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微波辅助萃取法提取滇池沉积物中的多氯联苯

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万幸, 王彬, 赵世民, 胡平, 李发荣, 潘学军. 微波辅助萃取法提取滇池沉积物中的多氯联苯[J]. 环境化学, 2011, 30(10): 1781-1787.
引用本文: 万幸, 王彬, 赵世民, 胡平, 李发荣, 潘学军. 微波辅助萃取法提取滇池沉积物中的多氯联苯[J]. 环境化学, 2011, 30(10): 1781-1787.
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WAN Xing, WANG Bin, ZHAO Shimin, HU Ping, LI Farong, PAN Xuejun. MICROWAVE-ASSISTED EXTRACTION OF PCBS IN SEDIMENT FROM DIANCHI LAKE[J]. Environmental Chemistry, 2011, 30(10): 1781-1787.
Citation: WAN Xing, WANG Bin, ZHAO Shimin, HU Ping, LI Farong, PAN Xuejun. MICROWAVE-ASSISTED EXTRACTION OF PCBS IN SEDIMENT FROM DIANCHI LAKE[J]. Environmental Chemistry, 2011, 30(10): 1781-1787.
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微波辅助萃取法提取滇池沉积物中的多氯联苯

  • 1.

    昆明理工大学环境科学与工程学院, 昆明, 650093;

  • 2.

    昆明市环境监测中心, 昆明, 650093

  • 基金项目:

    国家自然科学基金(20767002),云南省自然科学基金(2007B035M)和环境化学与生态毒理学国家重点实验室开放基金(KF2008-09号)资助.

MICROWAVE-ASSISTED EXTRACTION OF PCBS IN SEDIMENT FROM DIANCHI LAKE

  • 1.

    Faculty of Environmental Science and Engineering, Kunming University of Science and Technology, Kunming, 650093, China;

  • 2.

    Kunming Environmental Monitoring Center, Kunming, 650228, China

  • Fund Project:

