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
藤田 忠男 里 忠 内山 幹男 星田 晴彦 河部 靖 屋代 順治郎 若林 高明
出版者
公益社団法人日本薬学会
雑誌
衛生化学 (ISSN:0013273X)
巻号頁・発行日
vol.28, no.2, pp.106-110, 1982-02-28

Bonding between iron ions and soybean protein (produced by the hydrolysis of soybean meal) in an iron-protein compound, which was prepared by mixing the soybean protein and iron (II) sulfate solution, was studied by infrared spectroscopy and an X-ray powder diffraction method. The oxidation state of the predominant iron ions within the compound was +3,but some Fe (II) ions were also present. In the infrared spectrum of the iron-protein compound, the band ascribable to stretching of the COO^-group was shifted to the higher frequency side by 40 cm^<-1> in comparison with that of the free protein. No evidence was found for the formation of any crystalline iron compounds such as Fe_2O_3,Fe_3O_4 and FeO in the X-ray powder patterns. The possibility of the formation of gel-like compounds of iron (II) and iron (III) such as Fe(OH)_2 and Fe(OH)_3,respectively, was excluded, because the hydrolyzed product of iron (II) is easily oxidized to iron (III) and Fe(OH)_3 transforms, at least partly to Fe_2O_3 or Fe_3O_4 after aging or storing the product in air. Thus, we concluded that the iron ion is bound to the soybean protein molecule through one or more carboxyl groups. Although other coordination sites within the protein molecule could also combine with the iron ions, we could not find evidence for other bondings.
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.