加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱测定土壤和沉积物中8种多溴联苯醚
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摘要
建立了土壤和沉积物中8种多溴联苯醚(PBDEs,BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154、BDE-183和BDE-209)加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱(ASE-GC-MS-MS)的分析方法。通过优化加速溶剂萃取与弗罗里硅土在线净化和串联质谱多反应监测模式的条件,较好地去除基质干扰,并提高了三重四极杆串联质谱定性的准确性及定量的灵敏性。该方法采用改进的色谱柱能同时分析包括高溴代联苯醚BDE-209在内的8种PBDEs,其浓度范围为1～100 ng/mL(BDE-209为10～1 000 ng/mL),线性良好,线性回归系数均大于0.997。方法检出限为0.004～0.1 ng/g,方法回收率为75%～110%,方法精密度为2.4%～15.6%。适于批量处理土壤和沉积物中含有多组分痕量PBDEs的样品。
A synchronous extraction and purification method using accelerated solvent extraction gas chromatography-triple quadrupole mass spectrometry was developed for the determination of eight polybrominated diphenyl ethers(PBDEs) in soil and sediment, including BDE-28, BDE-47, BDE-99, BDE-100, BDE-153, BDE-154, BDE-183 and BDE-209. The samples from optimization for accelerated solvent extraction were purified by on-line clean-up of activated Florisil during PBDE extraction, combined with the multiple-reaction monitor modes of tandem mass spectrometry, so the background disturbing noise was reduced a lot and the qualitative and quantitative accuracy was improved. Eight PBDEs including high brominated diphenyl ethers(BDE-209) were analyzed synchronously by using improved chromatographic column, The good linear relationships were obtained with coefficient more than 0.997 in the range of 1 ng/mL to 100 ng/mL(10-1000 ng/mL for BDE-209)for eight PBDEs. The method detection limit, recoveries and relative standard deviation ranged from 0.004-0.1 ng/g, 75% to 110% and 2.4% to 15.6%, respectively. This method was suitable for processing a large batch of samples of trace PBDEs in soil and sediment.
A synchronous extraction and purification method using accelerated solvent extraction gas chromatography-triple quadrupole mass spectrometry was developed for the determination of eight polybrominated diphenyl ethers(PBDEs) in soil and sediment, including BDE-28, BDE-47, BDE-99, BDE-100, BDE-153, BDE-154, BDE-183 and BDE-209. The samples from optimization for accelerated solvent extraction were purified by on-line clean-up of activated Florisil during PBDE extraction, combined with the multiple-reaction monitor modes of tandem mass spectrometry, so the background disturbing noise was reduced a lot and the qualitative and quantitative accuracy was improved. Eight PBDEs including high brominated diphenyl ethers(BDE-209) were analyzed synchronously by using improved chromatographic column, The good linear relationships were obtained with coefficient more than 0.997 in the range of 1 ng/mL to 100 ng/mL(10-1000 ng/mL for BDE-209)for eight PBDEs. The method detection limit, recoveries and relative standard deviation ranged from 0.004-0.1 ng/g, 75% to 110% and 2.4% to 15.6%, respectively. This method was suitable for processing a large batch of samples of trace PBDEs in soil and sediment.
引文
[1] 王维,周俊丽,裴淑玮,等.多溴联苯醚在环境中的污染现状研究进展[J].环境化学,2014,33(7):1 084-1 093.WANG Wei,ZHOU Junli,PEI Shuwei,et al.Research Progress on Status of Environmental Pollutions of Polybrominated Diphenyl Ethers[J].Environmental Chemistry,2014,33(7):1 084-1 093.
[2] SYLWIA K,ZABIEGALA B,JACEK N.PBDEs in Environmental Samples:Sampling and Analysis[J].Talanta,2012,1(48):1-17.
