Method for separating and refining bisnorcholenaldehyde

Abstract

The invention discloses a method for separating and preparing bisnorcholenaldehyde (BA) from crystallization mother liquor obtained after extraction of phytosterol fermentation liquor. The fermentation liquor obtained after fermentation of phytosterol through mycobacteria is further subjected to steps of extraction, crystallization and the like for extraction of androstenedione (4AD), a crystallization mother liquor condensed extract after the steps is completely dissolved by low-carbon alcohol, and then filtration is performed to obtain a filtrate containing BA. The filtrate containing BA is adsorbed by a small amount of resin, then is subjected to volatilization drying at a room temperature, and then is added into the top end of a chromatographic column filled with macroporous adsorption resin. Stepwise elution is performed by using mixed solutions of ethanol and water with different concentrations as eluents; and an eluent containing the BA is collected, and the eluent is subjected to evaporating concentration, then is completely dissolved by a mixed solution of methanol, acetonitrile and water, and then is crystallized at a low temperature, and the BA with the purity of 98.5% or more is obtained after filtration and crystal washing. The method is simple in process, the mother liquor can be purified and recycled, the cost is low, industrialization can be realized easily, the process is pollution-free and wastewater-free and is in line with environmental protection requirements, and an obtained product is in line with requirements of the pharmaceutical industry.

Description

technical field [0001] The present invention relates to a method for separating and refining phytosterols, in particular to the method of separating and refining phytosterols from the crystallization mother liquor concentrated extract of phytosterol fermentation liquid by macroporous adsorption resin chromatographic separation and low-temperature crystallization craft. The invention belongs to the technical field of biochemical separation of steraldehyde substances in phytosterol fermentation liquid. Background technique [0002] During the process of phytosterol fermentation to obtain androstenedione (referred to as 4AD), some useful by-products will be produced; after the fermentation broth is separated from the main product androstenedione, the crystallization mother liquor also contains some substances with high application value. Products, such as phytosteraldehydes (referred to as BA), contain about 19% (see attached figure 1 ), if discarded directly, it is not only ...

AI Technical Summary

Problems solved by technology

The main disadvantages of this process are: 1. After the derivatization and reduction of phytosteroids, the chemical structure may change greatly; 2. The purity is not high enough to meet the purity requirements of industrial synthesis, and it also increases the burden. The pressure of the subsequent separation and purification process

The traditional separation methods that can be used for non-polar compounds (phytosteraldehydes also belong to non-polar compounds) include silica gel chromatography, but there are some obvious shortcomings in the silica gel separation process: 1. Use a large amount of organic solvents, easy to The environment will cause pollution; 2. The reusability of silica gel is not high, which increases production costs; 3. The content of concentrated extract of crystallization mother liquor is low, and the amount of separation and treatment using silica gel is small; 4. The process conditions of silica gel chromatography fluctuate greatly and are difficult to control

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