周玮,张盈,秦立新,段婷婷,陈明贵,魏进.化学通报,2017,80(5):460-465.
超速匀质超声波辅助萃取—气相色谱/质谱法测定沉积物中16种多环芳烃
GC/MS Determination of 16 Polycyclic Aromatic Hydrocarbons in Sediment by High Speed Homogeneous and Ultrasonic Extraction
投稿时间:2016-09-21  修订日期:2016-10-09
DOI:
中文关键词:  多环芳烃  沉积物  气相色谱/质谱法
英文关键词:Polycyclic aromatic hydrocarbons  Sediment  GC/MS
基金项目:贵州省科学技术(黔科合J字LKN[2013]19号;黔科合J字LKN[2013]14号);贵州省科研机构服务企业行动计划项目(黔科合服企[2015]4012号)
作者单位E-mail
周玮 贵州省土壤肥料研究所 232512147@qq.com 
张盈 贵州省植物保护研究所  
秦立新 贵州省植物保护研究所  
段婷婷 贵州省植物保护研究所  
陈明贵 贵州省植物保护研究所  
魏进* 贵州省植物保护研究所 wwjj0084@126.com 
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中文摘要:
      建立了用于检测沉积物中多环芳烃PAHs的超速匀质超声波辅助萃取—气相色谱/质谱法。以乙腈为提取剂对水体沉积物中16种PAHs进行提取,铜粉净化,所得净化液浓缩丙酮定容用Agilent HP-5MS毛细管柱进行分离,质谱全扫描检测。采用质谱检测器根据NIST 05谱图库比对进行定性分析;外标法进行定量分析。结果表明:16种PAHs的检出限在0.004~0.028 μg?kg-1之间。用标准加入法测得回收率在71.3%~117.2%,相对标准偏差(n=7)在1.2%~9.8%之间。通过实际样品中PAHs的分析表明,该法快速、溶剂用量小,满足痕量分析的要求。
英文摘要:
      Abstract:A method for determination of polycyclic aromatic hydrocarbons (PAHs)in sediment by high speed homogeneous ultrasonic extraction and GC/MS was established. 16 polycyclic aromatic hydrocarbons were separated from sediment by high speed homogeneous and ultrasonic extraction with acetonitrile, and the extract was purified by copper powder and 16 PAHs were reconstituted with acetone. Agilent HP-5MS capillary column was used for separation. The identification of the 16 PAHs was performed by comparing spectra obtained by MS detector with NIST 05 atlas database;and quantification was performed by GC/MS using external standard method. Values of detection limit of the method found were in the range of 0.004~0.028 ug.kg-1. Values of recovery found by adding the standards method, were ranged from 71.3 % to 117.2% with relative standard deviations (RSD’s) (n=7) range of 1.2 -9.8 %. The method was used for the determination of trace PAHs in real atmospheric particulate sample, it’s a rapid, efficient and solvent saving method.
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