色谱

色谱 ›› 2011, Vol. 29 ›› Issue (02): 126-130.DOI: 10.3724/SP.J.1123.2011.00126

• 研究论文 • 上一篇    下一篇

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

郭斐斐1,2, 王雨昕2, 李敬光2*, 张加玲1, 赵云峰2, 吴永宁2   

  1. 1. 山西医科大学公共卫生学院, 山西 太原 030001; 2. 中国疾病预防控制中心化学污染与健康安全重点实验室, 营养与食品安全所, 北京 100050
  • 收稿日期:2010-11-08 修回日期:2010-12-31 出版日期:2011-02-28 发布日期:2007-03-25
  • 通讯作者: 李敬光,副研究员,主要研究方向为食品安全与环境健康.
  • 基金资助:

    国家自然科学基金项目(No.21077089, No. 20837003)、卫生行业科研专项(No. 200902009)和国家科技支撑计划项目(No. 2007BAC27B02).

Determination of Perfluorinated Compounds in human urine by Ultra High Performance Liquid Chromatography-Electrospray-Tandem Mass Spectrometry（UPLC-ESI-MS/MS）

GUO Feifei1,2, WANG Yuxin2, LI Jingguang2*, ZHANG Jialing1, ZHAO Yunfeng2, WU Yongning2   

  1. 1. School of Public Health, Shanxi Medical University, Taiyuan 030001, China; 2. Key Laboratory of Chemical Safety and Health, National Institute for Nutrition and Food Safety, Chinese Center for Disease Control and Prevention, Beijing 100050, China
  • Received:2010-11-08 Revised:2010-12-31 Online:2011-02-28 Published:2007-03-25

PDF

651

被引次数

11

摘要： 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。

关键词: 超高效液相色谱-串联质谱, 尿液, 全氟有机化合物

Abstract: 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.

Key words: perfluorinated compounds, ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), urine