  • 摘要: 研究运用微波辅助萃取-固相萃取-气相色谱/质谱检测滇池沉积物中6种指示性多氯联苯(PCB28,PCB52,PCB101,PCB138,PCB153和PCB180).重点优化了微波辅助萃取技术,在萃取温度为100 ℃和萃取时间为30 min(升温和恒温各15 min)条件下,以30 mL 正己烷∶二氯甲烷(1∶1, V∶V)的混合溶液为萃取溶剂,萃取5 g加标沉积物样品.本方法对PCB28,PCB52,PCB101和PCB138,PCB153,PCB180的线性范围分别为1-3000 pg·g(d.w.)-1和5-3000 pg·g(d.w.)-1,相关系数R2>0.98,检出限和定量限分别为41.7-62.3 pg·g(d.w.)-1、139.0-207.7 pg·g(d.w.)-1.浓度水平为20 ng·g(d.w.)-1的滇池沉积物样品平均加标回收率在75.1%-93.9%之间,相对标准偏差为3.9%-12.8%(n=3).运用该方法对滇池环境样品进行了测定,结果表明滇池表层沉积物已受到多氯联苯的污染.
    Abstract: A method for simultaneous determination of six indicative polychlorinated biphenyls (PCB28, PCB52, PCB101, PCB138, PCB153 and PCB180) in sediments of Dianchi Lake by microwave-assisted extraction (MAE), solid phase extraction (SPE) and gas chromatography-mass spectrometry (GC-MS) detection was developed. Based on systematic optimization of MAE conditions, the most efficient extraction was achieved at 100 ℃ for 30 min (heating for 15 min and then holding for 15 min), using 30 mL of hexane∶DCM (1∶1, V∶V) as the solvent for 5 g sediment sample. Under the optimal conditions, linear range was 1-3000 pg·g(dry weight)-1 for PCB28, PCB52 and PCB101, while 5-3000 pg·g(dry weight)-1 for PCB138, PCB153 and PCB180. The correlation coefficient (R2) was above 0.98 for all the analytes, with the limit of detection (LOD) and the limit of quantification (LOQ) of 41.7-62.3 pg·g(dry weight)-1 and 139.0-207.7 pg·g(dry weight)-1, respectively. The proposed method was further verified by performing spiking experiments in sediment samples at 20 ng·g(dry weight)-1, with the overall recoveries ranging from 75.1% to 93.9% and relative standard deviations (RSD) (n=3) of 3.9%-12.8% for the entire procedure. The proposed method was applied to the determination of PCBs in surface sediment samples from Dianchi Lake, showing that the sediment had been contaminated by PCBs.
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  • [1] Parera J, Santos F J, Galceran M T. Microwave-assisted extraction versus Soxhlet extraction for the analysis of short-chain chlorinated alkanes in sediments [J]. J Chromatogr A, 2004, 1046(1-2):19-26
    [2] Bianco G, Novario G, Bochicchio D, et al. Polychlorinated biphenyls in contaminated soil samples evaluated by GC-ECD with dual-column and GC-HRMS [J]. Chemosphere, 2008, 73(1):104-112
    [3] Rodil R, Carro A M, Lorenzo R A, et al. Multicriteria optimisation of a simultaneous supercritical fluid extraction and clean-up procedure for the determination of persistent organohalogenated pollutants in aquaculture samples [J]. Chemosphere, 2007, 67(7):1453-1462
    [4] Bartolomé L, Cortazar E, Raposo J C, et al. Simultaneous microwave-assisted extraction of polycyclic aromatic hydrocarbons, polychlorinated biphenyls, phthalate esters and nonylphenols in sediments [J]. J Chromatogr A, 2005, 1068(2):229-236
    [5] Ken L, Michael L, Merv F, et al. Accelerated solvent extraction (ASE) of environmental organic compounds in soils using a modified supercritical fluid extractor [J]. J Hazard Mater, 2003,102(1):93-104
    [6] 吴瞻英,饶竹,李夏,等.微波萃取/气相色谱一质谱测定土壤中的多氯联苯[J].分析试验室,2008,27(6):61-63
    [7] 王英,陈晓斌,丛春林. MAE/GC-MS测定底泥中PCBs的研究[J].环境科学与管理,2007,32(7):141-143
    [8] Soporring S, Bwadt S, Svensmark B, et al. Comprehensive comparison of classic soxhlet extraction with soxtec extraction, wltrasonication extraction, supercritical fluid extration, microwave assistex extraction and accelerated solvent extraction for the determination of polychlorinated biphenyls in soil original Research Article[J]. J Chromatogr A, 2005, 1090(1/2):1-9.
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  • 收稿日期:  2010-12-02

微波辅助萃取法提取滇池沉积物中的多氯联苯

  • 1.  昆明理工大学环境科学与工程学院, 昆明, 650093;
  • 2.  昆明市环境监测中心, 昆明, 650093
  • 收稿日期:  2010-12-02
基金项目:

国家自然科学基金(20767002),云南省自然科学基金(2007B035M)和环境化学与生态毒理学国家重点实验室开放基金(KF2008-09号)资助.

摘要: 研究运用微波辅助萃取-固相萃取-气相色谱/质谱检测滇池沉积物中6种指示性多氯联苯(PCB28,PCB52,PCB101,PCB138,PCB153和PCB180).重点优化了微波辅助萃取技术,在萃取温度为100 ℃和萃取时间为30 min(升温和恒温各15 min)条件下,以30 mL 正己烷∶二氯甲烷(1∶1, V∶V)的混合溶液为萃取溶剂,萃取5 g加标沉积物样品.本方法对PCB28,PCB52,PCB101和PCB138,PCB153,PCB180的线性范围分别为1-3000 pg·g(d.w.)-1和5-3000 pg·g(d.w.)-1,相关系数R2>0.98,检出限和定量限分别为41.7-62.3 pg·g(d.w.)-1、139.0-207.7 pg·g(d.w.)-1.浓度水平为20 ng·g(d.w.)-1的滇池沉积物样品平均加标回收率在75.1%-93.9%之间,相对标准偏差为3.9%-12.8%(n=3).运用该方法对滇池环境样品进行了测定,结果表明滇池表层沉积物已受到多氯联苯的污染.

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