气相色谱-三重四极杆质谱法测定地下水中44种有机物污染物  

Determination of 44 Organic Pollutants in Groundwater by Gas Chromatography-Triple Quadrupole Mass Spectrometry

作　　者：余蕾 张小毅[1] YU Lei;ZHANG Xiao-yi(Xinjiang Research Institute of Mineral Resources,Urumuqi 830000,China)

机构地区：[1]新疆维吾尔自治区矿产实验研究所,新疆乌鲁木齐830000

出　　处：《岩矿测试》2021年第3期365-374,共10页Rock and Mineral Analysis

基　　金：中国地质环境监测院国家地下水监测工程运行维护项目(WKZB1911BJM300259)。

摘　　要：地下水中有机氯、多环芳烃、邻苯二甲酸酯等半挥发性有机污染物对生态环境和人体健康带来潜在威胁,开发高效、准确、快速的检测方法具有现实意义。通过液液萃取、固相萃取等方式将水中有机污染物分类萃取,利用气相色谱、气相色谱-质谱、液相色谱-质谱等方法测定,不能在满足低检出限的同时测定多种类别有机污染物。本文建立了一种改进的QuECHERS方法,即在水样中加入少量有机溶剂振荡后直接取有机相,无需净化,利用灵敏度更高的气相色谱-三重四极杆质谱仪多反应监测模式(MRM)进行定性、内标法定量,实现了44种有机污染物的同时测定。实验优化了质谱条件,对比了不同溶剂的提取效果以及传统方法和QuECHERS的优缺点。结果表明:44种有机物在1~200μg/L范围内线性关系良好,各有机物的检出限和回收率均满足要求。本方法具有前处理简单、检出限低、邻苯二甲酸酯类本底低、多类有机物同时测定等优点,可应用于地下水中痕量有机物的测定和评估。BACKGROUND:Organic pollutants such as organochlorine,polycyclic aromatic hydrocarbons and phthalate in groundwater are potential threats to the ecological environment and human health.The development of efficient,accurate and rapid detection methods has practical significance.The organic pollutants in water are extracted by liquid-liquid extraction and solid-phase extraction,for example,and are determined by gas chromatography,gas chromatography-mass spectrometry,and liquid chromatography-mass spectrometry.It is not possible to measure multiple types of organic pollutants with low detection limits.OBJECTIVES:To establish a rapid and accurate method for simultaneous determination of multiple semi-volatile organic compounds.METHODS:An improved QuECHERS method was proposed to pretreat the sample.The organic phase was taken directly from the water sample after a small amount of organic solvent was added to the water sample without purification.Multi-reaction monitoring mode(MRM)of triple quadrupole mass spectrometer was used for qualitative analysis and internal standard method for quantitative analysis.The improved method achieved the simultaneous determination of 44 organic pollutants.The conditions of mass spectrometry were optimized,the extraction effects of different solvents were compared,and the advantages and disadvantages of traditional methods and QuECHERS were compared.RESULTS:The results showed that the linear relationship of 44 organic compounds was good in the concentration range of 1-200μg/L,and the detection limit and recovery of each organic compound met the requirements.CONCLUSIONS:The method has the advantages of simple pretreatment,high sensitivity,low background of phthalate and simultaneous determination of multiple types of organics and can be effectively applied to the determination and evaluation of trace organic matter in groundwater.

关 键 词：地下水 有机污染物 QUECHERS 气相色谱-三重四极杆质谱法 

分 类 号：O657.63[理学—分析化学] P641[理学—化学]