[3] JAIME N M,ROQUE S,FéLIX H.Gas Chromatography-Mass Spectrometric Determination of Polybrominated Biphenyl Ethers in Complex Fatty Matrices from Aquaculture Activities[J].Analytica Chimica Acta,2010,664:190-198.
[4] 杨芳,张宪臣,卢俊文,等.气相色谱-质谱法测定水中多溴联苯醚残留量[J].食品科学,2016,37(16):254-257.YANG Fang,ZHANG Xianchen,LU Junwen,et al.Determination of Polybrominated Diphenyl Ethers Residues in Water by Gas Chromatography-Mass Spectrometry[J].Food Science,2016,37(16):254-257.
[5] 郑晓燕,于建钊,许秀艳,等.同位素稀释-高分辨气相色谱/高分辨质谱法测定大气中多溴联苯醚和多溴联苯153[J].色谱,2015,33(10):1 071-1 079.ZHENG Xiaoyan,YU Jianzhao,XU Xiuyan,et al.Determination of Atmospheric Polybrominated Diphenyl Ethers and Polybrominated Biphenyl 153 Using Isotope Dilution-High Resolution Gas Chromatography-High Resolution Mass Spectrometry[J].Chinese Journal of Chromatography,2015,33(10):1 071-1 079.
[6] 卢俊文,张宪臣,杨芳,等.QuEChERS-气相色谱-串联质谱法测定蔬菜中多溴联苯和多溴联苯醚[J].食品科学,2017,38(12):253-259.LU Junwen,ZHANG Xianchen,YANG Fang,et al.Rapid Quantification of 20 Polybrominated Biphenyls (PBBs) and Polybrominated Diphenyl Ethers (PBDEs) in Vegetables Using QuEChERS Coupled with Gas Chromatography-Tandem Mass Spectrometry[J].Food Science,2017,38(12):253-259.
[7] USEPA.Brominated Diphenyl Ethers in Water,Soil,Sediment,and Tissue by HRGC/HRMS:Method1614A[S].[2010-05-20].https://nepis.epa.gov/Exe/ZyPURL.cgi?Dockey=P100IKK7.txt.
[8] 生态环境部科技标准司.土壤和沉积物多溴二苯醚的测定气相色谱-质谱法:HJ 952—2018[S].北京:中国环境出版社,2018.
[9] ARIEL R F,ALEJANDR C,LUIS D M.Dispersive Solid-Phase Extraction as a Simplified Clean-Up Technique Forbiological Sample Extracts.Determination of Polybrominated Diphenyl Ethers by Gas Chromatography-Tandem Mass Spectrometry[J].Journal of Chromatography A,2011,1 218:2 490-2 496.
[10] UTE R T,BENJAMIN A,MUSA B,et al.Method Optimization to Measure Polybrominated Diphenyl Ether (PBDE) Concentrations in Soils of Bratislava,Slovakia[J].Environmental Pollution,2010,158:2 208-2 217.
[11] ZHANG Z L,EHIMAI O,STEWART M R.Simultaneous Extraction and Clean-Up of Diphenyl Ethers and Polychlorinated Biphenyls from Sheep Liver Tissue by Selective Pressurized Liquid Extraction and Analysis by Gas Chromatography-Mass Spectrometry[J].Journal of Chromatography A,2011,1 218:1 203-1 209.
[12] LABADIEA P,ALLIOT F,BOURGES C.Determination of Polybrominated Diphenyl Ethers in Fish Tissues by Matrix Solid-Phase Dispersion and Gas Chromatography Coupled to Triple Quadrupole Mass Spectrometry:Case Study on European Eel (Anguilla anguilla) from Mediterranean Coastal Lagoons[J].Analytica Chimica Acta,2010,675:97-105.
[13] SONG W L,LI A,FORD J C,et al.Polybrominated Diphenyl Ethers in the Sediments of the Great Lakes.2.Lakes Michigan and Huron[J].Environmental Science & Technology,2005,39(10):3 474-3 479.
