Determination of Organochlorine Pesticides in Fish by GC with Dual-Column and Dual-ECD
摘 要
采用气相色谱-双柱双电子捕获检测器(ECD)测定鱼肉样品中的10种有机氯农药(六氯苯、α-六六六、β-六六六、γ-六六六、δ-六六六、七氯、p,p'-DDE、o,p'-DDT、p,p'-DDD和p,p'-DDT)。样品经正己烷振荡提取后,提取液经自制酸性硅胶柱净化,采用DB-35MS和DB-5毛细管色谱柱进行双柱双ECD分析。10种有机氯农药的线性范围均为5.0~250 μg·L-1,检出限(3.143s)在0.2~1.2 μg·kg-1之间。加标回收率在85.7%~121%之间,测定值的相对标准偏差(n=6)不大于16%。
Abstract
GC with dual-column and dual-ECD was applied to the determination of 10 organochlorine pesticides in fish, including hexachlorobenzene, α-BHC, β-BHC, γ-BHC, δ-BHC, heptachlor, p,p'-DDE, o,p'-DDT, p,p'-DDD and p,p'-DDT. After the samples were extracted by oscillation with hexane, the extract was cleaned-up with self-made acidic silica gel column and the purified solution was analyzed by GC with dual-column (DB-35MS and DB-5) and dual-ECD system. The linearity ranges of 10 organochlorines were all 5.0-250 μg·L-1, with detection limits (3.143s) in the range of 0.2-1.2 μg·kg-1. Recovery rates obtained by standard addition method were in the range of 85.7%-121% and RSDs (n=6) were within 16%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201703003
所属栏目 试验与研究
基金项目 国家自然科学基金资助项目(41101476);流域水生态环境质量监测与评价研究(2013ZX07502001)
收稿日期 2016/2/24
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联系人作者许秀艳(xuxy@cnemc.cn)
备注曹方方(1988-),女,山东济宁人,硕士研究生,主要研究方向为环境有机污染物监测与分析。
引用该论文: CAO Fang-fang,YU Jian-zhao,FEI Jin-yan,XU Xiu-yan,XU Ren-ji,LÜ,Yi-bing. Determination of Organochlorine Pesticides in Fish by GC with Dual-Column and Dual-ECD[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(3): 258~262
曹方方,于建钊,费金岩,许秀艳,许人骥,吕怡兵. 气相色谱-双柱双电子捕获检测器测定鱼肉中的有机氯农药[J]. 理化检验-化学分册, 2017, 53(3): 258~262
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【3】WANG H S, ZHAO Y G, MAN Y B, et al. Oral bioaccessibility and human risk assessment of organochlorine pesticides(OCPs) vial fish consumption using an invitro gastrointestinal model[J]. Food Chemistry, 2011,127(4):1673-1679.
【4】POON C K K, LEUNG C K C, WONG M H, et al. Polychlorinated biphenyls and organochlorine pesticides in human adpose tissues and breast milk collected in Hongkong[J]. Archives of Environment Contamination and Toxicology, 2005,49(2):274-282.
【5】SN/T 0127-2011进出口源性食品中六六六、滴滴涕和六氯苯残留量的检测方法气相色谱质谱法[S].
【6】GB/T 9695.10-2008肉与肉制品六六六、滴滴涕残留量测定[S].
【7】GB/T 14551-2003动、植物中六六六和滴滴涕测定的气相色谱法[S].
【8】刘秀芬,劳文剑,毕新慧,等.南极鲍鱼样品中有机氯农药的测定[J].分析化学, 2002,30(9):1035-1037.
【9】GB 2763-2014食品安全国家标准食品中农药最大残留限量[S].
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