As already mentioned, there are several methods, which to choose depends on your research question and what instruments you have access to. GC-MS or GC-FID using internal standard are excellent methods. HPLC with evaporative light scattering detector is also useful, but watch out for the variations in detector respons due variation in chain length and unsaturation. If you wants to measure FFA in plasma, the clinical chemistry kits (enzyme linked reactions) are also useful.