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磁固相萃取-热脱附-气相色谱-串联质谱检测水中六氯苯、六六六和滴滴涕

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付善良, 陆静, 陈练, 成婧, 朱绍华, 罗芳, 符琼, 易锡, 梁香. 磁固相萃取-热脱附-气相色谱-串联质谱检测水中六氯苯、六六六和滴滴涕[J]. 环境化学, 2020, (2): 566-569.
引用本文: 付善良, 陆静, 陈练, 成婧, 朱绍华, 罗芳, 符琼, 易锡, 梁香. 磁固相萃取-热脱附-气相色谱-串联质谱检测水中六氯苯、六六六和滴滴涕[J]. 环境化学, 2020, (2): 566-569.
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FU Shanliang, LU Jing, CHEN Lian, CHENG Jing, ZHU Shohua, LUO Fang, FU Qiong, YI Xi, LIANG Xiang. Determination of HCB, BHCs and DDTs residues in water by magnetic solid phase extraction/thermal desorption-gas chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2020, (2): 566-569.
Citation: FU Shanliang, LU Jing, CHEN Lian, CHENG Jing, ZHU Shohua, LUO Fang, FU Qiong, YI Xi, LIANG Xiang. Determination of HCB, BHCs and DDTs residues in water by magnetic solid phase extraction/thermal desorption-gas chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2020, (2): 566-569.
shu

磁固相萃取-热脱附-气相色谱-串联质谱检测水中六氯苯、六六六和滴滴涕

  • 长沙海关技术中心 湖南省检验检疫科学研究院, 长沙, 410004

    • 通讯作者: 付善良, E-mail: fsl432@163.com ; 
  • 基金项目:

    海关总署科技计划项目（2017IK117）资助.

Determination of HCB, BHCs and DDTs residues in water by magnetic solid phase extraction/thermal desorption-gas chromatography-tandem mass spectrometry

  • Technology Center of Changsha Customs, Hunan Academy of Inspection and Quarantine, Changsha, 410004, China

    • Corresponding author: FU Shanliang, fsl432@163.com ; 
  • Fund Project: Supported by GAC Project of Science and Technology Program (2017IK117).

  • 摘要: 利用氧化石墨烯-四氧化三铁（GO-Fe3O4）磁性吸附剂进行磁固相萃取（MSPE），结合在线热脱附-气相色谱-三重四极杆串联质谱系统（TD-GC-MS/MS）建立了一种免有机溶剂的定量检测水中六氯苯、六六六和滴滴涕的方法.优化了GO-Fe3O4的用量、萃取时间及溶液pH等影响磁固相萃取效率的关键因素.在优化的条件下，六氯苯、六六六和滴滴涕在2-100 ng·L-1范围内呈良好线性，线性相关系数（r）大于0.99.检测限（S/N=3）和定量限（S/N=10）分别为0.04-0.26 ng·L-1和0.13-0.86 ng·L-1.2个添加水平的平均回收率为88.1%-105.8%，相对标准偏差（RSD）为2.8%-11.3%.该方法操作简单、快速、灵敏、准确、环保，可用于水样中痕量六氯苯、六六六和滴滴涕污染的监测.
    Abstract: Magnetic solid phase extraction(MSPE) based on Fe3O4-grafted graphene oxide (GO-Fe3O4) was combined with thermal desorption-gas chromatography-tandem mass spectrometry(TD-GC-MS/MS) to develop an organic solvent free quantitative analysis method for the determination of hexachlorobenzene (HCB), hexachlorocyclohexane (BHCs) and dichloro-diphenyl-trichloroethane (DDTs) residues in water. The factors, such as amount of GO-Fe3O4, extraction time and pH of water sample, were investigated. Under the optimized conditions, an excellent linearity was observed in the range of 2-100 ng·L-1, with the correlation coefficients(r)>0.99. The detection limits(S/N=3) and the quantitation limits(S/N=10) were 0.04-0.26 ng·L-1 and 0.13-0.86 ng·L-1, respectively. The mean recoveries at 2 spiked levels ranged from 88.1%-105.8% with the relative standard deviations(RSD) of 2.8%-11.3%.The proposed method was simple, rapid, sensitive, accurate and environmentally friendly, and could be used in the monitoring of trace HCB, BHCs and DDTs contaminants in water sample.
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  • [1] 魏连通, 杨少博, 谢健, 等. 气相色谱法测定水中八种有机氯农药[J]. 贵州科学, 2018, 36(4):80-82.

