超高效液相色谱-串联质谱法测定人尿液中全氟有机化合物

采用超高效液相色谱-串联质谱(UPLC-MS/MS)联用技术,建立了对人尿液中12种全氟有机化合物(PFCs)的分析方法。首先在尿液样品中加入相应的同位素内标,以2%(体积分数)甲酸甲醇溶液超声萃取、离心后,将提取液用弱阴离子交换固相萃取柱净化,采用UPLC-MS/MS测定,内标法定量。12种目标化合物在0.05～50 μg/L质量浓度范围内线性良好,相关系数(r)均大于0.992,检出限在0.44～3.47 ng/L之间。在20、100、500 ng/L添加水平下,平均回收率范围为80.3%～116.2%,相对标准偏差(n=6)在5.5%～13.8%之间。该方法灵敏度高、重现性好、回收率高、操作简单,适合人尿液中PFCs的测定。

Determination of perfluorinated compounds in human urine by ultra high performance liquid chromatography tandem mass spectrometry

A method for the analysis of 12 perfluorinated compounds (PFCs) in human urine by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed and validated. One mL 2% formic acid in methanol was added into the urine. After ultrasonication and centrifugation, the samples were purified by a solid phase extraction column and examined by UPLC-MS/MS. The target compounds were quantified by stable isotope dilution technique. The linear range was 0.05~50 μg/L for the 12 PFCs and the correlation coefficient ≥ 0.992. The limits of detection of 12 PFCs were in the range of 0.44~3.47 ng/L. The matrix recoveries of the method for the 12 PFCs in three spiked levels (20, 100, 500 ng/L) ranged from 80.3% to 116.2%. The relative standard deviations (RSDs, n=5) were between 5.5% and 13.8%. The sensitive and accurate method was successfully applied to the analysis of PFCs in human urine.