自动固相萃取—气相色谱—高分辨质谱法测定地表水中41种持久性有机污染物
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摘要
目的建立同时测定地表水中41种持久性有机污染物的自动固相萃取—气相色谱—高分辨质谱方法(GC-HRMS)。方法地表水样品采用HLB固相萃取柱富集提取,乙酸乙酯和二氯甲烷联合洗脱,氮吹浓缩进样分析。结果 41种持久性有机污染物在(0.10～20.0) ng/L范围内线性关系良好,其相关系数均≥0.997,检出限范围(0.002～0.15) ng/L,定量限范围(0.005～0.51) ng/L,回收率范围70.4%～122.4%,精密度(RSD)范围4.2%～19.4%。结论该方法操作简便,灵敏度高,选择性强,适用于同时测定地表水中41种持久性有机污染物。
Objectives To establish a method for simultaneous determination of 41 persistent organic pollutants in surface water by automatic solid phase extraction-gas chromatography-high resolution mass spectrometry(GC-HRMS). Methods Water samples were extracted by HLB solid phase extraction, extracted with the mixture of dichloromethane and acetic ether, and the final eluate was then concentrated and detected. Results The calibration curves of 41 persistent organic pollutants showed a good linearity in the range of(0.10～20.0) ng/L,and the correlation coefficients were more than 0.997. The detection limits(LOD)of method were in the range of(0.002～0.15) ng/L,and the limits of quanti?cation(LOQ)of method were in the range of(0.005～0.51) ng/L. The spiked recoveries ranged from 70.4%～122.4% and the relative standard deviations ranged from 4.2%～19.4%. Conclusions The method was simple, sensitive, selective and suitable for simultaneous determination of 41 persistent organic pollutants in surface water.
Objectives To establish a method for simultaneous determination of 41 persistent organic pollutants in surface water by automatic solid phase extraction-gas chromatography-high resolution mass spectrometry(GC-HRMS). Methods Water samples were extracted by HLB solid phase extraction, extracted with the mixture of dichloromethane and acetic ether, and the final eluate was then concentrated and detected. Results The calibration curves of 41 persistent organic pollutants showed a good linearity in the range of(0.10～20.0) ng/L,and the correlation coefficients were more than 0.997. The detection limits(LOD)of method were in the range of(0.002～0.15) ng/L,and the limits of quanti?cation(LOQ)of method were in the range of(0.005～0.51) ng/L. The spiked recoveries ranged from 70.4%～122.4% and the relative standard deviations ranged from 4.2%～19.4%. Conclusions The method was simple, sensitive, selective and suitable for simultaneous determination of 41 persistent organic pollutants in surface water.
引文
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[8]陆一夫,胡小键,丁昌明,等.地表水中23种有机氯农药的自动固相萃取-气相色谱-高分辨质谱联用测定法[J].环境与健康,2017,34(2):146-148.(In English:Lu YF,Hu XJ,Ding CM,et al.Determination of 23 organochlorine pesticides in surface water by automatic solid phase extraction-gas chromatography-high resolution mass spectrometry[J].J Environ Health,2017,34(2):146-148.)
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[2]刘明和.有机氯在我国的污染现状及监控对策[J].内蒙古环境保护,2003,15(1):35-38.(In English:Liu MH.Persistent organic chorine pollutants and monitoring method in China[J].Inner Mongolia Environ Prot,2003,15(1):35-38.)
[3]联合国环境规划署.关于对持久性有机污染物的斯德哥尔摩公约[EB/OL].(2001-05-22).https://www.un.org/zh/documents/treaty/files/WIPO-2001.shtml.
[4]Rezaei F,Bidari A,Birjandi AP,et al.Development of a dispersive liquid-liquid microextraction method for the determination of polychlorinated biphenyls in water[J].J Hazard Mater,2008,158(2-3):621-627.
[5]Namies'nik J,Zygmunt B.Selected concentration techniques for gas chromatographic analysis of environmental samples[J].Chromatographia,2002,56(1):S9-S18.
[6]赵云峰,陈建民,王绪卿.有机氯农药多残留GC-MS分析方法研究[J].卫生研究,1998,27(6):425-428.(In English:Zhao YF,Chen JM,Wang XQ.Study on the analytical method for organochlorine pesticide residue using gas chromatographymass spectrometry[J].J Hyg Res,1998,27(6):425-428.)
[7]陈弘丽,潘锦,彭红.气相色谱-质谱联用测定饮用水源中半挥发性有机物[J].福建分析测试,2013,22(2):54-57.(In English:Chen HL,Pan J,Peng H.Determination of semivolatile organic compounds in source water by GC-MS[J].Fujian Anal Test,2013,22(2):54-57.)
[8]陆一夫,胡小键,丁昌明,等.地表水中23种有机氯农药的自动固相萃取-气相色谱-高分辨质谱联用测定法[J].环境与健康,2017,34(2):146-148.(In English:Lu YF,Hu XJ,Ding CM,et al.Determination of 23 organochlorine pesticides in surface water by automatic solid phase extraction-gas chromatography-high resolution mass spectrometry[J].J Environ Health,2017,34(2):146-148.)
[9]Haynes D,Mosse P,Oswald L.The use of transplanted cultured mussels(Mytilus edulis)to monitor pollutants along the ninety mile beach,Victoria,Australia-Ⅱ.Polychlorinated dibenzo-pdioxins and dibenzofurans[J].Mar Pollut Bull,1995,30(12):834-839.
[10]US EPA.Method 8080A Organochlorine pesticides and polychlorinated biphenyls by gas chromatography[S].Washington DC:United States Environmental Protection Agency,1994.
[11]US EPA.Method 1668C Chlorinated biphenyl congeners in water,soil,sediment,biosolids,and tissue by HRGC/HRMS[S].Washington DC:United States Environmental Protection Agency,2010.
[12]国家环境保护总局,国家质量监督检验检疫总局.GB 3838-2002地表水环境质量标准[S].北京:中国环境科学出版社,2002.(In English:State Environmental Protection Administration,State Administration of Quality Supervision,Inspection and Quarantine.GB 3838-2002 Environmental quality standards for surface water[S].Beijing:China Environmental Science Press,2002.
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