CNSL contains phenolic lipids with aliphatic chains such as anacardic acid, cardanol, cardol, and methyl cardol, and their derivatives. The developed GC/MS method was rapid, accurate, and selective using a selected derivatizing reagent namely N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA) that was previously diluted 1:1% with anhydrous pyridine. The proposed GC/MS method was applied for the analysis of different CNSL samples, the results showed that all classes of the CNSL compounds were detected. The four alkyl phenols were purely detected with their different alkyl sidechains without any interference. This method is also specified for detection of fatty acid of saturated and unsaturated chains. Silylation did not affect any alteration in the chemical structure of CNSL compounds regardless esterification action. Silylation considered a safe derivatizing agent compatible with GC chromatography and specific for all volatile and non-volatile polar and nonpolar CNSL compounds could be detected in CNSL sample.