Han Yehua, Ren Limin, Xu Kai, Yang Fan, Li Yongfeng, Cheng Tingting, Kang Xiaomeng, Xu Chunming, Shi Quan
State Key Laboratory of Heavy Oil Processing, College of Chemical Engineering, China University of Petroleum, Beijing 102249, China.
State Key Laboratory of Heavy Oil Processing, College of Chemical Engineering, China University of Petroleum, Beijing 102249, China.
J Chromatogr A. 2015 May 22;1395:1-6. doi: 10.1016/j.chroma.2015.03.038. Epub 2015 Mar 24.
A supercritical fluid extraction (SFE) method with an online solid collection trap has been developed for the quantitative analysis of 16 polycyclic aromatic hydrocarbons (PAHs) and 15 typical PAH derivatives in solid matrix. Compared with liquid trapping and C18 solid-phase trapping, multi-walled carbon nanotubes (CNTs) were proved to be the most efficient trapping sorbent for the collection of PAHs and their nitro-, oxy- and alkyl-derivatives. The proposed extraction-collection procedure was systematically optimized in terms of pressure, temperature, extraction time, trapping materials, supercritical fluid flow rate, co-solvent type, and co-solvent percentage, taking into account the interaction between these variables. The whole extraction process could be completed in 15min followed by GC-MS analysis. Quantitative recoveries of PAHs and their derivatives from spiked soil samples (50ngg(-1)) were obtained in the range of 62.9-111.8% with the precisions (RSD, intra-day) ranged from 1.9% to 13.7%. The developed SFE method with online CNTs trapping followed by GC-MS analysis has been demonstrated to be an efficient way for quantitative analysis of trace-level PAHs and their nitro-, oxy-, and alkyl-derivatives in soil samples.
一种带有在线固体收集阱的超临界流体萃取(SFE)方法已被开发出来,用于对固体基质中的16种多环芳烃(PAHs)和15种典型PAH衍生物进行定量分析。与液体捕集和C18固相捕集相比,多壁碳纳米管(CNTs)被证明是收集PAHs及其硝基、氧基和烷基衍生物最有效的捕集吸附剂。考虑到这些变量之间的相互作用,对所提出的萃取 - 收集程序在压力、温度、萃取时间、捕集材料、超临界流体流速、共溶剂类型和共溶剂百分比方面进行了系统优化。整个萃取过程可在15分钟内完成,随后进行GC - MS分析。加标土壤样品(50ng g(-1))中PAHs及其衍生物的定量回收率在62.9 - 111.8%范围内,精密度(日内RSD)在1.9%至13.7%之间。所开发的采用在线CNTs捕集随后进行GC - MS分析的SFE方法已被证明是定量分析土壤样品中痕量PAHs及其硝基、氧基和烷基衍生物的有效方法。