猪胆汁中三种主要胆汁酸的提取分离

目的从提取胆红素下脚料中同时提取三种胆汁酸。方法混合猪胆汁酸粗品在硫酸催化下形成甲酯,利用猪去氧胆酸甲酯与苯形成的加合物不溶于苯的性质将其分离出来;用乙酸酐将剩余胆汁酸甲酯中的所有羟基转化为乙酸酯,利用猪胆酸甲酯三乙酸酯在正己烷中溶解度低的性质,使其分离,最后用无水乙醇结晶分离出鹅去氧胆酸甲酯二乙酸酯。所得各种猪胆汁酸酯经乙醇-NaOH溶液水解得到纯猪去氧胆酸、猪胆酸和鹅去氧胆酸,并对产物结构进行了表征,纯度经HPLC测定均大于98%。结果通过一次工艺流程分离出三种胆酸,含量均大于98%。结论该提取工艺提高了原料的利用率,适合工业化生产。

The extraction and purification of three kinds of bile acids from pig bile

Purpose To prepare three bile acids from the mixed pig bile acids.Methods The mixed pig bile acids were first methyl-esterified then methyl hyodeoxycholanate was separated and recrystallized from benzene because of the insolubility of methyl hyodeoxycholanate-benzene complex in benzene,The mother liquor was distilled and then acetic acid anhydride was added to make all the hydroxyl of bile acid methyl esters transforming to acetate ester.Methyl hyocholanate triacetate was separated in hexane,methyl chenodeoxycholanate diacetate was precipitated from ethanol,and purified by recrystallization from methanol.After hydrolyzing of the three kinds of separated bile acid methyl esters,three individual components whose purities were higher than 98% were obtained.Results By this extraction process could be isolated pure hyodeoxycholic acid,hyocholic acid and chenodeoxycholic acid at one time with short steps,simplified method and less solvent.Conclusion The route,which could not only make the best recycle of raw material,but also reduce environmental pollution,is applicable to the industrial production.