Sánchez-Avila N, Mata-Granados J M, Ruiz-Jiménez J, Luque de Castro M D
Department of Analytical Chemistry, University of Córdoba, Spain.
J Chromatogr A. 2009 Oct 2;1216(40):6864-72. doi: 10.1016/j.chroma.2009.08.045. Epub 2009 Aug 21.
A method for the determination of fatty acids in serum based on GC-MS (micro-SIS detection mode) has been developed and the separation and cis/trans isomers have been identified. A prior two-step extraction/derivatization procedure accelerated by ultrasound allows individual determination of esterified (EFAs) and non-esterified fatty acids (NEFAs), and shortening of the derivatization steps to 5 min for EFAs and 15 min for NEFAs. The total analysis time for 39 fatty acids was 61 min. The minimum LOD and LOQ values were 0.002 and 0.006 microg/ml, respectively. The proposed method was validated for EFAs and NEFAs using two different methods and the results show no statistical differences between the proposed method and those used as reference. The proposed derivatization-extraction methodology is suitable for fatty-acid analysis of human serum, and can be applied to nutritional and epidemiological studies.
已开发出一种基于气相色谱 - 质谱联用(微单离子监测检测模式)测定血清中脂肪酸的方法,并对其分离及顺式/反式异构体进行了鉴定。通过超声加速的两步萃取/衍生化预处理程序能够分别测定酯化脂肪酸(EFA)和非酯化脂肪酸(NEFA),同时将EFA的衍生化步骤缩短至5分钟,NEFA的衍生化步骤缩短至15分钟。39种脂肪酸的总分析时间为61分钟。最低检测限(LOD)和最低定量限(LOQ)分别为0.002和0.006微克/毫升。使用两种不同方法对EFA和NEFA验证了所提出的方法,结果表明所提出的方法与用作参考的方法之间无统计学差异。所提出的衍生化 - 萃取方法适用于人血清脂肪酸分析,可应用于营养和流行病学研究。