同位素稀释-高分辨气相色谱-高分辨质谱法测定土壤和沉积物中27种有机氯农药
Determination of 27 Organochlorine Pesticides in Soil and Sediment by Isotope Dilution-HRGC-HRMS
摘 要
采用同位素稀释-高分辨气相色谱-高分辨质谱法测定土壤、沉积物中的27种有机氯农药.以二氯甲烷-丙酮(1+1)混合液为提取溶剂对样品进行加速溶剂萃取,萃取液分别经凝胶渗透色谱柱和硅胶、氧化铝混合柱净化后,在DB-5MS非极性色谱柱上分离,以同位素稀释法进行定性定量分析.检出限(3s)不大于0.11 μg·L-1,加标回收率在65.1%~102%之间,测定值的相对标准偏差(n=5)不大于7.0%.
同位素稀释
有机氯农药
土壤
沉积物
HRGC-HRMS
Isotope dilution
OCPs
Soils
Sediment
Abstract
Isotope dilution-high resolution gas chromatography-high resolution mass spectrometry (ID-HRGC-HRMS) was applied to the determination of 27 organochlorine pesticides (OCPs) in soil and sediment.The sample was extracted with a mixture of dichloromethane and acetone (1+1) in accelerated solvent extractor.The extract was purified by a gel permeation chromatographic column and a mixed column containing silica gel and alumina as stationary phase,and then separated on a DB-5MS non-polar column.The OCPs were analyzed qualitatively and quantitatively by the method of isotope dilution.The detection limits (3s) of this method for all 27 OCPs were within 0.11 μg·L-1.The recovery rates measured by standard addition method ranged from 65.1% to 102% and RSD (n=5) were less than 7.0%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201507004
所属栏目 工作简报
基金项目 环保公益项目(20120916)
收稿日期 2014/7/2
修改稿日期
网络出版日期
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备注邓力(1979-),女,重庆人,教授级高级工程师,主要从事有机监测及研究.
引用该论文: DENG Li,YU Yi-song. Determination of 27 Organochlorine Pesticides in Soil and Sediment by Isotope Dilution-HRGC-HRMS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(7): 907～913
邓力,余轶松. 同位素稀释-高分辨气相色谱-高分辨质谱法测定土壤和沉积物中27种有机氯农药[J]. 理化检验－化学分册, 2015, 51(7): 907～913
被引情况:
【1】王荟,高占啟,章勇,胡冠九, "同位素稀释-气相色谱-高分辨双聚焦磁质谱法测定土壤中毒杀芬的含量",理化检验－化学分册 52, 7-10(2016)
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参考文献
【1】WOODWELL G M,CRAIG P P,JOHNSON H A.Modeling global emissions and residues of pesticides[J].Science,1971,174:1101-1107．
【2】WILLETT K L,ULRICH E M,HITES R A.Differential toxicity and environmental fates of HCH isomers[J].Environ Sci Technol,1998,32:2197-2207．
【3】HITCH R K,DAY H R.Unusual persistence of DDT in some Western USA soils[J].B Environ Contam Tox,1992,48:259-264．
【4】LEE K T,TANABE S,KOH C H.Distribution of organochlorine pesticides in sediments from Kyeonggi Bay and nearby areas,Korea[J].Environ Pollut,2001,114:207-213．
【5】QIU Xing-hua,ZHU Tong,JING Li,et al.Organochlorine pesticides in the air around the Taihu Lake,China[J].Environ Sci Technol,2004,38:1368-1374．
【6】ANDRADE A S,SACHETO D,HOFF R B,et al.Evaluation of lipid removal from animal fats for the determination of organochlorine,pesticides,and polychlorinated biphenyl indicators by gas chromatography with electron capture detector.[J].J Sep Sci,2012,35:2233-2240．
【7】KUMAR K S,WATANABE K,TAKEMORI H,et al.Using transgenic Caenorhabditis elegans in soil toxicity testing[J].Arch Environ Contam Toxicol,2005,48(4):538-542．
【8】ZOU Xi-mei,LIN Zhu-guang,PENG Shu-nv,et al.Determination of 29 pesticide residues in tobacco by gas chromatography-electron impact ionization mass spectrometry[J].Chinese Journal of Chromatography,2009,27(2):169-174．
【9】LOU Zheng-yun,CHEN Zong-mao,LUO Feng-jian,et al.Determination of 92 pesticide residues in tea by gas chromatography with solid-phase extraction[J].Chinese Journal of Chromatography ,2008,26(5):568-576．
