大体积全自动固相萃取-气相色谱-质谱法同时测定饮用水中43种半挥发性有机物
作者:
作者单位:

(珠海市疾病预防控制中心,广东 珠海 519000)

作者简介:

梁素丹 女 副主任技师 研究方向为水质和食品及工作场所等毒物分析 E-mail:┣┣超链接:MAILTO:LSUDAN@126.COM┫┫lsudan@126.com┣┣超链接结束┫┫通信作者:┣┣(中)通信作者┫┫陈剑刚 男 主任技师 研究方向为水质和食品及工作场所等毒物分析 E-mail:davidchenjg@sina.com

通讯作者:

中图分类号:

基金项目:

珠海市科技计划项目(20171009E030065)


Simultaneous determination of 43 compounds of semi-volatile organic compounds in drinking water by gas chromatography-mass spectrometry with automatic bulk solid phase extraction
Author:
Affiliation:

(Zhuhai Center for Disease Control and Prevention,Guangdong Zhuhai 519000,China)

Fund Project:

  • 摘要
  • |
  • 图/表
  • |
  • 访问统计
  • |
  • 参考文献
  • |
  • 相似文献
  • |
  • 引证文献
  • |
  • 资源附件
  • |
  • 文章评论
    摘要:

    目的 建立大体积全自动固相萃取-气相色谱-质谱(SPE-GC-MS)法同时测定饮用水中43种半挥发性有机物(SVOCs)。方法 1.0 L饮用水样品经HLB固相萃取柱富集、净化后,分别以2 ml乙酸乙酯、4 ml二氯甲烷洗脱,洗脱液氮吹浓缩至0.5 ml,用乙酸乙酯定容至1.0 ml,经HP-5 ms UI超高惰性毛细管柱(30 m×250 μm, 0.25 μm)分离,采用GC-MS的选择离子扫描模式(SIM)分析,以保留时间和特征离子定性,内标法定量。结果43种SVOCs均得到有效分离,方法的线性关系良好,相关系数r2≥0.995,方法检出限为0.000 13~0.008 2 μg/L,定量限为0.000 42~0.027 μg/L,平均回收率为70.0%~138%,精密度为0.3%~12.1%。应用该方法测定16份不同水质样品,结果共检出六氯苯、五氯硝基苯和萘等10种SVOCs。结论 本方法灵敏、高效,适用于饮用水中多种SVOCs的同时检测,可为突发公共卫生事件提供依据。

    Abstract:

    Objective To establish a method for the simultaneous determination of 43 compounds of semi-volatile organic compounds (SVOCs) in drinking water by gas chromatography-mass spectrometry with automatic bulk solid phase extraction(SPE-GC-MS). Methods SVOCs in 1.0 L drinking water sample were enriched and purified by HLB solid phase extraction column, eluted by 2 ml ethyl acetate and 4 ml dichloromethane, purged and concentrated to 0.5 ml and volumed to 1.0 ml by ethyl acetate, separated by HP-5 ms ultra-inert capillary column(30 m×250 μm,0.25 μm), and then analyzed by selective ion scanning mode (SIM) coupled with GC-MS. Qualitative analysis was performed by retention time and characteristic ions, and quantitative analysis was performed by the internal standard method. Results Forty-three compounds of SVOCs were effectively separated and showed good linear relationship (r2≥0.995). The detection limits and quantitative limits of the method were 0.000 13-0.008 2 μg/L and 0.000 42-0.027 μg/L. The recoveries and precisions were 70.0%-138% and 0.3%-12.1%. Sixteen samples of different water were determined by the method, and ten compounds of SVOCs such as hexachlorobenzene, pentachloronitrobenzene and naphthalene were detected. Conclusion The method was sensitive and efficient, it was suitable for simultaneous detection of SVOCs in drinking water and provide a basis for public health emergencies.

    参考文献
    相似文献
    引证文献
引用本文

梁素丹,陈剑刚,林丽玲,张艳,冯翠霞.大体积全自动固相萃取-气相色谱-质谱法同时测定饮用水中43种半挥发性有机物[J].中国食品卫生杂志,2019,31(6):533-539.

复制
分享
文章指标
  • 点击次数:
  • 下载次数:
  • HTML阅读次数:
  • 引用次数:
历史
  • 收稿日期:2019-10-28
  • 最后修改日期:
  • 录用日期:
  • 在线发布日期: 2020-01-14
  • 出版日期:
文章二维码
《中国食品卫生杂志》邮寄地址与联系方式变更通知
关闭