A rapid methodology for direct analysis of meat acylglycerides is proposed. A transesterification is carried out in a microwave reactor consisting of a monomode oven using chlorotrimethylsilane (CTMS) and methanol. High-temperature gas chromatography was used to check the absence of underivatized acylglycerides. Whereas transesterification is complete after 30 s at 90 °C in the microwave method, the reference method needs 2 h to complete this process. Moreover, the CTMS–microwave method shows higher recoveries of individual saturated, monounsaturated and polyunsaturated fatty acids. No influence of microwave irradiation on the composition of the fatty acids was observed. ; This work was supported in part by a Grant-in-Aid from the Secretaría de Estado de Política Científica y Tecnológica of the Spanish Ministry of Education and Science (contract grant number: CTQ2006-07451/PPQ). The authors are grateful to Ferran Gatius for his contribution in the statistical analysis.