摘要
本文对牛磺熊去氧胆酸(Tauroursodeoxycholic acid,简称TUDCA)结构及性质进行了研究,结果表明:游离TUDCA是易溶于水的酸性化合物,其1%水溶液pH 2～3;差热分析测得其含两分子结晶水,且mp为180.4℃;元素分析结果,其C、H、N平均含量分别为57.75%、8.77%及2.61%;红外光谱表明具有典型的酰胺基、羟基及磺基吸收;^(13)SCNMR表明酰基C_(24)δ为177.4 ppm,羟亚甲基C_及C_7 δ均为71.7 ppm,牛磺酸基团中C_(25)及C_(26)的δ分别为37.6 ppm及50.8 ppm;质谱分析测得其(MWNa)+为522,与计算值521.70完全相同;比旋光度测定结果,其[α]_D^(17.5)=+43.28°,与计算值相一致;薄层层析结果R_f值为0.3.～0.32;磺酸基试验及其水解产物薄层色谱结果确证其分子中含磺酸基及熊去氧胆酸(UDCA)基团;几种胆酸Gregory-Pascoe反应物吸收光谱还表明,TUDCA分子中牛磺酸基团对显色反应产生显著影响。
This paper mainly deals with the structure and properties of free TUDCA. TUDCA is a water-soluble and white powder. The pH value of the 1% TUDCA solution is about 2-3. This compound contains two molecule of H_2O with rap. of 180℃, containing C, H and N 57.75%, 8.77% and 2.61% respectively, consistent with the expectant value. The result of infra-red spectrum studies shows that the U_(CON) is 3391 cm^(-1)and 1683 cm^(-1) and that U_(SOS) is 1367 cm^(-1). The spectrum of ^(13)CNMR shows that the δ of C_(24) is 177.4 ppm and the δ of C_3 and C_7 is 71.7 ppm, the δ of C_(25) and C_(26) is 37.6 and 50. 8 ppm respectively. The molecular weight of TUDCA is 522 by the method of mass spectrum, consistent with the calculating value 521.70. The [α]_D^(17.5) is+43.28° by using optical rotational analysis. The R_t value is ranging from 0.31 to 0.32 by thin-layer chromatography. This compound contains the basis of sulphonic acid group and UDCA group. The absorhtion experiment of several cholic acids Gregory Pascoe Reaction has indicated that there are significant effects of sulphonic acid group on color reaction.
出处
《中国药科大学学报》
CAS
CSCD
北大核心
1993年第3期145-149,共5页
Journal of China Pharmaceutical University
关键词
牛磺
熊去氧胆酸
差热分析
TUDCA
UDCA
CDCA
TLC
Thermo-gravimetric analysis
