Salm Paul, Taylor Paul J, Kostner Karam
Australian Bioanalytical Services Pty Ltd, Princess Alexandra Hospital, Woolloongabba, Queensland, Australia.
Biomed Chromatogr. 2011 Jun;25(6):652-9. doi: 10.1002/bmc.1496. Epub 2010 Aug 25.
A method for the simultaneous quantification of eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA) and arachidonic acid (AA) in human plasma by HPLC-tandem mass spectrometry (HPLC-MS/MS) was developed and validated. Free and esterified forms of fatty acids were hydrolysed from plasma samples in the presence of an internal standard and subjected to liquid-liquid extraction. The chromatographic run time was 3.5 min per sample. The assay was linear from 0.5 to 300 mg/L (r(2) > 0.997, n = 18). Based on matrix addition, accuracy deviation was <15%, except for AA at 10 mg/L (30-90%), whereas precision was <8% for all fatty acids studied. The method was applied to the measurement of these omega-3 fatty acids in a fish oil supplement study with healthy volunteers. Healthy males (n = 4) were administered a supplement containing 465 mg EPA and 375 mg DHA per capsule (Omacor®). A dose of two capsules was given daily over a 4 week period. Pre-treatment concentrations varied between subjects for EPA (17-68 mg/L), DHA (36-63 mg/L) and AA (121-248 mg/L). During the dosing period EPA increased 460-480% from the baseline concentration, while DHA increased 150-160%. The EPA-AA ratio increased from 0.07-0.56 to 0.3-3.1 after 4 weeks of dosing. In conclusion, the method described could be suitable for monitoring EPA, DHA and AA in clinical studies that may aid in achieving optimal concentrations of these fatty acids in patients who could be at risk of sudden cardiac death.
建立并验证了一种通过高效液相色谱-串联质谱法(HPLC-MS/MS)同时定量人血浆中二十碳五烯酸(EPA)、二十二碳六烯酸(DHA)和花生四烯酸(AA)的方法。在存在内标的情况下,从血浆样品中水解游离和酯化形式的脂肪酸,并进行液-液萃取。每个样品的色谱运行时间为3.5分钟。该测定在0.5至300 mg/L范围内呈线性(r(2)>0.997,n = 18)。基于基质加标,除了10 mg/L的AA(偏差为30 - 90%)外,准确度偏差<15%,而所有研究的脂肪酸的精密度<8%。该方法应用于一项针对健康志愿者的鱼油补充剂研究中这些ω-3脂肪酸的测量。健康男性(n = 4)服用一种每粒胶囊含465 mg EPA和375 mg DHA的补充剂(Omacor®)。在4周的时间内每天服用两粒胶囊。治疗前,受试者的EPA浓度在17 - 68 mg/L之间,DHA浓度在36 - 63 mg/L之间,AA浓度在121 - 248 mg/L之间。在给药期间,EPA从基线浓度增加了460 - 480%,而DHA增加了150 - 160%。给药4周后,EPA与AA的比值从0.07 - 0.56增加到0.3 - 3.1。总之,所描述的方法可能适用于临床研究中监测EPA、DHA和AA,这可能有助于在可能有心脏性猝死风险的患者中实现这些脂肪酸的最佳浓度。