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

付善良; 陆静; 陈练; 成婧; 朱绍华; 罗芳; 符琼; 易锡; 梁香

环境化学

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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:

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:

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.
- 磁固相萃取 /
- 氧化石墨烯-四氧化三铁 /
- 热脱附-气相色谱-串联质谱
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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[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).
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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

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.

关键词:

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.

English Abstract

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

Corresponding author: FU Shanliang, fsl432@163.com ;

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

Available Online: 2020-02-27

Fund Project: Supported by GAC Project of Science and Technology Program (2017IK117).

Keywords:

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.