论文部分内容阅读
建立了分析兔血浆中游离脂肪酸(Free fatty acid, FFA)的三甲基硅烷衍生化GC-MS方法.兔血浆样品经N,O-双(三甲基甲硅烷基)三氟乙酰胺(BSTFA)-三甲基氯硅烷(TMCS)衍生化后,用GC-MS测定了兔血浆中的游离脂肪酸(棕榈酸,硬脂酸,油酸,亚油酸和花生四烯酸).考察了从脂质萃取到三甲基硅烷化反应在内各项实验条件的影响,并选定实验条件.经方法学验证,FFA峰面积及其浓度之间的线性相关系数(r2)均大于0.999,回收率在82％-111％之间.不同浓度血浆样品中的FFA日内变化RSD均小于6％.16种兔血浆样品的FFA分析结果表明,该方法可以较好用于体内血浆样品的测定,与传统的FFA衍生化方法相比,所建立的三甲基硅烷衍生化方法简单、特异性好,且完全不受已酯化脂肪酸(例如甘油三酯)的干扰,可用于临床实验室或药理研究中的FFA谱分析.“,”In the present study,free fatty acids (FFAs,including palmitic acid,stearic acid,oleic acid,linoleic acid and arachidonic acid) in rabbit plasma were determined by gas chromatography-mass spectrometry (GC-MS) after trimethylsilylation derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA)-trimethylchlorosilane (TMCS) as derivatization reagent.The experimental conditions,including extraction and silylation reaction,were investigated.The method was experimentally validated.The linearity between fatty acids' peak areas and their concentrations was obtained with the corelative coefficient (r2) all more than 0.999,and the recoveries were between 82％ and 111％.The intra-day variations of FFAs' in plasma samples at different concentrations were all less than 6％.FFA analysis results of 16 rabbit plasma samples showed that the method could be well applied in the determination of plasma samples in vivo.In contrast to the traditional method of FFA derivatization,the established trimethylsilylation method presented simplicity,high specificity,and completely free from the interference of the esterified fatty acid,such as triacylglyceride.The method could be applied for analyzing FFA profiles in the clinical laboratory or pharmacological research.