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高分辨气相色谱/高分辨质谱法测定南极样品中有机氯农药

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陈昭晶, 李英明, 王璞, 朱超飞, 高冠军, 肖珂, 任代卫, 张庆华. 高分辨气相色谱/高分辨质谱法测定南极样品中有机氯农药[J]. 环境化学, 2014, 33(10): 1655-1661. doi: 10.7524/j.issn.0254-6108.2014.10.008
引用本文: 陈昭晶, 李英明, 王璞, 朱超飞, 高冠军, 肖珂, 任代卫, 张庆华. 高分辨气相色谱/高分辨质谱法测定南极样品中有机氯农药[J]. 环境化学, 2014, 33(10): 1655-1661. doi: 10.7524/j.issn.0254-6108.2014.10.008
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CHEN Zhaojing, LI Yingming, WANG Pu, ZHU Chaofei, GAO Guanjun, XIAO Ke, REN Daiwei, ZHANG Qinghua. Determination of organochlorine pesticides in Antarctic samples using high resolution gas chromatography/high resolution mass spectrometry(HRGC/HRMS)[J]. Environmental Chemistry, 2014, 33(10): 1655-1661. doi: 10.7524/j.issn.0254-6108.2014.10.008
Citation: CHEN Zhaojing, LI Yingming, WANG Pu, ZHU Chaofei, GAO Guanjun, XIAO Ke, REN Daiwei, ZHANG Qinghua. Determination of organochlorine pesticides in Antarctic samples using high resolution gas chromatography/high resolution mass spectrometry(HRGC/HRMS)[J]. Environmental Chemistry, 2014, 33(10): 1655-1661. doi: 10.7524/j.issn.0254-6108.2014.10.008
shu

高分辨气相色谱/高分辨质谱法测定南极样品中有机氯农药

  • 1.

    中国科学院生态环境研究中心, 环境化学与生态毒理学国家重点实验室, 北京, 100085

  • 基金项目:

    国家海洋局南极科学考察项目(2011GW02003)

    国家自然科学基金项目(41276195,21277165, 21107121)

    中国科学院战略性先导科技专项(B类)(XDB14010100)资助.

Determination of organochlorine pesticides in Antarctic samples using high resolution gas chromatography/high resolution mass spectrometry(HRGC/HRMS)

  • 1.

    State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing, 100085, China

  • Fund Project:

  • 摘要: 建立了同位素稀释-高分辨气相色谱/高分辨质谱法(HRGC/HRMS)测定南极土壤、苔藓和地衣样品中23种有机氯农药的分析方法.样品经冷冻干燥、研磨处理后用正己烷:二氯甲烷(1:1, V:V)混合溶剂进行加速溶剂萃取(ASE),萃取液经硅胶-氧化铝层析柱和C18小柱净化后,进HRGC/HRMS检测分析.样品中目标物定量采用平均相对响应因子法,6点标准曲线响应因子的相对标准偏差(RSD)≤20%,方法的线性范围为0.4—800 μg·L-1,回收率在62%—101%之间.实际样品分析结果表明,23种OCPs的加标回收率为40%—100%,在土壤、苔藓和地衣样品中的检出限(LODs)分别为0.024—5.01、0.2—12.2、0.020—13.7 pg·g-1,可以满足南极环境样品中有机氯农药的检测分析.
    Abstract: An analytical method was developed for the determination of 23 organochlorine pesticides (OCPs) in soil, moss and lichen samples from the Antarctic using isotope dilution high resolution gas chromatography coupled with high resolution mass spectrometry (HRGC/HRMS). The sample extraction was performed on accelerated solvent extractor (ASE) and the extract was cleaned up on silica gel-alumina chromatographic column and C18 solid phase extraction cartridge. Instrumental analysis was performed by HRGC/HRMS. The average relative response factors were calculated by the calibration standards and employed for the quantification of the targets, of which the relative standard deviations (RSD) were lower than 20%, the linear range and the recoveries of this method was 0.4—800 μg·L-1 and 62%—101% respectively. The recoveries of the field samples for all OCPs ranged from 40% to 100%, and the limits of detection (LODs) were in the range of 0.024—5.01 pg·g-1, 0.2—12.2 pg·g-1, 0.020—13.7 pg·g-1 in soils, mosses and lichens, which can satisfy the determination of organochlorine pesticides in Antarctic environmental samples.
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  • 收稿日期:  2014-05-23
陈昭晶, 李英明, 王璞, 朱超飞, 高冠军, 肖珂, 任代卫, 张庆华. 高分辨气相色谱/高分辨质谱法测定南极样品中有机氯农药[J]. 环境化学, 2014, 33(10): 1655-1661. doi: 10.7524/j.issn.0254-6108.2014.10.008
引用本文: 陈昭晶, 李英明, 王璞, 朱超飞, 高冠军, 肖珂, 任代卫, 张庆华. 高分辨气相色谱/高分辨质谱法测定南极样品中有机氯农药[J]. 环境化学, 2014, 33(10): 1655-1661. doi: 10.7524/j.issn.0254-6108.2014.10.008
shu
CHEN Zhaojing, LI Yingming, WANG Pu, ZHU Chaofei, GAO Guanjun, XIAO Ke, REN Daiwei, ZHANG Qinghua. Determination of organochlorine pesticides in Antarctic samples using high resolution gas chromatography/high resolution mass spectrometry(HRGC/HRMS)[J]. Environmental Chemistry, 2014, 33(10): 1655-1661. doi: 10.7524/j.issn.0254-6108.2014.10.008
Citation: CHEN Zhaojing, LI Yingming, WANG Pu, ZHU Chaofei, GAO Guanjun, XIAO Ke, REN Daiwei, ZHANG Qinghua. Determination of organochlorine pesticides in Antarctic samples using high resolution gas chromatography/high resolution mass spectrometry(HRGC/HRMS)[J]. Environmental Chemistry, 2014, 33(10): 1655-1661. doi: 10.7524/j.issn.0254-6108.2014.10.008
shu

高分辨气相色谱/高分辨质谱法测定南极样品中有机氯农药

  • 1. 中国科学院生态环境研究中心, 环境化学与生态毒理学国家重点实验室, 北京, 100085
  • 收稿日期:  2014-05-23
基金项目:

国家海洋局南极科学考察项目(2011GW02003)

国家自然科学基金项目(41276195,21277165, 21107121)

中国科学院战略性先导科技专项(B类)(XDB14010100)资助.

摘要: 建立了同位素稀释-高分辨气相色谱/高分辨质谱法(HRGC/HRMS)测定南极土壤、苔藓和地衣样品中23种有机氯农药的分析方法.样品经冷冻干燥、研磨处理后用正己烷:二氯甲烷(1:1, V:V)混合溶剂进行加速溶剂萃取(ASE),萃取液经硅胶-氧化铝层析柱和C18小柱净化后,进HRGC/HRMS检测分析.样品中目标物定量采用平均相对响应因子法,6点标准曲线响应因子的相对标准偏差(RSD)≤20%,方法的线性范围为0.4—800 μg·L-1,回收率在62%—101%之间.实际样品分析结果表明,23种OCPs的加标回收率为40%—100%,在土壤、苔藓和地衣样品中的检出限(LODs)分别为0.024—5.01、0.2—12.2、0.020—13.7 pg·g-1,可以满足南极环境样品中有机氯农药的检测分析.

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