色谱

色谱 ›› 2013, Vol. 31 ›› Issue (8): 734-738.DOI: 10.3724/SP.J.1123.2013.01050

• 研究论文 • 上一篇    下一篇

杂环衍生化-气相色谱-三重四极杆质谱法检测人血液中的二十二碳六烯酸

王静1, 王丹2, 张华1, 彭孝军1, 董珺璞2   

  1. 1. 精细化工国家重点实验室, 大连理工大学, 辽宁 大连 116024;
    2. 大连理工大学化工学院, 辽宁 大连 116024
  • 收稿日期:2013-01-30 修回日期:2013-03-17 出版日期:2013-08-28 发布日期:2013-09-29
  • 通讯作者: 张华

Analysis of docosahexenoic acid in human blood using heterocyclic derivatization-gas chromatography-triple quadrupole mass spectrometry

WANG Jing1, WANG Dan2, ZHANG Hua1, PENG Xiaojun1, DONG Junpu2   

  1. 1. State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116024, China;
    2. School of Chemical Engineering, Dalian University of Technology, Dalian 116024, China
  • Received:2013-01-30 Revised:2013-03-17 Online:2013-08-28 Published:2013-09-29
  • Contact: O658

PDF

289

被引次数

5

摘要：

建立了人血液中二十二碳六烯酸(DHA)的杂环衍生化-气相色谱-三重四极杆质谱(GC-MS/MS)检测方法。以2-氨基-2-甲基-1-丙醇(AMP)作为DHA的杂环衍生化试剂,优化了杂化反应的最佳反应条件,并使用GC-MS/MS在多反应监测模式下,以内标法对DHA进行定量检测。在0.07~10 μg/mL范围内,线性关系良好(r2=0.9991);检出限(S/N=2.8)为0.02 μg/mL;定量限(S/N=10)为0.07 μg/mL。在高、中、低3个不同添加水平下,其平均回收率在94.40%~103.13%之间,相对标准偏差(RSD)在1.51%~3.16%之间。该方法操作简便,所需样品量少,结果准确可靠,适用于人血液中DHA的分析检测。

关键词: 多反应监测, 二十二碳六烯酸, 气相色谱-三重四极杆质谱, 人血液, 杂环衍生化

Abstract:

A method was developed and validated for the analysis of docosahexenoic acid (DHA) in human blood by heterocyclic derivatization-gas chromatography coupled with triple quadrupole mass spectrometry (GC-MS/MS). 2-Amino-2-methyl-1-propanol (AMP) was used as the reaction reagent of DHA heterocyclic derivatization and the most optimal reaction conditions of this reaction were optimized. Multiple reaction monitoring and internal standard calibration curve were applied to detect DHA by GC-MS/MS. The linear range for the determination of DHA was 0.07-10 μg/mL (r2=0.9991). The limit of detection (S/N=2.8) was 0.02 μg/mL and the limit of quantification (S/N=10) was 0.07 μg/mL. The average recoveries of DHA at three spiked levels of 0.5, 1.5 and 2.5 μg ranged from 94.40% to 103.13% and the relative standard deviations (RSD) were in the range of 1.51%-3.16%. The method was simple, accurate, reliable and small amount of sample was required. It was suitable for detecting the contents of DHA in human blood.

Key words: docosahexenoic acid, gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS), heterocyclic derivatization, human blood, multiple reaction monitoring

中图分类号: