7,8-二甲基-10-(D-1-核糖醇基)-异咯嗪半合成中间体气相色谱分析  

Gas Chromatographic Analysis of the Intermediates in 7,8-Dimethyl-10-(D-1-ribityl)-isoalloxazine Production

作　　者：邓国才[1] 杨四海[1] 陈荣悌[1] 王健刚[2] 

机构地区：[1]南开大学化学系,天津300071 [2]天津市红十字医院,天津300130

出　　处：《分析化学》1999年第4期419-422,共4页Chinese Journal of Analytical Chemistry

摘　　要：提出以三氟乙酸酐作为衍生化试剂,将核黄素半合成中问体N-(D)-脱氧核糖醇基-3,4-二甲苯胺(Ⅰ)及4,5-二甲基-N-(D)-脱氧核糖醇基-2-偶氮苯基苯胺(Ⅱ)转化为低沸点易汽化物质,采用以苯乙酮作内标,测定中间体(Ⅰ)和(Ⅱ)纯度的气相色谱法.方法具有分析速度快、准确度高、重现性好等优点,方法回收率(Ⅰ)为96.9%～101.2%、(Ⅱ)为99.4%～100.4%,相对标准偏差(Ⅰ)在4.4%、(Ⅱ)在2.6%以内.The intermediates of riboflavin production, 1-deoxy-l-[(3,4-dimethylphenyl)amino]-D-ribitol(Ⅰ) and 1-deoxy-1-[4, 5-dimethyl-2-( phenylazo) phenylamino]-D-ribitol (Ⅱ), were convertedinto volatile derivatives using trifluoroacetic anhydride as a derivative agent, and then determined by gaschromatography with acetophenone as internal standard. It has many advantages, such as rapid analysis,high precision and good reproducibility. In addition, by using this method the two intermediates could beanalyzed in 10 minutes , the recovery of ( Ⅰ) and ( Ⅱ) was 96.9%-101.2% and 99.4%-100.4%for the determination of 30-103 mg (Ⅰ) and 127-259 mg(Ⅱ) ( n = 4) respectively, the relativestandard deviation was less than 4.4% and 2.6% respectively.

关 键 词：气相色谱法 核黄素 合成 中间体 测定 

分 类 号：TQ463.4[化学工程—制药化工]