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

发布时间：2018-08-09 08:51

【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(R~20.997),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- double (three methyl silicon alkyl) three fluoroacetamide (BSTFA) derivative gas chromatography for the rapid determination of 4 kinds of chlorophenols in water. [Methods] to compare 4 chlorophenols (2- chlorophenol, 2,4- two chlorophenol, 2,4,6- three chlorophenol, pentachlorophenol) and internal standard (2,4- dibromo phenol) in different proportion of extraction solvent (cyclohexane: ethyl acetate) Extraction effect. The optimum conditions of BSTFA derivatization were determined by orthogonal experiment (derivative medium, amount of derivatization reagents, derivatization temperature, derivatization time), gas chromatography electron capture detector detection, quantitative determination of 4 chlorophenols in water by internal standard method, in order to verify the applicability of the method. [results] with a ring of volume ratio of 4: 1 The extraction effect of hexane and ethyl acetate as extraction solvents is better. Orthogonal experimental results show that 4 kinds of phenolic compounds have the best derivative effect when the dosage of cyclohexane and ethyl acetate are derived medium with volume ratio of 4 to 1, the dosage of BSTFA derivatization reagent is 140 mu L, derivatization temperature is 80, and the derivative time is 30 min. The results of methodological verification show 4 The linear relationship of chlorophenol compounds in the corresponding concentration range is good (R~20.997), the detection limit is 0.01 mu g/L (2,4,6- three chlorophenol) ~0.8 mu g/L (2- chlorophenol), and the quantitative limit is 0.05 mu g/L (2,4,6- three chlorophenol) ~3.0 micron g/L (2- chlorophenol); the recovery rate of the different concentration levels is 85.2%~101.2%, the relative standard deviation is the drinking water sample The test results show that the relative standard deviation between the optimized method and the national standard detection method is 1.4%~3.7%.[Conclusion] the method is simple, accurate, and the derived reagent is nontoxic and can be applied to the rapid detection of actual water samples.
【作者单位】：贵州省疾病预防控制中心卫生监测检验所理化科;
【基金】：贵州省疾病预防控制中心青年项目(编号:2015-E2-2青)
【分类号】：O657.71;R123.1

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