同位素稀释-气相色谱-高分辨双聚焦磁质谱法测定土壤中毒杀芬的含量
Determination of Toxaphenes in Soil by High-Resolution Double-Focusing Magnetic MS Combined with Isotope Dilution and GC
摘 要
提出了同位素稀释-气相色谱-高分辨质谱法测定土壤样品中3种指示性毒杀芬Parlar26(P26)、Parlar50(P50)和Parlar62(P62)。以二氯甲烷-丙酮(1+1)混合液为提取溶剂对土壤样品进行微波萃取,提取液经活化硅胶柱净化分离,洗脱液经氮气吹扫浓缩至100 μL后,以13C12-PCB153为同位素内标,在DB-5MS色谱柱上分离,质谱中采用电子轰击离子源。P26、P50和P62的检出限(3.143S)分别为1,3,5 pg,测定值的相对标准偏差(n=5)小于6%。方法用于某地区表层土壤中3种指示性毒杀芬的检测,测得P26,P50,P62的含量分别为0.08,0.04,0.03 ng·g-1。
气相色谱法
双聚焦磁质谱法
毒杀芬
土壤
Isotope dilution
GC
High-resolution double-focusing magnetic MS
Toxaphene
Soil
Abstract
A novel method for the determination of 3 indicative toxaphenes comprised of Parlar26 (P26), Parlar50 (P50) and Parlar62 (P62) in soil was proposed, based on high-resolution double-focusing magnetic MS combined with isotope dilution and GC. The sample was treated by microwave assisted extraction with a mixture (1+1) of dichloromethane and acetone as solvent. The extract was then purified on an activated silica gel column. The eluate was concentrated to 100 μL by N2-blowing, 13C12-PCB153 was added as internal standard, and the solution was separated on a DB-5MS column. EI was adopted in MS. The detection limits (3.143S) of P26, P50 and P62 were 1, 3, 5 pg, respectively. RSDs (n=5) were all less than 6%. The method was used to determine P26, P50 and P62 in a top soil sample, giving results of 0.08,0.04 ,0.03 ng·g-1, respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201601002
所属栏目 试验与研究
基金项目 江苏省环境监测科研基金项目(1415)
收稿日期 2015/1/18
修改稿日期
网络出版日期
作者单位点击查看
联系人作者王荟(wh_nju@163.com)
备注王荟(1976-),女,江苏宿迁人,高级工程师,硕士, 主要从事有机污染物分析与研究。
引用该论文: WANG Hui,GAO Zhan-qi,ZHANG Yong,HU Guan-jiu. Determination of Toxaphenes in Soil by High-Resolution Double-Focusing Magnetic MS Combined with Isotope Dilution and GC[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(1): 7～10
王荟,高占啟,章勇,胡冠九. 同位素稀释-气相色谱-高分辨双聚焦磁质谱法测定土壤中毒杀芬的含量[J]. 理化检验－化学分册, 2016, 52(1): 7～10
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【4】WITTE J, BUTHE A, TERNES W. Congener-specific analysis of toxaphene in eggs of seabirds from Germany by HRGC-NCI-MS using a carborane-siloxane copolymer phase (HT-8)［J］. Chemosphere, 2000,41:529-539.
【5】GAO Y, ZHANG H J, CHEN H P, et al. Optimized cleanup method for the determination of short chain polychlorinated n-alkanes in sediments by high resolution gas chromatography electron capture negative ion-low resolution mass spectrometry［J］. Analytica Chimica Acta, 2011,703:187-193.
【6】JAMES C Y, ANNE D F, ROBERT M A, et al. Comparing the mutagenicity of toxaphene after aging in anoxic soils and accumulating in fish［J］. Ecotoxicology and Environmental Safety, 2009,72:162-172.
【7】吴欣江.三种POPs物质与环境致突变物苯并［a］芘的联合遗传毒性研究［J］.华中科技大学学报, 2002,267(5):134-142.
【8】VEYRAND B, VENISSEAU A, MARCHAND P, et al. Determination of toxaphene specific congeners in fish liver oil and feeding stuff using gas chromatography coupled to high resolution mass spectrometry［J］. Journal of Chromatography B, 2008,865:121-126.
【9】JOHN R, ADRIAN R W, VINCENT L M, et al. Measurement of toxaphene congeners in pooled human serum collected in three U.S. cities using high-resolution mass spectrometry［J］. Arch Environ Contam Toxicol, 2004,46:551-556.
【10】邓力,余轶松.同位素稀释-高分辨气相色谱-高分辨质谱法测定土壤和沉积物中27种有机氯农药［J］.理化检验-化学分册, 2015,51(7):907-913.
【11】BRAEKEVELT E, TOMY G T, GARY A. Comparison of an individual congener standard and a technical mixture for the quantification of toxaphene in environmental matrices by HRGC ECNI-HRM［J］. Environ Sci Technol, 2001,35:3513-3518.
【12】刘志斌,张建清,蒋友胜,等.同位素稀释-气相色谱/高分辨质谱法测定食品中的指示性毒杀芬［J］.食品安全质量检测学报, 2014,5(2):475-484.
【13】田绍琼,毛秀红,苗水,等.气相色谱-串联质谱法测定人参和黄芪中7种毒杀芬残留量［J］.色谱, 2012,30(1):14-20.
【14】张兵,吴嘉嘉,刘国瑞,等.同位素稀释-气相色谱-串联质谱法测定土壤中的指示性毒杀芬［J］.色谱, 2010,28(5):456-458.
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