Poster Presentations
Day 3, June 12（Fri.） Room P (5F 501+502)
- 3P-28
Development of a Free Fatty Acid Analysis Method in Biological Samples Using Online Solid-Phase Dehydration Derivatization-GC/MS
(AiSTI SCIENCE)
oRyoichi Sasano, Chiaki Maruyama, Shoya Arakawa
GC/MS analysis of Free fatty acids (FFAs) is commonly performed after methyl ester derivatization; however, methyl esters of unsaturated fatty acids such as EPA and DHA produce weak fragment ions in the high-mass region. Consequently, quantification often relies on mid-mass fragments that are susceptible to interference from matrix components. In addition, the conventional methylation method requires heating with HCl–MeOH at 60 °C for approximately 30 min, resulting in complicated sample preparation. In this study, a rapid and reliable analytical method for FFAs in biological samples was developed using tert-butyldimethylsilyl (TBDMS) derivatization combined with an online solid-phase dehydration derivatization GC/MS system. Biological samples were extracted with HCl solution and an acetonitrile–toluene mixture, followed by NaCl-assisted liquid–liquid partitioning to remove proteins and polar ionic matrix components. The organic phase was loaded onto an anion-exchange SPE cartridge, where FFAs were retained, dehydrated by acetone washing, and derivatized on the solid phase at room temperature within 1 min. The derivatives were directly introduced into GC/MS. Spike-recovery experiments using biological samples showed good recoveries and reproducibility, demonstrating that the method provides rapid, accurate, and automated analysis of FFAs.