[14] 余彬彬,牛禾,徐方曦,等.测量土壤中多溴联苯和多溴联苯醚含量不确定度评定[J].中国环境监测,2017,33(1):121-126.YU Binbin,NIU He,XU Fangxi,et al.Evaluation on the Uncertainty in Determination of Polybrominated Biphenyls and Polybrominated Diphenyl Ethers in Soil Using Gas-Chromatography Mass Spectrometry[J].Environmental Monitoring in China,2017,33(1):121-126.
[15] 相雷雷,宋洋,卞永荣,等.土壤中10种多溴联苯醚的加速溶剂-固相萃取净化方法优化研究[J].分析化学,2016,44(5):671-677.XIANG Leilei,SONG Yang,BIAN Yongrong,et al.A Purification Method for Determination of 10 Polybrominated Diphenyl Ethers in Soil Using Accelerated Solvent Extraction-Solid Phase Extraction[J].Chinese Journal of Analytical Chemistry,2016,44(5):671-677.
[16] 梁淑轩,李立勇,张国峰,等.微波辅助萃取-气相色谱质谱法检测生物体内的多溴联苯醚[J].分析试验室,2010,29(4):115-118.LIANG Shuxuan,LI Liyong,ZHANG Guofeng,et al.Determination of Polybrominated Diphenyl Ethers in Biota by Microwave-Assisted Extraction and Gas Chromatography-Mass Spectrometry[J].Chinese Journal of Analysis Laboratory,2010,29(4):115-118.
[17] 张莉莉,彭淑女,赵汝松,等.食品中多溴联苯醚残留的气相色谱-串联质谱分析方法研究[J].分析测试学报,2010,29(6):603-607.ZHANG Lili,PENG Shunü,ZHAO Rusong,et al.Study on the Analysis of PBDEs Residues in Food by Gas Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2010,29(6):603-607.
[2] SYLWIA K,ZABIEGALA B,JACEK N.PBDEs in Environmental Samples:Sampling and Analysis[J].Talanta,2012,1(48):1-17.
[3] JAIME N M,ROQUE S,FéLIX H.Gas Chromatography-Mass Spectrometric Determination of Polybrominated Biphenyl Ethers in Complex Fatty Matrices from Aquaculture Activities[J].Analytica Chimica Acta,2010,664:190-198.
[4] 杨芳,张宪臣,卢俊文,等.气相色谱-质谱法测定水中多溴联苯醚残留量[J].食品科学,2016,37(16):254-257.YANG Fang,ZHANG Xianchen,LU Junwen,et al.Determination of Polybrominated Diphenyl Ethers Residues in Water by Gas Chromatography-Mass Spectrometry[J].Food Science,2016,37(16):254-257.
[5] 郑晓燕,于建钊,许秀艳,等.同位素稀释-高分辨气相色谱/高分辨质谱法测定大气中多溴联苯醚和多溴联苯153[J].色谱,2015,33(10):1 071-1 079.ZHENG Xiaoyan,YU Jianzhao,XU Xiuyan,et al.Determination of Atmospheric Polybrominated Diphenyl Ethers and Polybrominated Biphenyl 153 Using Isotope Dilution-High Resolution Gas Chromatography-High Resolution Mass Spectrometry[J].Chinese Journal of Chromatography,2015,33(10):1 071-1 079.
[6] 卢俊文,张宪臣,杨芳,等.QuEChERS-气相色谱-串联质谱法测定蔬菜中多溴联苯和多溴联苯醚[J].食品科学,2017,38(12):253-259.LU Junwen,ZHANG Xianchen,YANG Fang,et al.Rapid Quantification of 20 Polybrominated Biphenyls (PBBs) and Polybrominated Diphenyl Ethers (PBDEs) in Vegetables Using QuEChERS Coupled with Gas Chromatography-Tandem Mass Spectrometry[J].Food Science,2017,38(12):253-259.
