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    • 6. 发明授权
    • Purification of salts of riboflavin 5'-phosphate, in particular of
monosodium riboflavin 5'-phosphate
    • 核黄素5'-磷酸盐,特别是核黄素5'-磷酸一钠的盐的纯化
    • US4987229A
    • 1991-01-22
    • US323795
    • 1989-03-15
    • Walter DoblerManfred EggersdorferJoachim Paust
    • Walter DoblerManfred EggersdorferJoachim Paust
    • C07D475/14C07F9/6561
    • C07F9/65618
    • Salts of riboflavin 5'-phosphate which are obtained by phosphorylation of riboflavin and reaction of the resulting riboflavin 5'-phosphate (5'-FMN), contaminated with unconverted riboflavin and isomeric riboflavin monophosphates and diphosphates, with an alkali metal hydroxide or a nitrogen base are purified by a process in which(a) a roughly 1-15% strength by weight homogeneous, clear, aqueous 5'-FMN salt solution having a pH of from 4 to 7 is prepared from the crude 5'-FMN obtained in the phosphorylation, water and the alkali metal hydroxide or the nitrogen base, preferably sodium hydroxide solution, if necessary with heating at from 30.degree. to 100.degree. C.,(b) the resulting solution is treated with a suitable polymeric adsorber resin and(c) the 5'-FMN salt substantially freed from unconverted riboflavin is isolated from the resulting solution and, if desired, the solution is fed to a subsequent fine purification.Treatment with the suitable polymeric adsorber resin is advantageously carried out in a column filled with adsorber resin. The subsequent fine purification can be effected by evaporative crystallization or by chromatographing a 5'-FMN solution, containing from 1 to 15% by weight of dry substance, in water or in a mixture of water and a lower aliphatic alcohol, having a pH of from 4 to 7, in a minimum amount of from 5 to 50% of the bed volume of the column over RP silica gel derivatized with alkyl groups, using water, or a mixture of water and a lower aliphatic alcohol, as the eluant. Preparative chromatography of 5'-FMN salts over derivatized RP silica gel using water, or a mixture of water and a lower aliphatic alcohol, as the solvent and eluant is also claimed independently of pretreatment with the suitable adsorber resin.
    • 通过核黄素磷酸化获得的核黄素5'-磷酸盐的盐和由未转化的核黄素和异构核黄素单磷酸酯和二磷酸酯污染的所得核黄素5'-磷酸(5'-FMN)与碱金属氢氧化物或氮 碱通过以下方法纯化,其中(a)从所得粗制5'-FMN制备了具有约1-15%重量的均匀,透明的pH5-4的5-FMN盐水溶液, 磷酸化,水和碱金属氢氧化物或氮碱,优选氢氧化钠溶液,如果需要,在30℃至100℃下加热,(b)所得溶液用合适的聚合物吸附树脂处理,(c )从所得溶液中分离出基本上未转化的核黄素的5'-FMN盐,并且如果需要,将溶液加入到随后的精细纯化中。 用合适的聚合物吸附树脂处理有利地在填充有吸附树脂的柱中进行。 随后的精细纯化可以通过蒸发结晶或通过色谱法将含有1至15重量%干物质的5-FMN溶液在水或水和低级脂族醇的混合物中进行,其pH为 作为洗脱剂,使用水或水和低级脂族醇的混合物,用烷基衍生的RP硅胶的柱体积的最小量为5至50%。 独立于合适的吸附剂树脂的预处理,也要求使用水,或水和低级脂族醇的混合物作为溶剂和洗脱剂的衍生化RP硅胶的5-FMN盐的制备色谱法。