【10】JIA Li-juan,DENG Yun-yun.Determination of organochlorine pesticides in soils using gas chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography,2008,26(6):697-702．
【11】RASHID A NAWAZ S,BARKER H,et al.Development of a simple extraction and clean-up procedure for determination of organochlorine pesticides in soils using gas chromatography-tandem mass spectrometry[J].J Chromatogr A,2010,1217:2933-2933．
【12】ZACHARIS C K,TAZANAVARAS P D,ROUBOS K,et al.Solvent-based de-emulsification dispersive liquid-liquid microextraction combined with gas chromatography-mass spectrometry for determination of trace organochlorine pesticides in environmental water samples[J].J Chromatogr A,2010,1217:5896-5901．
【13】HUANG Wen-jun,GAO Li-rong,GONG Ai-jun,et al.Determination of trace organochlorine pesticides in soil using isotope dilution-high resolution gas chromatography-high resolution mass spectrometry[J].Chinese Journal of Chromatography,2010,28(5):460-464．
【2】WILLETT K L,ULRICH E M,HITES R A.Differential toxicity and environmental fates of HCH isomers[J].Environ Sci Technol,1998,32:2197-2207．
【3】HITCH R K,DAY H R.Unusual persistence of DDT in some Western USA soils[J].B Environ Contam Tox,1992,48:259-264．
【4】LEE K T,TANABE S,KOH C H.Distribution of organochlorine pesticides in sediments from Kyeonggi Bay and nearby areas,Korea[J].Environ Pollut,2001,114:207-213．
【5】QIU Xing-hua,ZHU Tong,JING Li,et al.Organochlorine pesticides in the air around the Taihu Lake,China[J].Environ Sci Technol,2004,38:1368-1374．
【6】ANDRADE A S,SACHETO D,HOFF R B,et al.Evaluation of lipid removal from animal fats for the determination of organochlorine,pesticides,and polychlorinated biphenyl indicators by gas chromatography with electron capture detector.[J].J Sep Sci,2012,35:2233-2240．
【7】KUMAR K S,WATANABE K,TAKEMORI H,et al.Using transgenic Caenorhabditis elegans in soil toxicity testing[J].Arch Environ Contam Toxicol,2005,48(4):538-542．
【8】ZOU Xi-mei,LIN Zhu-guang,PENG Shu-nv,et al.Determination of 29 pesticide residues in tobacco by gas chromatography-electron impact ionization mass spectrometry[J].Chinese Journal of Chromatography,2009,27(2):169-174．
【9】LOU Zheng-yun,CHEN Zong-mao,LUO Feng-jian,et al.Determination of 92 pesticide residues in tea by gas chromatography with solid-phase extraction[J].Chinese Journal of Chromatography ,2008,26(5):568-576．
【10】JIA Li-juan,DENG Yun-yun.Determination of organochlorine pesticides in soils using gas chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography,2008,26(6):697-702．
【11】RASHID A NAWAZ S,BARKER H,et al.Development of a simple extraction and clean-up procedure for determination of organochlorine pesticides in soils using gas chromatography-tandem mass spectrometry[J].J Chromatogr A,2010,1217:2933-2933．
【12】ZACHARIS C K,TAZANAVARAS P D,ROUBOS K,et al.Solvent-based de-emulsification dispersive liquid-liquid microextraction combined with gas chromatography-mass spectrometry for determination of trace organochlorine pesticides in environmental water samples[J].J Chromatogr A,2010,1217:5896-5901．
【13】HUANG Wen-jun,GAO Li-rong,GONG Ai-jun,et al.Determination of trace organochlorine pesticides in soil using isotope dilution-high resolution gas chromatography-high resolution mass spectrometry[J].Chinese Journal of Chromatography,2010,28(5):460-464．
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