张权, 李磊, 林野, 周贻兵, 刘利亚, 刘文政. 正交实验优化BSTFA衍生-气相色谱法快速测定水中4种氯酚化合物[J]. 环境与职业医学, 2017, 34(9): 831-835. DOI: 10.13213/j.cnki.jeom.2017.17238
引用本文: 张权, 李磊, 林野, 周贻兵, 刘利亚, 刘文政. 正交实验优化BSTFA衍生-气相色谱法快速测定水中4种氯酚化合物[J]. 环境与职业医学, 2017, 34(9): 831-835. DOI: 10.13213/j.cnki.jeom.2017.17238
ZHANG Quan, LI Lei, LIN Ye, ZHOU Yi-bing, LIU Li-ya, LIU Wenzheng. Rapid determination of four chlorophenols in water by orthogonal experiment optimization-BSTFA derivatization-gas chromatography[J]. Journal of Environmental and Occupational Medicine, 2017, 34(9): 831-835. DOI: 10.13213/j.cnki.jeom.2017.17238
Citation: ZHANG Quan, LI Lei, LIN Ye, ZHOU Yi-bing, LIU Li-ya, LIU Wenzheng. Rapid determination of four chlorophenols in water by orthogonal experiment optimization-BSTFA derivatization-gas chromatography[J]. Journal of Environmental and Occupational Medicine, 2017, 34(9): 831-835. DOI: 10.13213/j.cnki.jeom.2017.17238

正交实验优化BSTFA衍生-气相色谱法快速测定水中4种氯酚化合物

Rapid determination of four chlorophenols in water by orthogonal experiment optimization-BSTFA derivatization-gas chromatography

  • 摘要: 目的 优化N,O-双(三甲基硅烷基)三氟乙酰胺(BSTFA)衍生-气相色谱法,快速测定水中4种氯酚类化合物。

    方法 比较不同比例的提取溶剂(环己烷:乙酸乙酯)对水中4种氯酚化合物(2-氯酚、2,4-二氯酚、2,4,6-三氯酚、五氯酚)及内标(2,4-二溴酚)的提取效果。利用正交实验确定BSTFA衍生化的最佳条件(衍生介质、衍生化试剂用量、衍生温度、衍生时间),采用气相色谱法-电子捕获检测器检测,内标法定量,快速测定水中4种氯酚类化合物,以验证方法的适用性。

    结果 以体积比为4:1的环己烷与乙酸乙酯为提取溶剂时的提取效果较好。正交实验结果显示,以体积比为4:1的环己烷与乙酸乙酯为衍生介质、BSTFA衍生化试剂用量为140μL、衍生温度为80℃、衍生时间为30 min时,4种酚类化合物衍生效果最佳;方法学验证结果显示,4种氯酚化合物在相应浓度范围内的线性关系良好(R2>0.997),检出限为0.01μg/L(2,4,6-三氯酚)~0.8μg/L(2-氯酚),定量限为0.05μg/L(2,4,6-三氯酚)~3.0μg/L(2-氯酚);不同浓度水平的加标回收率为85.2%~101.2%,相对标准偏差为0.65%~3.21%。100份生活饮用水样的检测结果显示,优化后的方法与国标检测方法的相对标准偏差为1.4%~3.7%。

    结论 该方法操作简单,定量准确,所用衍生试剂无毒,可应用于实际水样的快速检测。

     

    Abstract: Objective To optimize N, O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) derivatization-gas chromatography for rapid determination of four kinds of chlorophenols.

    Methods Mixtures of solvents (hexamethylene:ethyl acetate) at different ratios were compared for the extraction effects of four chlorophenols (2-chlorophenol, 2, 4-dichlorophenol, 2, 4, 6-trichlorophenol, and pentachlorophenol) and one internal standard (2, 4-dibromophenol). The best conditions of BSTFA derivatization were confirmed by orthogonal experiment, including derivation medium, derivatization reagent dosage, derivative temperature, and derivative time. Then gas chromatography with electron capture detector and internal standard was applied to rapidly determine four kinds of chlorophenols in water to verify the applicability of the established method.

    Results Using hexamethylene:ethyl acetate (v/v, 4:1) as extraction solvent showed the best extraction effect. According to the results of orthogonal experiment, the best derivative conditions for the selected four chlorophenols included using cyclohexane:acetic ether (4:1) as derivation medium, BSTFA derivatization reagent volume at 140 μL, derivative temperature at 80℃, and derivative time for 30 min. The methodology validation results showed that the linear relationships of the four chlorophenols were good with R2> 0.997 in corresponding concentration ranges, the detection limits were from 0.01 μg/L (2, 4, 6-trichlorophenol) to 0.8 μg/L (2-chlorophenol), and the quantitative limits were from 0.05 μg/L (2, 4, 6-trichlorophenol) to 3.0 μg/L (2-chlorophenol). The addition standard recoveries were in the range of 85.2%-101.2%, and the relative standard deviations were between 0.65% and 3.21% (n=5). After applying to 100 drinking water samples, the relative standard deviations for the optimized method versus national standard testing method were 1.4%-3.7%.

    Conclusion The optimized method is advantaged in simple operation, accurate quantification, and nontoxic derivatization reagent; therefore, it is suitable for rapid detection for water samples.

     

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