Myo-inositol　(MI)　is　one　of　the　stereoisomers　of　hexahydroxycyclohexane,　which　plays　an　important　role　in　intracellular　signal　pathway.　Derivatization　is　an　indispensable　step　in　both　external　and　internal　standard　method　during　the　chromatography-mass　spectrometer　(GC–MS)　detection,　as　MI　can＇t　be　ionized　directly.　It　is　valuable　to　optimize　the　derivative　process　and　the　detection　volume　for　clinical　detection.　This　article　contains　optimization　data　related　to　research　publication　“Quantification　of　plasma　myo-inositol　using　gas　chromatography–mass　spectrometry”　[1].　Here　we　introduce　the　data　on　the　optimized　derivatization　volume,　temperature,　duration　and　the　detection　volume.　©　2016　The　Authors