【引用本文】 李忠煜, 李艳广, 黎卫亮, 等. 衍生化气相色谱-质谱法测定复垦土地样品中19种酚类污染物[J]. 岩矿测试, 2021, 40(2): 239-249. doi: 10.15898/j.cnki.11-2131/td.202007080101
LI Zhong-yu , ZHAO Jiang-hua , LI Yan-guang , et al. Determination of 19 Phenolic Pollutants in Reclaimed Land Samples by Derivation Gas Chromatography-Mass Spectrometry[J]. Rock and Mineral Analysis, 2021, 40(2): 239-249. doi: 10.15898/j.cnki.11-2131/td.202007080101

衍生化气相色谱-质谱法测定复垦土地样品中19种酚类污染物

中国地质调查局西安地质调查中心, 陕西 西安 710054

收稿日期: 2020-07-08  修回日期: 2020-10-10 

基金项目: 国家重点研发计划项目“土地生态恢复评价检验检测及质量控制标准研究”(2017YFF0206804-25)

作者简介: 李忠煜,高级工程师,主要从事地质有机分析工作。E-mail:147331515@qq.com。

通信作者:

Determination of 19 Phenolic Pollutants in Reclaimed Land Samples by Derivation Gas Chromatography-Mass Spectrometry

Xi'an Geological Survey Center, China Geological Survey, Xi'an 710054, China

Corresponding author: WANG Shuang-shuang , 主要从事地质有机分析工作。676410267@qq.com。

Received Date: 2020-07-08
Revised Date: 2020-10-10

摘要:近年来国家对自然环境的保护愈加重视,更多被破坏或污染的土地需要进行复垦整治。在评价效果时,需要检测酚类等多项污染物指标。采用气相色谱与气相色谱-质谱联用等方法对酚类化合物直接测定时,存在色谱响应值低、稳定性差、检出限高等问题。本文针对复垦土地样品基质复杂、干扰因素多、前处理困难等特点,对该类样品的提取与净化方法进行筛选优化。根据酚类污染物检测中浓度范围大、重现性差等问题,对衍生化与非衍生化效果进行对比确定了提取和净化方法,结合衍生化条件的优化、实际样品测定结果等方面的综合研究,建立了复垦土地样品19种酚类污染物的衍生化气相色谱-质谱检测方法。该方法采用加速溶剂萃取仪,以正己烷-丙酮(体积比1:1)提取样品,提取液经浓缩、净化后,由五氟苄基溴衍生化,气相色谱-质谱联用仪测定。该方法基质加标回收率为73.3%~107%,检出限为0.67~3.95μg/kg,相比非衍生化方法的检出限(10~80μg/kg)显著降低;并且衍生物的稳定性更好,色谱响应值更高,各组分表现在色谱图上的峰高(峰面积)更均衡,对于低浓度样品的测定结果更加准确。该方法能有效去除基质干扰,可为复杂基质土壤样品中的酚类污染物痕量检测提供参考。

关键词: 复垦土地, 酚类化合物, 衍生化, 气相色谱-质谱法, 加速溶剂萃取, 五氟苄基溴

Determination of 19 Phenolic Pollutants in Reclaimed Land Samples by Derivation Gas Chromatography-Mass Spectrometry

KEY WORDS: reclamation of land, phenolic compounds, derivation, gas chromatography-mass spectrometry, accelatored solvent extraction, pentafluorobenzyl bromide

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衍生化气相色谱-质谱法测定复垦土地样品中19种酚类污染物

李忠煜, 李艳广, 黎卫亮, 汪双双, 赵江华