Method for separation and purification of bound total bile acid in bile paste

Abstract

The invention discloses a method for separation and purification of bound total bile in a bile paste. The method is characterized by comprising the following steps of: (1) preparing a bile paste water solution from a raw material bile paste, and cooling; (2) preparing a bound total bile acid precipitate: adding 3-5mol/L diluted acid to the cooled bile paste water solution to regulate pH to 2-5, thus obtaining the bound total bile acid precipitate; and (3) washing the bound total bile acid precipitate, and discarding a washing liquid to obtain high-purity bound total bile acid. The method, on the basis of the researched property of the bound total bile acid which is insoluble in water in an acid environment, achieves the purpose of purification by removing water-soluble impurities through a water washing process, and has the advantages of being low in cost, short in duration, simple in process, high in purity, high in safety and the like, thus being convenient for industrial mass production.

Description

technical field [0001] The invention belongs to the field of biochemical pharmacy, in particular to a method for separating and purifying bound total bile acids in gall paste. Background technique [0002] Bile extract is a traditional Chinese medicine with great medical value and an important raw material in biochemical pharmacy. It is a paste-like substance extracted from the bile of pigs, cattle, sheep and other animals, so it is also called bile extract. The main components of bile cream are bile acid (also known as combined total bile acid), bile pigment, neutral fat, phospholipids, mucin, etc. [0003] Many pharmacological actions of bile cream are mainly the effect of bile acid, and bile acid is the main component of bile cream, mainly composed of cholic acid (CA), chenodeoxycholic acid (CDCA) and deoxycholic acid (DCA) produced in metabolism and A small amount of lithocholic acid (LCA) and trace amount of ursodeoxycholic acid (UDCA) are combined with glycine and tau...

AI Technical Summary

Problems solved by technology

[0010] The above-mentioned ethanol extraction and purification method has the following disadvantages: 1. The amount of 95% ethanol used is large, the recovery rate is low (about 50%) and the cost is high; 2. Ethanol is flammable, and the danger in the purification process is high; 3. The purification process requires Long time; 4. The workshop space required for purification is large

But the weak point of this invention is: the medicinal extract (bile paste) that is extracted with bile must first be mixed with silica gel for column chromatography, stirred, and after the solvent is volatilized, column chromatography is carried out with neutral alumina, and then ethanol Rinse, then use ethanol ethyl ester and methanol as developing solvent to carry out thin layer chromatography, and then use organic solvents to elute and dry to obtain combined total cholic acid

[0016] The weak point of this invention is: the selected raw material is the leftovers after bile extracts bilirubin, and the leftovers are saponified and hydrolyzed with alkali, so that the combined bile acids are hydrolyzed into free type bile acids, and usually the saponification process often requires Heating to a high temperature of 100°C, and the saponification time often takes 12-18 hours, and the saponification process needs to continuously replenish the lost water, the process is complicated and the time is long

This method is characterized in that bear bile powder needs to be subjected to column chromatography to remove water-soluble impurities before saponification, but the disadvantage of this invention is that it is complicated and consumes a large amount of ethanol for elution, and the cost is high

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