高分辨气相色谱-高分辨质谱法(HRGC/HRMS)分析环境样品中二噁英类物质前处理技术探讨  

Discussion on the Pretreatment Techniques for the Analysis of Dioxins from Environmental Samples by High Resolution Gas Chromatography and High Resolution Mass Spectrometry(HRGC/HRMS)

作　　者：冉艳琼 曹阳 黄芸 鲜文婷 熊杰 RAN Yan-qiong;CAO Yang;HUANG Yun;XIAN Wen-ting;XIONG Jie(SiChuan Ecological&Environmental Monitoring Center,Chengdu 610091,China)

机构地区：[1]四川省生态环境监测总站,成都610091

出　　处：《四川环境》2022年第4期1-6,共6页Sichuan Environment

基　　金：四川省生态环境厅环境保护科技项目(2019HB04)。

摘　　要：为解决环境样品中二噁英类物质分析前处理过程中技术难度大、周期长、试剂用量大、操作安全性等相关问题。采用高分辨气相色谱-高分辨质谱法(HRGC/HRMS)对分别经快速溶剂萃取和索式提取后,再通过LCTech全自动净化、手动净化和半自动净化净化三种净化方式处理后的样品进行分析。结果显示:采用快速溶解萃取或索氏提取两种提取方法对二噁英类土壤标准样品进行测定准确度分别在-0. 8~4. 5和-9. 6~19. 3之间,均在±20%以内,二噁英提取内标的回收率均在72%以上,因此两种提取方式提取效率基本一致,但快速溶解萃取相比索氏提取试剂用量更少,前处理周期更短,实验室安全性能更高。采用全自动净化、手动净化、半自动净化三种方法对某垃圾焚烧厂周边实际土壤样品进行测定回收率分别为79%~107%,63%~96%,63%~83%,采用全自动净化方式的回收率整体上优于手动净化和半自动净化,且全自动净化方式单个样品耗时更短、自动化程度高,操作简单,试剂用量少,安全性能高。结果表明采用快速溶剂萃取的方法和全自动净化相结合的方式进行前处理能够更简便、高效、准确安全的进行环境样品中二噁英类物质的前处理,对分析、改进二噁英类污染物监测技术必将起到基础性支撑作用。In order to solve the relative problems about the dioxins from environmental samples in the process of pre-treatment,such as technical difficulties,long cycle,large reagent dosage and operation safety,etc,HRGC/HRMS was used to analyze the samples treated by three purification methods in this paper:LCTech full automatic purification,manual purification and semi-automatic purification after fast solvent extraction and Soxhlet extraction respectively.The results showed that the accuracy of the determination of dioxins soil standard samples by fast solvent extraction or Soxhlet extraction were around-0.8~4.5 and-9.6~19.3,both of which were within±20%,and the internal standard recovery rate of dioxins extraction was above 72%.Therefore,the extraction efficiency of the two extraction methods was basically the same.However,the amount reagent usage of the fast solvent extraction was less,the pre-treatment period is shorter and the laboratory safety performance is higher than Soxhlet extraction.Three methods of fully automatic purification,manual purification and semi-automatic purification were used to determine the actual soil samples around a waste incineration plant,and the recovery rates were 79%~107%,63%-96%and 63%~83%,respectively.The recovery rate of fully automatic purification was better than manual purification and semi-automatic purification.In addition,the single sample by automatic purification method takes shorter time,has high degree of automation,requires simple operation,consumes less reagent and has higher safety performance.The results showed that the combination of the fast solvent extraction method and the fully automatic purification method can make the pretreatment of dioxin from environmental samples more simple,efficient,accurate and safe.It will play a fundamental role in the analysis and improvement of dioxin monitoring technology.

关 键 词：二噁英类 高分辨气相色谱-质谱法 前处理 快速溶剂萃取 索式提取 净化 

分 类 号：X132[环境科学与工程—环境科学]