崔世勇, 樊珠凤, 姜丽华. 饮用水中4种氯酚的单液滴微萃取气相色谱-质谱测定方法研究[J]. 环境与职业医学, 2014, 31(9): 715-719. DOI: 10.13213/j.cnki.jeom.2014.0175
引用本文: 崔世勇, 樊珠凤, 姜丽华. 饮用水中4种氯酚的单液滴微萃取气相色谱-质谱测定方法研究[J]. 环境与职业医学, 2014, 31(9): 715-719. DOI: 10.13213/j.cnki.jeom.2014.0175
CUI Shi-yong , FAN Zhu-feng , JIANG Li-hua . Determination of Four Chlorophenols in Drinking Water by Single-Drop Microextraction and Gas Chromatography-Mass Spectrometry[J]. Journal of Environmental and Occupational Medicine, 2014, 31(9): 715-719. DOI: 10.13213/j.cnki.jeom.2014.0175
Citation: CUI Shi-yong , FAN Zhu-feng , JIANG Li-hua . Determination of Four Chlorophenols in Drinking Water by Single-Drop Microextraction and Gas Chromatography-Mass Spectrometry[J]. Journal of Environmental and Occupational Medicine, 2014, 31(9): 715-719. DOI: 10.13213/j.cnki.jeom.2014.0175

饮用水中4种氯酚的单液滴微萃取气相色谱-质谱测定方法研究

Determination of Four Chlorophenols in Drinking Water by Single-Drop Microextraction and Gas Chromatography-Mass Spectrometry

  • 摘要: 目的 研究单液滴微萃取气相色谱-质谱法快速测定饮用水中4 种氯酚的最优实验条件。

    方法 取50 mL 水样,加入内标2,4-二溴酚,经不同条件萃取和衍生后,采用气相色谱-质谱法检测定量。选择单液滴微萃取最佳实验条件,并应用于样本中4 种氯酚的测定,再将测定结果与标准方法进行比较。

    结果 实验显示最优条件分别为:萃取剂为正己烷-甲苯(1:1),衍生剂为N-叔丁基二甲基甲硅烷基-N-甲基三氟乙酰胺(MTBSTFA),衍生剂比例为20%,搅拌速度为200 r/min,萃取时间为30 min,溶液离子强度为200 g/L 的氯化钠溶液。在上述优化的实验条件下,2-氯酚、2,4-二氯酚、2,4,6-三氯酚、五氯酚在0.2~100.0 μg/L 质量分数范围内,其相关系数分别为0.999 3,0.999 3,0.998 7,0.999 9,检出限分别为0.021、0.018、0.026、0.035 μg/L。在1、10、80 μg/L 三个氯酚水平的平均回收率在85.6%~104.0%,相对标准偏差为2.5%~9.4%。本法测定结果与标准方法比较,无统计学差异。

    结论 本研究的优化实验条件下采用单液滴微萃取气相色谱-质谱法步骤简单,快速,与标准方法测定结果一致性高,适用于饮用水中氯酚的快速检测。

     

    Abstract: Objective To identify the best experimental condition for simultaneous determination of four chlorophenols in drinking water by single-drop microextraction (SDME) and gas chromatography-mass spectrometry (GC-MS).

    Methods The method involved addition of 2, 4-dibromophenol as internal standard into 50 mL water samples, followed by extraction and derivatization at different conditions, and quantification using GC-MS detection. The best conditions for SDME efficiency was applied to analyze four chlorophenols in drinking water. The results determined by this method were compared with those by the national standard method.

    Results The optimized conditions for SDME were summarized as follows: hexane-toluene (1:1) as solvent; N-methyl-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTF) as derivatization reagent; 20% MTBSTFA; microextraction was performed in a medium of 200 g/L NaCl, with a stirring rate of 200 r/min for 30 min. Calibration curves for the four chlorophenols (2-chlorophenols, 2, 4-dichlorophenols, 2, 4, 6-trichlorophenols, and pentachlorophenols) were linear within the range of 0.2-100.0 μg/L. The correlation coefficients were 0.999 3, 0.999 3, 0.998 7, and 0.999 9, respectively. The limits of detection were 0.021, 0.018, 0.026, and 0.035 μg/L, respectively. The average recoveries ranged from 85.6% to 104.0% at three spiked levels of 1, 10, and 80 μg/L for each chlorophenol, and the relative standard deviations ranged from 2.5% to 9.4%. No significant difference was found in the results between the proposed method and the national standard method.

    Conclusion The proposed method is simple, rapid, highly consistent with the standard method, and thus suitable for the determination of chlorophenols in drinking water.

     

/

返回文章
返回