首页> 外国专利> METHOD FOR PURIFYING SALTS OF RIBOFLAVIN 5'-PHOSPHATE, ESPECIALLY MONONATRIUM RIBOFLAVIN 5'-PHOSPHATE

METHOD FOR PURIFYING SALTS OF RIBOFLAVIN 5'-PHOSPHATE, ESPECIALLY MONONATRIUM RIBOFLAVIN 5'-PHOSPHATE

机译:纯化核黄素5'-磷酸盐,特别是单核类核黄素5'-磷酸盐的盐的方法

摘要

Process for the purification of salts of riboflavin 5'-phosphate obtained by phosphorylation of riboflavin and reaction of the riboflavin 5'-phosphate (5'-FMN) contaminated with unreacted riboflavin and isomeric riboflavin monophosphates and diphosphates and formed in this process with alkali metal hydroxides or nitrogen bases, which is characterised in that… a) an approximately 1 to 15% strength by weight homogeneous, clear, aqueous 5'-FMN salt solution having a pH 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, optionally with warming at 30 to 100 DEG C,… b) the solution obtained is treated with a suitable polymeric adsorber resin and… c) the 5'-FMN salt largely purified of unreacted riboflavin is isolated from the solution obtained in this process and, if desired, the solution is submitted to a subsequent fine purification. …??The treatment with the suitable polymeric adsorber resin is advantageously carried out in a column packed with adsorber resin. The subsequent fine purification can be carried out by means of crystallisation by evaporation or by chromatography of a 5'-FMN solution containing 1 to 15% by weight of dry material in water or a mixture of water and a lower aliphatic alcohol having a pH between 4 and 7 in a minimum amount of 5 to 50% of the bed volume of the column on RP silica gel derivatised with alkyl groups using water or a mixture of water and a lower aliphatic alcohol as the eluent. The preparative chromatography of 5'-FMN salts on derivatised RP silica gel with water or a mixture of water and a lower aliphatic alcohol as the solvent and eluent is also claimed independently of the pretreatment with the suitable adsorber resin.
机译:通过核黄素的磷酸化得到的核黄素5'-磷酸盐的纯化方法,以及被未反应的核黄素和异构核黄素单磷酸和二磷酸盐污染的核黄素5'-磷酸(5'-FMN)的反应,并在此过程中与碱金属形成氢氧化物或氮碱,其特征在于……a)由所得的粗制5'-FMN制备pH为4-7的约1-15%重量均匀,透明的5'-FMN盐水溶液。在磷酸化,水和碱金属氢氧化物或氮碱(最好是氢氧化钠)溶液中,可选地在30至100℃下加热,…b)将所得溶液用合适的聚合物吸附树脂处理,……c)从在该方法中获得的溶液中分离出未反应的核黄素的大量纯化的5'-FMN盐,并且如果需要,将该溶液进行随后的精细纯化。 ……用合适的聚合物吸附剂树脂处理最好在装有吸附剂树脂的塔中进行。随后的精细纯化可以通过蒸发或通​​过色谱法对5'-FMN溶液进行结晶,所述5'-FMN溶液包含1至15重量%的干物质在水中或水与pH值在5至10之间的低级脂肪醇的混合物在使用水或水与低级脂族醇的混合物作为洗脱剂,经烷基衍生的RP硅胶上,柱床的床体积的最小数量为床床体积的5至50%(最小值)为4和7。还要求保护了在衍生的RP硅胶上用水或水与低级脂肪醇的混合物作为溶剂和洗脱液的5'-FMN盐的制备色谱,而与用合适的吸附树脂进行的预处理无关。

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