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

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

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0.07～10μg/mL范围内,线性关系良好(r2=0.999 1);检出限(S/N=2.8)为0.02μg/mL;定量限(S/N=10)为0.07μg/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。

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 condi- tions of this reaction were optimized. Multiple reaction monitoring and internal standard cali- bration curve were applied to detect DHA by GC-MS/MS. The linear range for the determina- tion of DHA was 0. 07 -10μg/mL （r2 =0.999 1）. The limit of detection （S/N=2.8） was0.02μg/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 rel- ative standard deviations （RSD） were in the range of I. 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.