[7] USEPA.Brominated Diphenyl Ethers in Water,Soil,Sediment,and Tissue by HRGC/HRMS:Method1614A[S].[2010-05-20].https://nepis.epa.gov/Exe/ZyPURL.cgi?Dockey=P100IKK7.txt.
[8] 生态环境部科技标准司.土壤和沉积物多溴二苯醚的测定气相色谱-质谱法:HJ 952—2018[S].北京:中国环境出版社,2018.
[9] ARIEL R F,ALEJANDR C,LUIS D M.Dispersive Solid-Phase Extraction as a Simplified Clean-Up Technique Forbiological Sample Extracts.Determination of Polybrominated Diphenyl Ethers by Gas Chromatography-Tandem Mass Spectrometry[J].Journal of Chromatography A,2011,1 218:2 490-2 496.
[10] UTE R T,BENJAMIN A,MUSA B,et al.Method Optimization to Measure Polybrominated Diphenyl Ether (PBDE) Concentrations in Soils of Bratislava,Slovakia[J].Environmental Pollution,2010,158:2 208-2 217.
[11] ZHANG Z L,EHIMAI O,STEWART M R.Simultaneous Extraction and Clean-Up of Diphenyl Ethers and Polychlorinated Biphenyls from Sheep Liver Tissue by Selective Pressurized Liquid Extraction and Analysis by Gas Chromatography-Mass Spectrometry[J].Journal of Chromatography A,2011,1 218:1 203-1 209.
[12] LABADIEA P,ALLIOT F,BOURGES C.Determination of Polybrominated Diphenyl Ethers in Fish Tissues by Matrix Solid-Phase Dispersion and Gas Chromatography Coupled to Triple Quadrupole Mass Spectrometry:Case Study on European Eel (Anguilla anguilla) from Mediterranean Coastal Lagoons[J].Analytica Chimica Acta,2010,675:97-105.
[13] SONG W L,LI A,FORD J C,et al.Polybrominated Diphenyl Ethers in the Sediments of the Great Lakes.2.Lakes Michigan and Huron[J].Environmental Science & Technology,2005,39(10):3 474-3 479.
[14] 余彬彬,牛禾,徐方曦,等.测量土壤中多溴联苯和多溴联苯醚含量不确定度评定[J].中国环境监测,2017,33(1):121-126.YU Binbin,NIU He,XU Fangxi,et al.Evaluation on the Uncertainty in Determination of Polybrominated Biphenyls and Polybrominated Diphenyl Ethers in Soil Using Gas-Chromatography Mass Spectrometry[J].Environmental Monitoring in China,2017,33(1):121-126.
[15] 相雷雷,宋洋,卞永荣,等.土壤中10种多溴联苯醚的加速溶剂-固相萃取净化方法优化研究[J].分析化学,2016,44(5):671-677.XIANG Leilei,SONG Yang,BIAN Yongrong,et al.A Purification Method for Determination of 10 Polybrominated Diphenyl Ethers in Soil Using Accelerated Solvent Extraction-Solid Phase Extraction[J].Chinese Journal of Analytical Chemistry,2016,44(5):671-677.
[16] 梁淑轩,李立勇,张国峰,等.微波辅助萃取-气相色谱质谱法检测生物体内的多溴联苯醚[J].分析试验室,2010,29(4):115-118.LIANG Shuxuan,LI Liyong,ZHANG Guofeng,et al.Determination of Polybrominated Diphenyl Ethers in Biota by Microwave-Assisted Extraction and Gas Chromatography-Mass Spectrometry[J].Chinese Journal of Analysis Laboratory,2010,29(4):115-118.
[17] 张莉莉,彭淑女,赵汝松,等.食品中多溴联苯醚残留的气相色谱-串联质谱分析方法研究[J].分析测试学报,2010,29(6):603-607.ZHANG Lili,PENG Shunü,ZHAO Rusong,et al.Study on the Analysis of PBDEs Residues in Food by Gas Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2010,29(6):603-607.
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