    WEI L T, YANG S B, XIE J, et al. Determination of 8 organic chloride pesticides in water by gas chromatography[J]. Guizhou Science, 2018, 36(4):80-82(in Chinese).

    [2] 马兴华, 王婷, 黄旭锋, 等. 气相色谱法测定水中六六六和滴滴涕[J]. 河南科学, 2014, 32(3):352-354.

    MA X H, WANG T, HUANG X F, et al. Detemination of BHCs and DDTs in water by gas chromatography[J]. Henan Science, 2014, 32(3):352-354(in Chinese).

    [3] 郭家辰. 固相萃取-气相色谱法同时测定水中的毒死蜱和六氯苯[J]. 净水技术, 2019, 38(4):28-30

    ,45. GUO J C. Simultaneous determination of chlorpyrifos and hexachlorobenzene in tap water by solid phase extraction-gas chromatography[J]. Water Purification Technology, 2019, 38(4):28-30,45(in Chinese).

    [4] 龙素群, 钟志京, 何小波, 等. 水中有机氯农药的固相萃取-气相色谱测定法[J]. 环境与健康杂志, 2010, 27(8):704-706.

    LONG S Q, ZHONG Z J, HE X B, et al. Determination of organochlorine pesticides in water by solid phase extraction-gas chromatography[J]. Journal of Environment and Health,2010, 27(8):704-706(in Chinese).

    [5] 付善良, 丁利, 戴华, 等. 磁固相萃取/气相色谱-质谱法分析水样中的16种邻苯二甲酸酯类化合物[J]. 分析测试学报, 2011, 30(8):847-852.

    FU S L, DING L, DAI H, et al. Determination of 16 phthalate acid esters in water samples by magnetic solid phase extraction/gas chromatography-mass spectrometry[J]. Journal of Instrumental Analysis, 2011, 30(8):847-852(in Chinese).

    [6]
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付善良, 陆静, 陈练, 成婧, 朱绍华, 罗芳, 符琼, 易锡, 梁香. 磁固相萃取-热脱附-气相色谱-串联质谱检测水中六氯苯、六六六和滴滴涕[J]. 环境化学, 2020, (2): 566-569.
引用本文: 付善良, 陆静, 陈练, 成婧, 朱绍华, 罗芳, 符琼, 易锡, 梁香. 磁固相萃取-热脱附-气相色谱-串联质谱检测水中六氯苯、六六六和滴滴涕[J]. 环境化学, 2020, (2): 566-569.
shu
FU Shanliang, LU Jing, CHEN Lian, CHENG Jing, ZHU Shohua, LUO Fang, FU Qiong, YI Xi, LIANG Xiang. Determination of HCB, BHCs and DDTs residues in water by magnetic solid phase extraction/thermal desorption-gas chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2020, (2): 566-569.
Citation: FU Shanliang, LU Jing, CHEN Lian, CHENG Jing, ZHU Shohua, LUO Fang, FU Qiong, YI Xi, LIANG Xiang. Determination of HCB, BHCs and DDTs residues in water by magnetic solid phase extraction/thermal desorption-gas chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2020, (2): 566-569.
shu

磁固相萃取-热脱附-气相色谱-串联质谱检测水中六氯苯、六六六和滴滴涕

    通讯作者: 付善良, E-mail: fsl432@163.com ; 
  • 长沙海关技术中心 湖南省检验检疫科学研究院, 长沙, 410004
  • 网络出版日期:  2020-02-27
基金项目:

海关总署科技计划项目（2017IK117）资助.

摘要: 利用氧化石墨烯-四氧化三铁（GO-Fe3O4）磁性吸附剂进行磁固相萃取（MSPE），结合在线热脱附-气相色谱-三重四极杆串联质谱系统（TD-GC-MS/MS）建立了一种免有机溶剂的定量检测水中六氯苯、六六六和滴滴涕的方法.优化了GO-Fe3O4的用量、萃取时间及溶液pH等影响磁固相萃取效率的关键因素.在优化的条件下，六氯苯、六六六和滴滴涕在2-100 ng·L-1范围内呈良好线性，线性相关系数（r）大于0.99.检测限（S/N=3）和定量限（S/N=10）分别为0.04-0.26 ng·L-1和0.13-0.86 ng·L-1.2个添加水平的平均回收率为88.1%-105.8%，相对标准偏差（RSD）为2.8%-11.3%.该方法操作简单、快速、灵敏、准确、环保，可用于水样中痕量六氯苯、六六六和滴滴涕污染的监测.

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