环境水体中9种内分泌干扰物的同时高效富集方法
Simultaneous and efficient extraction of nine endocrine disrupting chemicals in aqueous matrices
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摘要: 本文以双酚A、雌酮、17β-雌二醇、雌三醇、炔雌醇、辛基酚、壬基酚、邻苯二甲酸二丁酯、邻苯二甲酸二(2-乙基己基)酯等环境水体中检出频率高的9种内分泌干扰物为研究对象,从目标污染物的结构特征出发,考察了不同萃取剂对目标污染物的吸附特征,筛选出性能互补的两种萃取剂C18和NAX进行组合,实现了对目标污染物的高效富集.同时,通过比较多种洗脱剂对目标污染物的洗脱效率,确定乙腈为洗脱剂.在此基础上,为评价本方法对目标污染物的浓缩富集效果,建立了9种污染物的液相色谱-质谱检测方法,标准曲线线性关系良好,线性决定系数大于0.9983,线性范围为0.01—8 mg·L-1.9种目标物在不同水体的加标回收率范围为71.6%—108.5%,相对偏差为1.2%—6.3%.本文所建立的浓缩富集方法操作简单,成本低,回收率高,适合于不同水体基质中9种内分泌干扰物的定性及定量分析.Abstract: Nine endocrine disrupting chemicals, including bisphenol A, estrone, 17β-estradiol, estriol, ethinylestradiol, 4-octylphenol, nonylphenol, dibutyl phthalate, di-(ethylhexyl) phthalate were selected as the compounds target. The adsorption capability of several adsorbents and elution efficiency of eluents were investigated. Two adsorbents C18 and NAX with complementary high concentration efficiency for nine targets were selected, and acetonitrile was chosen as eluent for nine targets as well. To evaluate the extraction efficiency of nine targets, a detection method based on ultra-performance liquid phase chromatography in tandom with mass spectrometry (UPLC-MS) was established. The composition of mobile phase, gradient elution conditions, and operating parameters for detection method was optimized. All the nine EDCs had good linearity (r> 0.9983) within the range of 0.01—8 mg·L-1. The average recovery of spiked water sample ranged from 71.6%—108.5% and their relative standard deviation varied between 1.2%—6.3%. The established method in this study is low cost, simple, has high recovery rate, and is therefore suitable for the qualitutive and quantitative analysis of the 9 EDCs in different aqueous matrices.
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Key words:
- endocrine disrupting chemicals /
- aquatic environment /
- solid-phase extraction /
- UPLC-MS
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