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高效液相色谱-串联质谱法测定润滑剂中的全氟有机化合物

张代辉1,2*,卢利军1,张勋1,牟峻1,周晓1,胡婷婷1,韩大川1   

  1. (1.吉林出入境检验检疫局 长春 130062;2.吉林大学生命科学学院 长春 130023)
  • 收稿日期:2011-09-08 修回日期:2012-03-07 出版日期:2012-10-10 发布日期:2012-10-10
  • 通讯作者: 张代辉，高级工程师; Tel:0431-87607202; Fax:0431-87607733; E-mail:zdh30924@yahoo.com.cn; 研究方向：工业品中有毒有害物质分析
  • 基金资助:
    国家质检总局课题（2007IK142）和吉林检验检疫局科技课题（2009JK51）资助

Simultaneous Determination of Ten Kinds of Perfluorinated Compounds in Lubricant Samples by High-performance Liquid Chromatography-Tandem Mass Spectrometry

ZHANG Daihui1,2*, LU Lijun1, ZHANG Xun1, MU Jun1, ZHOU Xiao1, HU Tingting1, HAN Dachuan1   

  1. (1.Jilin EntryExit Inspection and Quarantine Bureau,Changchun 130062,China;
    2.College of Life Sciences,Jilin University,Changchun 130023,China)
  • Received:2011-09-08 Revised:2012-03-07 Published:2012-10-10 Online:2012-10-10

PDF

956

被引次数

6 | 1

摘要： 建立了测定润滑剂中10种全氟有机化合物的高效液相色谱-串联质谱（HPLC-MS/MS）分析方法。 不同类型的润滑剂样品经溶剂提取后，采用弱阴离子交换柱和石墨化碳柱净化，经C18色谱柱分离后进行HPLC-MS/MS多反应监测模式下的定性及定量分析。 10种全氟有机化合物的方法检出限为0.001~0.005 mg/kg；在低、中、高的3个添加水平范围内的平均回收率在79.05％~106.26％；日内精密度均小于10%，日间精密度均小于20%。

关键词: 高效液相色谱-串联质谱, 润滑剂, 全氟有机化合物, 检测

Abstract: An analytical method based on high-performance liquid chromatography tandem mass spectrometry has been developed for the determination of 10 perfluorinated compounds. Various lubricant samples were extracted with the solvent. Then the extract was cleaned up by Oasis WAX and Envi-carb solid phase cartridge. Qualitative and quantitative analyses were carried out for the analyte under the multiple reaction monitoring(MRM) mode after the chromatographic separation over Waters Xbridge C18(150 mm×2.1 mm, 3.5 μm）column. The limits of detection for 10 perfluorinated compounds were 0.001~0.005 mg/kg. The mean recoveries at the three spiked levels were 79.05％~106.26％, with the intra-day precision less than 10% and the inter-day precision less than 20%.

Key words: High performance liquid chromatography tandem mass spectrometry, lubricants, perfluorinated compounds, detection

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