The current international reference method (IP585/10) for the determination of rapeseed methyl ester (RME) in jet fuel [aviation turbine fuel (AVTUR), current specifications U.S. ASTM 1655 and DEF STAN 91-91] uses gas chromatographymass spectrometry (GC-MS). The fuel matrix requirements demand that a slow temperature gradient method (50 min) must be used. The fuel matrix also limits the application of this approach in relation to the detection and quantification of low-carbon-number fatty acid methyl esters (FAMEs), e.g., coconut methyl ester (CME), C8-C14 from coconut oil, a feedstock for FAME production in the Pacific Rim region. A 3 min ultrahigh-performance supercritical fluid chromatographymass spectrometry (UHPSFC-MS) method has been developed for the analysis of RME and CME. This is compared to the existing reference method and an adapted form of the reference GC-MS method for the detection of low-carbon-number FAMEs. The UHPSFC-MS method is approximately 20 times faster than the ASTM reference method, affords a comparable linear dynamic range for the detection of total FAME content up to 100 ppm with a linear correlation (R-2 > 0.99 for RME), and is more suitable for the detection and quantification of lower chain length methyl esters.