著者
大前 雅彦 勝井 五一郎
出版者
公益社団法人 日本ビタミン学会
雑誌
ビタミン (ISSN:0006386X)
巻号頁・発行日
vol.39, no.3, pp.181-189, 1969

The products of the photolysis of vitamin K_1 in benzene solution were subjected to thin layer chromatograpy using silica gel and chloroform as solvent to give colored spots with Rf of 0 (spot 4), 0.21 (spot 5) and colorless spot with Rf of 0.56 (spot 6) along with other spots. Spot 5 and 6 were elucidated as 5-hydroxy-4-methyl-6,7-benzocoumaran-3-one and phytone, and spot 4 was revealed to be polymer which had the same structure as spot 5.
著者
山野 喜昭 池谷 理 大前 雅彦 河部 靖
出版者
公益社団法人 日本薬学会
雑誌
YAKUGAKU ZASSHI (ISSN:00316903)
巻号頁・発行日
vol.99, no.11, pp.1102-1110, 1979-11-25 (Released:2008-05-30)
参考文献数
8
被引用文献数
2 8

In order to study cis-trans photo-isomerization of phylloquinone (K) and menaquinone-4 (MK-4), a high-performance liquid chromatographic method for the determination of cis-trans isomers was developed. After removal of the surface active agent and photo-decomposition products, cis-trans isomers were separated on a Nucleosil 50 (particle size ; 5 μm) column using di-n-butyl ether-n-hexane (6 : 94) as a mobile phase. The internal standards used were MK-4 for K and K for MK-4. When either cis or trans compound of K and MK-4 were photo-irradiated in benzene, cis⇌trans photo-isomerization was observed and an equilibrium favoring the trans isomers was attained. Trans→cis photo-isomerization of MK-4 was also observed in injection and in infusion solution. Photo-isomerization and photolysis in their solution were inhibited considerably by using a light-intercepting shade.
著者
阿部 皓一 石橋 恭子 大前 雅彦 河部 靖 勝井 五一郎
出版者
日本ビタミン学会
雑誌
ビタミン (ISSN:0006386X)
巻号頁・発行日
vol.51, no.3, pp.111-117, 1977-03-25
被引用文献数
2

A Method for the determination of ubiquinone homologues (UQ) in serum and liver is described. Serum or liver homogenate was saponified with methanolic alkaline solution after addition of 2,3,6-trimethyl-5-nonaprenyl-1,4-benzoquinone (TQ-9) as an internal standard and then extracted with n-hexane. The n-hexane extract was evaporated under N_2 gas at 30℃, and the residue was dissolved in dioxane. The sample solution was applied to the high-speed liquid chromatography (HSLC) using a Permaphase ODS column and ethanol・water (80 : 20) as a mobile phase. The peaks of UQ and TQ-9 were not disturbed by other fat-soluble substances when an on-line high-sensitive multiple wavelength detector set at 275 nm (absorption maximum of UQ) was used as a detector. The proposed HSLC method was found to be more simple and specific than the other conventional determination methods.