| Summary: | To address limited food frequency questionnaire (FFQ) capacity in public health monitoring in Malaysia, we aimed to develop a semi-quantitative FFQ for an adult multiethnic population for comprehensive fatty acid (FA) profiling inclusive of saturated (SFA), monounsaturated (MUFA), polyunsaturated fatty acids (PUFA), PUFA:SFA ratio, trans fatty acids, omega-3 and omega-6 FAs. A 240-food itemed FFQ used diet records (DR) of Malaysia Lipid Study (MLS) participants and fatty acid composition database from laboratory analyzed foods. The developed MLS-FFQ underwent face and content validation before relative validation in a free-living population (<i>n</i> = 114). Validation was facilitated for macronutrient data comparisons between DR and FFQ via Spearman’s correlation coefficient analyses; and for fatty acid composition data by independent pairing of DR, FFQ and plasma triglyceride using the triads method. Moderate correlation between dietary methods was obtained for macronutrients and FAs (<i>r</i> = 0.225–0.457, <i>p</i> < 0.05) except for ω-3 FAs, presenting good agreement with grossly misclassified nutrients <10%. For fatty acid composition data, the magnitude of validity coefficients (<i>z</i>) for SFA, PUFA, PUFA:SFA ratios and ω-6 FAs by all 3 methods were not significantly different (<i>p</i> > 0.05). In conclusion, the MLS-FFQ was shown to be a valid tool to assess population dietary intakes.
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