同位素稀释-气相色谱高分辨磁质谱法测定土壤中卤代咔唑  

Determination of Halogenated Carbazoles in Soil by Isotope Dilution Gas Chromatography High-resolution Magnetic Mass Spectrometry

作　　者：崔立迁 庞博 李柳佳 石春正 穆丽美 CUI Li-qian;PANG Bo;LI Liu-jia;SHI Chun-zheng;MU Li-mei(Tianjin Product Quality Inspection Technology Research Institute)

机构地区：[1]天津市产品质量监督检测技术研究院

出　　处：《中国标准化》2024年第24期232-238,共7页China Standardization

基　　金：天津市市场监督管理委员会科技计划项目“土壤中卤代咔唑分析方法研究”(项目编号:2021-W12)资助。

摘　　要：卤代咔唑(PHCZs)是一类新型环境持久性有机污染物,因其具有类似二噁英的毒性、环境难降解性和生物体积累性,近年来受到广泛关注。本研究建立了同位素稀释-气相色谱高分辨磁质谱法测定土壤中11种PHCZs的方法,该方法以快速溶剂萃取法提取试样,结合串联硅胶-炭柱净化方法,实现PHCZs的有效净化和准确测定,方法检出限0.40~2.77 pg/g。在不同添加浓度下,PHCZs回收率分别为86.3%~112.5%、90.3%~104.6%、95.3%~107.6%。采用本方法测定垃圾焚烧厂周边土壤样品,结果表明PHCZs总毒性当量为0.0043~1.4 pg TEQ/g dw。Halogenated carbazoles(PHCZs)is a new type of persistent organic pollutant in the environment,which has received widespread attention in recent years due to its toxicity similar to dioxins,environmentally diffi cult degradable,and bioaccumulation.This paper establishes a method for determining 11 types of PHCZs in soil using isotope dilution gas chromatography high-resolution magnetic mass spectrometry(GC-HRMS).The samples are extracted with a rapid solvent extraction device and purifi ed by silica gel/carbon column to achieve eff ective purifi cation and accurate determination of PHCZs.The detection limit of the method is as low as 0.40-2.77 pg/g.For diff erent concentrations,the recovery rates of PHCZs are 86.3%~112.5%,90.3%~104.6%,and 95.3%~107.6%,respectively.The method is used to determine soil samples around a waste incineration plant,and the results show that the total toxic equivalent of PHCZs is 0.0043~1.4 pg TEQ/g dw.

关 键 词：卤代咔唑 持久性有机污染物 同位素稀释 高分辨磁质谱 土壤 

分 类 号：O657.63[理学—分析化学] X833[理学—化学]