超速匀质超声波辅助萃取-气相色谱/质谱法测定沉积物中多环芳烃

摘要

A method for determination of polycyclic aromatic hydrocarbons (PAHs) in sediment by high speed homogeneous ultrasonic extraction and GC/MS was established.16 kinds of PAHs were separated from sediment by high speed homogeneous and ultrasonic extraction with acetonitrile,and the extracts were purified by copper powder,and 16 PAHs were reconstituted with acetone.Agilent HP-SMS capillary column was used for separation.The identification of the 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.The detection limits of the method were in the range of 0.004 ～0.028 μg· kg-1,and the recoveries were ranged from 71.3％ to 117.2％ with relative standard deviations (RSD) (n =7) of 1.2％ ～ 9.8％.The method was used for the determination of trace PAHs in real samples,and was found to be a rapid,efficient and solvent saving method,which could meet the requirements of analyzing trace analytes.%本文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,然后用铜粉净化,所得净化液经浓缩、丙酮定容后用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,采用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,加标回收率71.3％ ～ 117.2％,相对标准偏差(n=7)在1.2％～9.8％之间.通过对实际样品中PAHs的分析表明,该法检测快速,溶剂用量小,可以满足痕量分析的要求.