A very sensitive and efficient high performance liquid chromtographic (HPLC) method for measuring 0.5-50ng of free and acylated sterylglycosides (FSG and ASG) in oils in the form of their 1-anthroylnitrile derivatives has been developed. Before to derivatization, the whole sterylglycosides were simply isolated with silica gel cartridge then fractionated via thin layer chromatography (TLC) into pure FSG and ASG. Derivatization was done on the FSG molecular species, therefore ASG was converted into FSG with mild alkaline hydrolysis. The derivatives separated by reversed phase mode were detected at 254nm. Avenasterylglycoside can not be separated from isofucosterylglycoside and campesterylglycoside from stigmasterylglycoside. The method was successful with to different vegetable oils commercially extracted with hexane as well as those laboratory-extracted with a polar solvent mixture.
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