气相色谱串联质谱法测定尿中四种氯酚含量
Determination of Four Chlorophenols in Human Urine by Gas Chromatography Coupled with Tandem Mass Spectrometry
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摘要:
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、0.50~100.0 μg/L 和1.0~100.0 μg/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0.1~0.3 μg/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。 Abstract:Objective To establish a method for simultaneous determination of four chlorophenols including 2-chlorophenol (2-CP), 2, 4-dichlorophenol (2, 4-DCP), 2, 4, 6-trichlorophenol (2, 4, 6-TCP), and pentachlorophenol (PCP) in human urine by gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). Methods Urine samples were hydrolyzed with hydrochloric acid, extracted by liquid-liquid extraction (LLE) method, and then derivatized using acetic anhydride. The products were detected by GC-MS/MS and quantified by internal standard method. Results Using artificial urine as urine blank and matrix for matched calibration, good linear relationships were obtained in the range of 0.50-100.0, 0.50-100.0, 0.50-100.0 μg/L, and 1.0-100.0 μg/L for 2-CP, 2, 4-DCP, 2, 4, 6-TCP, and PCP, respectively. Correlation coefficients were all greater than 0.999. Limits of detection ranged from 0.1 μg/L to 0.3 μg/L. Recoveries were between 88.8% and 118.2% with relative standard deviations in the range of 1.3% to 5.5%. Conclusion The method is featured by simple operation, high accuracy, and good repeatability to detect multiple chlorophenols in human urine samples.