固相萃取-气相色谱-质谱法测定原水和饮用水中的18种多氯联苯  

Determination of 18 Types of Polychlorinated Biphenyls for Raw Water and Drinking Water by Solid Phase Extraction-Gas Chromatography-Mass Spectrometry

作　　者：吴艳龙 张琪雨 冯秋仪 张祥汉 任柯柯 WU Yanlong;ZHANG Qiyu;FENG Qiuyi;ZHANG Xianghan;REN Keke(Zhuhai Water Supply and Drainage Pollution Control Center,Zhuhai 519000,China)

机构地区：[1]珠海市供水与排水治污中心,广东珠海519000

出　　处：《净水技术》2025年第3期193-200,共8页Water Purification Technology

基　　金：广东省自然科学基金项目(2021A1515010365)。

摘　　要：【目的】为提高固相萃取-气相色谱-质谱法测定水源水和生活饮用水中多氯联苯(PCBs)的回收率与检测效率,文章建立了应用固相萃取-气相色谱串联质谱同时测定水源水和生活饮用水中18种PCBs的分析方法。【方法】样品经调整活化步骤的HLB固相萃取小柱萃取后,浓缩直接进气相色谱-质谱联用仪进行分析,使用电子轰击电离源电离,Agilent HP-5ms色谱柱(长为30 m,内径为0.25 mm,膜厚度为0.25μm)进行分离,选择离子检测模式进行扫描。【结果】结果显示:18种PCBs在0.05~200.00μg/L的不同线性范围均呈现良好的线性关系(相关系数=0.9979~0.9994),方法检出限为0.029~1.300 ng/L。对水源水(加标60 ng/L)和出厂水(加标30 ng/L)实际样品的18种PCBs加标回收率分别为65.5%~108.0%和81.3%~131.0%。测定低质量浓度(40 ng/L)、中质量浓度(100 ng/L)、高质量浓度(160 ng/L)纯水加标样品的相对误差分别为-4.5%~5.0%、-5.9%~8.0%和-6.3%~8.1%,相对标准偏差分别为1.5%~9.4%、1.7%~13.0%和2.0%~12.0%。【结论】该检测方法灵敏度能满足《生活饮用水卫生标准》(GB 5749—2022)标准限值要求,具有操作简单、效率高、灵敏度高等优点,适用于水源水和生活饮用水中多氯联苯的检测。[Objective]In order to improve the recovery and detection efficiency of polychlorinated biphenyls(PCBs)in source water and drinking water using solid-phase extraction gas chromatography-mass spectrometry,this paper established an analytical method for simultaneously determining 18 types of PCBs in source water and drinking water using solid-phase extraction gas chromatography-mass spectrometry.[Methods]After adjusting the activation steps,the sample was extracted by HLB solid-phase extraction small column and concentrated for analysis by gas chromatography-mass spectrometry.The sample was ionized using an electron impact ionization source and separated using an Agilent HP-5 ms chromatography column(30 m,0.25 mm inner diameter,0.25μm membrane thickness).Scanning was conducted in selected ion monitoring mode.[Results]Result revealed that the 18 types of polychlorinated biphenyls exhibited excellent linear relationships within the range of 0.05μg/L to 200.00μg/L(related coefficient is 0.9979 to 0.9994),with detection limits ranging from 0.029 ng/L to 1.300 ng/L.The recovery rates for the actual samples of source water(spiked at 60 ng/L)and finished water(spiked at 30 ng/L)spiked with 18 types of PCBs were 65.5%to 108.0%and 81.3%to 131.0%,respectively.The relative errors for the low(40 ng/L),medium(100 ng/L),and high(160 ng/L)concentration pure water spiked samples were-4.5%to 5.0%,-5.9%to 8.0%,and-6.3%to 8.1%,respectively,with relative standard deviations of 1.5%to 9.4%,1.7%to 13.0%,and 2.0%to 12.0%.[Conclusion]The sensitivity of this detection method meets the Standards For Drinking Water Quality(GB 5749—2022)limit requirements,offering advantages such as simple operation,high efficiency and high sensitivity,making it suitable for detecting polychlorinated biphenyls in source waterand drinking water.

关 键 词：固相萃取 气质联用 原水 饮用水 多氯联苯 

分 类 号：X703[环境科学与工程—环境工程]