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[目的]建立同时测定尿液中2-氯酚、2,4-二氯酚、2,4,6-三氯酚及五氯酚4种氯酚的气相色谱串联质谱(GC-MS/MS)方法。[方法]尿样经盐酸水解结合型氯酚,液液萃取法(LLE)提取,乙酸酐衍生化,采用GC-MS/MS检测,内标法定量。[结果]采用人工模拟尿样作为空白,基质匹配标准条件下,2-氯酚、2,4-二氯酚、2,4,6-三氯酚及五氯酚分别在0.50~100.0、0.50~100.0、0.50~100.0μg/L和1.0~100.0μg/L的范围内均具有良好的线性关系,相关系数均大于0.999。方法的检出限为0.1~0.3μg/L,回收率为88.8%~118.2%,相对标准偏差(RSD)为1.3%~5.5%。[结论]本方法操作简便、准确度高、重现性好,适用于尿样中多种氯酚含量的检测。
[Objective] To establish a gas chromatography-tandem mass spectrometry (GC-MS / MS) method for the simultaneous determination of 2 chlorophenols, 2,4-dichlorophenols, 2,4,6-trichlorophenol and pentachlorophenol in urine )method. [Methods] Urine samples were extracted by hydrochloric acid hydrolysis combined with chlorophenol, liquid-liquid extraction (LLE) and derivatized with acetic anhydride. The urine samples were determined by GC-MS / MS and internal standard method. [Results] The simulated urine samples were used as blank, and under the standard conditions of matrix matching, 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol were 0.50 ~ 100.0,0.50 ~ 100.0,0.50 ~ 100.0μg / L and 1.0 ~ 100.0μg / L in the range of all have a good linear relationship, the correlation coefficient is greater than 0.999. The detection limits were 0.1-0.3 μg / L, the recoveries were 88.8% -118.2%, and the relative standard deviations (RSDs) were 1.3% -5.5%. [Conclusion] The method is simple, accurate and reproducible. It is suitable for the determination of chlorophenols in urine samples.