职业与健康 ›› 2026, Vol. 42 ›› Issue (12): 1607-1621.

• 论著—实验·监测与检验 • 上一篇    下一篇

盘膜固相萃取-气相色谱串联质谱法同时测定水中208种半挥发性有机物

李琰, 董洁, 金王健, 杨亦骋, 张雄伟, 郝春慧()   

  1. 上海市闵行区疾病预防控制中心(上海市闵行区卫生健康监督所)上海 201101
  • 收稿日期:2026-02-03 修回日期:2026-02-25 出版日期:2026-06-15 发布日期:2026-06-18
  • 通信作者: 郝春慧,E-mail:haohao.hch@163.com
  • 作者简介:李琰,女,副主任技师,主要从事环境和食品污染物检测工作。
  • 基金资助:
    上海市闵行区自然科学研究课题专项资金(2022MHZ071)

Simultaneous determination of 208 semi-volatile organic compounds in water by disk membrane solid-phase extraction-gas chromatography-tandem mass spectrometry

LI Yan, DONG Jie, JIN Wangjian, YANG Yicheng, ZHANG Xiongwei, HAO Chunhui()   

  1. Shanghai Minhang District Center for Disease Control and Prevention(Shanghai Minhang District Health Supervision Institute)Shanghai 201101, China
  • Received:2026-02-03 Revised:2026-02-25 Online:2026-06-15 Published:2026-06-18
  • Contact: HAO Chunhui,E-mail:haohao.hch@163.com

摘要:

目的 建立1种基于盘膜固相萃取(disk membrane solid-phase extraction,DMSPE)-气相色谱串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)技术,同时测定生活饮用水和水源水中208种半挥发性有机物(semi-volatile organic compounds,SVOCs)的分析方法。方法 取1 000 mL水样,经除氯处理后加入5 mL甲醇,采用DMSPE进行富集与净化,依次采用3 mL乙酸乙酯和3 mL二氯甲烷洗脱,40 ℃下氮吹浓缩至近干,用1 mL乙酸乙酯-二氯甲烷(8∶2,V/V)复溶后,经HP-5MS Ultra Inert色谱柱(30 m×250 μm×0.25 μm)分离,在电子轰击离子源(electron ionization,EI)下电离,采用动态多反应监测(dynamic multiple reaction monitoring,dMRM)模式进行质谱检测,工作曲线法定量。结果 208种目标化合物分离良好,在各自线性范围内线性关系良好(r>0.995)。方法检出限为0.012~2.200 ng/L,定量限为0.047~7.400 ng/L。在水样加标回收实验中,目标物的平均回收率为70.0%~130.0%,相对标准偏差(relative standard deviation,RSD)为0.45%~18.30%。结论 所建立的方法操作便捷、分析周期短,具有高通量、高灵敏度、良好的精密度与准确度,适用于生活饮用水及水源水中多种SVOCs的日常监测和应急检测。

关键词: 盘膜固相萃取, 气相色谱串联质谱法, 半挥发性有机物, 生活饮用水, 水源水

Abstract:

Objective To establish an analytical method based on disk membrane solid-phase extraction(DMSPE) and gas chromatography-tandem mass spectrometry(GC-MS/MS) for the simultaneous determination of 208 semi-volatile organic compounds(SVOCs) in drinking water and source water. Methods A 1 000 mL water sample was dechlorinated,mixed with 5 mL methanol,and subjected to enrichment and clean-up using DMSPE. The analytes were eluted sequentially with 3 mL of ethyl acetate and 3 mL of dichloromethane,concentrated to near dryness under a nitrogen stream at 40 ℃,and reconstituted in 1 mL of ethyl acetate-dichloromethane(8∶2,V/V). Separation was performed on an HP-5MS Ultra Inert column(30 m×250 μm×0.25 μm) with electron ionization(EI). Detection was carried out in dynamic multiple reaction monitoring(dMRM) mode,and quantification was achieved using a working curve method. Results All 208 target compounds were well separated,showing good linearity(r>0.995) within their respective concentration ranges. The method detection limits ranged from 0.012 to 2.200 ng/L,and the quantification limits ranged from 0.047 to 7.400 ng/L. In spiked water samples,the average recoveries of the target compounds were 70.0%-130.0%,with relative standard deviations(RSD) of 0.45%-18.30%. Conclusion The developed method is simple,rapid,and demonstrates high throughput,high sensitivity,good precision,and accuracy. It is suitable for routine monitoring and emergency detection of multiple SVOCs in drinking water and source water.

Key words: Disk membrane solid-phase extraction, Gas chromatography-tandem mass spectrometry, Semi-volatile organic compounds, Drinking water, Source water

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