人,硕士,主要研究方向为理化检验.
引用该论文: ZHANG Qian,LAI Fa-wei. Simultaneous Determination of Residual Amounts of 37 Pesticides in Rice by Gas Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(11): 1289~1292
张潜,赖发伟. 气相色谱法同时测定大米中37种农药残留[J]. 理化检验-化学分册, 2010, 46(11): 1289~1292
被引情况:
【1】张利强,程盛华,李琪,杨春亮, "气相色谱法测定谷物中9种有机磷农药残留量的基质效应",理化检验-化学分册 52, 136-140(2016)
【2】张勇,刘玉波,陈丽丽,夏品华,李存雄,张明时, "超声提取-气相色谱法测定保健品中15种有机氯农药残留量",理化检验-化学分册 49, 337-340(2013)
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参考文献
【1】GB/T 5009.20-2003食品中有机磷农药残留量的测定[S].
【2】GB/T 5009.146-2003植物性食品中有机氯和拟除虫菊酯类农药多种残留的测定[S].
【3】林维宣,田苗,李继业,等.双柱固相萃取-高效液相色谱法测定大米中氨基甲酸酯农药残留量的研究[J].中国粮油学报,2003,18(2):79-84.
【4】王明泰,牟峻,吴剑,等.GC-MS法测定粮谷及油料中55种有机磷农药残留量[J].分析试验室,2006,25(11):110-117.
【5】ANASTASSIADES M,LEHOTAY S J,STAJNBAHER D,et al.Fast and easy multiresidue method employing acetonitrile extraction/partitioning and "dispersive solid-phase extraction" for the determination of pesticide residues in produce[J].Journal of AOAC International,2003,86(2):412-431.
【6】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分析[J].中国测试技术,2006,32(3):132-133.
【7】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):371-3741.
【8】陈舒舒,许凯,徐彦军,等.蜂蜜中氯霉素残留的检测及净化方法研究[J].安全与环境学报,2006,6(2):92-951.
【9】廖百森,肖义夫,赵舰,等.电子捕获鉴定器-气相色谱测定1605有机磷农药的探讨[J].现代预防医学,2002,29(2):156-157.
【10】张潜,高玲,赖发伟,等.电子捕获检测器-气相色谱法测定饮用水中多种有机磷残留[J].现代预防医学,2007,34(14):2715-2717.
【2】GB/T 5009.146-2003植物性食品中有机氯和拟除虫菊酯类农药多种残留的测定[S].
【3】林维宣,田苗,李继业,等.双柱固相萃取-高效液相色谱法测定大米中氨基甲酸酯农药残留量的研究[J].中国粮油学报,2003,18(2):79-84.
【4】王明泰,牟峻,吴剑,等.GC-MS法测定粮谷及油料中55种有机磷农药残留量[J].分析试验室,2006,25(11):110-117.
【5】ANASTASSIADES M,LEHOTAY S J,STAJNBAHER D,et al.Fast and easy multiresidue method employing acetonitrile extraction/partitioning and "dispersive solid-phase extraction" for the determination of pesticide residues in produce[J].Journal of AOAC International,2003,86(2):412-431.
【6】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分析[J].中国测试技术,2006,32(3):132-133.
【7】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):371-3741.
【8】陈舒舒,许凯,徐彦军,等.蜂蜜中氯霉素残留的检测及净化方法研究[J].安全与环境学报,2006,6(2):92-951.
【9】廖百森,肖义夫,赵舰,等.电子捕获鉴定器-气相色谱测定1605有机磷农药的探讨[J].现代预防医学,2002,29(2):156-157.
【10】张潜,高玲,赖发伟,等.电子捕获检测器-气相色谱法测定饮用水中多种有机磷残留[J].现代预防医学,2007,34(14):2715-2717.
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