超高效液相色谱-串联质谱法测定人尿中全氟化合物
[Determination of perfluorinated compounds in human urine by ultra high performance liquid chromatography-tandem mass spectrometry].
作者信息
Guo Feifei, Wang Yuxin, Li Jingguang, Zhang Jialing, Zhao Yunfeng, Wu Yongning
机构信息
School of Public Health, Shanxi Medical University, Taiyuan 030001, China.
出版信息
Se Pu. 2011 Feb;29(2):126-30. doi: 10.3724/sp.j.1123.2011.00126.
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 microg/L for the 12 PFCs and the correlation coefficient > or = 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.
建立并验证了一种采用超高效液相色谱-串联质谱法（UPLC-MS/MS）分析人尿中12种全氟化合物（PFCs）的方法。向尿液中加入1 mL含2%甲酸的甲醇。超声处理和离心后，样品通过固相萃取柱进行净化，然后用UPLC-MS/MS进行检测。目标化合物采用稳定同位素稀释技术进行定量。12种PFCs的线性范围为0.05 - 50 μg/L，相关系数≥0.992。12种PFCs的检测限在0.44 - 3.47 ng/L范围内。该方法对12种PFCs在三个加标水平（20、100、500 ng/L）下的基质回收率在80.3%至116.2%之间。相对标准偏差（RSDs，n = 5）在5.5%至13.8%之间。该灵敏且准确的方法成功应用于人尿中PFCs的分析。
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