熊胆粉中3个新胆汁酸的结构研究与确定  

Structure determination of three novel bile acids from bear bile powder

作　　者：简龙海[1] 毛秀红[1] 王柯[1] 季申[1] 

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《药学学报》2013年第8期1297-1300,共4页Acta Pharmaceutica Sinica

摘　　要：为了研究熊胆粉中的新胆汁酸结构,采用液相色谱四极杆飞行时间质谱法(LC-QTOF/MS)结合化学反应进行分析。首先取牛磺熊去氧胆酸和牛磺鹅去氧胆酸对照品,经氯铬酸吡啶氧化后,以LC-QTOF/MS对氧化产物进行分析,可确证所有4个氧化产物的结构,其中含3个同分异构体。再取熊胆粉样品,以甲醇提取后进行LC-QTOF/MS测定,并与上述氧化产物的结果进行比较,可推断熊胆粉中含其中3个氧化产物。A method of LC-QTOF/MS combining with chemical synthesis has been used to determine the structures of three novel bile acids from bear bile powder. Reference substances of tauroursodeoxycholic acid and taurochenodeoxycholic acid were oxidized by pyridinium chlorochromate. The products were analyzed by LC-QTOF/MS. Total 4 products including 3 isomers were predicted and identified according to the PCC oxidation theory and LC-QTOF/MS results. Bear bile powder samples were dissolved by methanol and analyzed by LC-QTOF/MS. Three unknown peaks were found and identified as 2-[[（3β, 5β）-3-hydroxy-7, 24-dioxocholan- 24-yl]amino]-ethanesulfonic acid, 2-[[（5β）-3, 7, 24-trioxocholan-24-yl]amino]-ethanesulfonic acid and 2-[[（5β, 7β）-7-hydroxy-3, 24-dioxocholan-24-yl]amino]-ethanesulfonic acid, separately, by matching their results with that of oxidation products above.

关 键 词：液相色谱-四极杆-飞行时间质谱 熊胆粉 牛磺熊去氧胆酸 牛磺鹅去氧胆酸 

分 类 号：R917[医药卫生—药物分析学]