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

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。

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

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.