Abstract
Quantitative cleavage of epoxyoctadecanoates with periodic acid (HIO4) has been demonstrated and the technique incorporated into an all gas chromatographic system for detailed lipid analysis. The overall procedure involves three sequential gas chromatographic separations interspersed by two microreactions. By this procedure, a complete analysis forcis- andtrans-geometric isomers corresponding to each positional octadecenoate isomer is obtained. Total sample requirements are less than 10 mg, and the elapsed analysis time/sample is less than 10 hr. In this all gas chromatographic procedure, a lipid methyl ester sample is first separated by preparative gas chromatography, and the monoene fraction is collected and epoxidized. Next, the epoxidized sample is separated by gas chromatography intocis- andtrans-epoxyoctadecanoate fractions. These epoxyoctadecanoate fractions are collected and cleaved with HIO4 into aldehyde and aldehyde-ester fragments, which are quantitatively analyzed by gas chromatography. The double bond positions are determined from the aldehyde and aldehyde-ester cleavage data, which are stored and processed by a computerized on-line gas chromatographic data acquisition system. The procedure was tested on pure octadecenoate isomers, standard mixtures, and commercially hydrogenated vegetable oils. Analyses of hydrogenated vegetable oils are compared with data acquired by reverse-phase and argentation chromatography followed by reductive ozonolysis.
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ARS, USDA.
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Emken, E.A., Dutton, H.J. Sequential gas chromatographic procedure for microanalysis of monoenoic double bond position in hydrogenated oils. Lipids 9, 272–278 (1974). https://doi.org/10.1007/BF02532205
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DOI: https://doi.org/10.1007/BF02532205