Method for separating and refining polyprenol in ginkgo biloba extract

Abstract

The invention relates to a method for separating and refining polyprenol in ginkgo biloba extract. The method comprises the following steps: placing polyprenol extract in alcoholic lye to fully stir, saponifying at 30-80 DEG C for 0.5-4h, neutralizing the reaction liquid with acid, concentrating to obtain the saponified polyprenol extract; dissolving urea in loading solvent, adding carrier to ensure that urea is loaded on the carrier, removing solvent, preparing stationary phase; performing the column-packing of the prepared stationary phase, then adding the saponified polyprenol extract in the column, injecting mobile phase in the chromatographic column at a constant speed to elute, collecting elution components during different periods; combining the elution components which are rich inpolyprenol, concentrating and evaporating; dissolving polyprenol which is processed by the urea column chromatography in the refluxed methanol, ethanol or acetonitrile to obtain saturated solution, freezing to crystallize, filtering, and drying to obtain polyprenol. The method of the invention has the advantages of mild operating conditions, high process recovery, high production purity, simple process and low operation cost.

Description

technical field [0001] The invention relates to a method for extracting and purifying polyprenol from ginkgo biloba extract. Background technique [0002] Polyprenol, also known as polyi soprenol (polyi soprenol), is a general term for isoprene monomers (prenyl) linked into a linear polymer compound, which exists widely in nature. Weak polarity, easily soluble in organic solvents. Polyprenol is a long-chain fatty alcohol with multiple non-conjugated double bonds in its structure, which has a very strong ability to absorb free radicals. The polyprenol compound present in mammals is called dolichol, which is an important sugar carrier in the synthesis of glycoproteins in biofilms, but its content is extremely low, and the content of polyprenol in Ginkgo biloba can account for dry leaves. 1 to 2% by weight, it is considered to be the most suitable intermediate for the synthesis of animal dolichols. The polyprenyl alcohol compounds in Ginkgo biloba are non-toxic to human body...

AI Technical Summary

Problems solved by technology

Polyprenol and a variety of complex chemical components exist in Ginkgo biloba and its extract, which is difficult to separate and store, with many steps and limited refining effect

Since polyprenol is a long-chain polyprenyl alcohol with weak polarity, it is very similar to the physical and chemical properties of the waxy substance in the extract, which brings great challenges to the separation and storage of polyprenol

[0004] Invention patent CN01113696.0 uses methods such as solvent precipitation, extraction and silica gel column chromatography to refine polyprenol, and can obtain polyprenol products with a purity of 95%. Invention patent CN200410041670.4 utilizes secondary molecular distillation method, 75-95% polyprenol product can be obtained; the invention patent CN200410074088.8 utilizes the method of supercritical carbon dioxide fractionation to obtain a polyprenol product with a content of 80%; solvent precipitation and silica gel column chromatography can Most of the polar substances in the product are removed, but the effect on waxy substances close to the physical and chemical properties (including polarity) of polyprenol is very limited; molecular distillation has the advantages of cleanness and greenness, but its theoretical basis is based on the substance Because the molecular weight of waxy substances and polyprenol has a wide range of distribution, the intersection of molecular free paths is very large, so it is difficult to separate the product by molecular distillation alone. In addition, molecular distillation must be carried out under high vacuum and high temperature, which will increase the possibility of destroying the structure of polyprenol in the product; the fractional separation of supercritical carbon dioxide is based on different temperatures and pressures Under the condition of supercritical carbon dioxide, the solubility changes of different substances are separated and purified, which often requires that the separated substances have certain differences in parameters such as polarity or molecular weight, but the waxy substances in Ginkgo biloba extract and polypentyl Enols are substances with extremely weak polarity and a wide distribution range of molecular weight. Therefore, although supercritical carbon dioxide fractionation can obtain polyprenol with a content of 80%, it is at the cost of sacrificing the yield of the process

It can be seen that in the existing process, there is no separation step for the waxy substance in the product, so the product also contains a certain amount of waxy substance, in order to obtain a higher polyprenol product of purity, It must go through a complicated process, and the process yield is often very low

The industrialized production of polyprenol is restricted