酸化魚油の抗菌作用に関する研究-II : 酸化イカ肝油methyl ester中のcarbonylのpaper chromatographyによる分離・同定
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In the present paper experiment were done to separate, identify and estimate carbonyls in the oxidized methyl ester. By the combined use of column and paper chromatography and spectrophotometry, the joint quantitative and qualitative analyses for carbonyls were successfully carried out. For the enrichment of carbonyls from the oxidized calamary oil methyl ester, steam distillation and acetic acid extraction were employed. Carbonyls were converted to 2, 4-dinitro-phenylhydrazones. The derivatives were fractionated on the basis of the molecular weight of the parent carbonyls except 2, 4-dienal by chromatography on columns of silica gel and celite analytical filter aid (2:1) with 2 ?? 6% ether solution in hexane as a developing solvent. The fractions were resolved into classes of carbonyls by paper chromatography using Toyo No. 51 filter paper and 5% ether solution in hexane as a developing solvent. Both paper chromatographic separation of the classes of carbonyls into the individual components and their identification were made by using Toyo No. 51 A filter paper impregnated by dipping in 7% vaseline solution in hexane and 96% methanol as a developing solvent. Butanal, pentanal, hexanal, heptanal, nonanal, 2-butenal, 2-heptenal, 2-octenal, and 2, 4-undecadienal were found in steam distillate. In ligroin and 85% acetic acid soluble fraction butanal, pentanal, hexanal, heptanal, 2-butenal, 2-heptenal, 2-octenal, and 2, 4-undecadienal were found (Table 2, 3 and 4). Spectrophotometric examination of the column chromatographic fractions and paper chromatographic spots in vaseline-methanol system permitted the differential determination of all carbonyls in the oxidized calarnary oil methyl ester (Table 5). Further investigations were carried out on carbonyls in ligroin insoluble fraction, and the possibility of polymerization taking place through an oxygen linkage was considered.
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