A method for extracting refined polyprenol from ginkgo biloba dregs

A technology of polyprenol and ginkgo biloba, applied in chemical instruments and methods, preparation of oxygen-containing compounds, preparation of hydroxyl compounds, etc., can solve the problems of low purity and low utilization value of polyprenol, and achieve increased purity and production The effect of large batch and high purity

Active Publication Date: 2018-09-14
NANJING UNIVERSITY OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The polyprenol obtained by the traditional method has low purity and low utilization value

Method used

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  • A method for extracting refined polyprenol from ginkgo biloba dregs
  • A method for extracting refined polyprenol from ginkgo biloba dregs
  • A method for extracting refined polyprenol from ginkgo biloba dregs

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1 The optimization of polyprenyl alcohol extraction single factor

[0031] In the production process of ginkgolide injection, the ginkgo leaves were decocted in water for 3 times, and the dregs of ginkgo leaves produced after 2 hours each time were divided into six parts, one part was not crushed, and the rest were crushed into Nos. Sieve (pharmacopoeia standard), add ginkgo biloba dregs raw material weight-to-volume ratio (1:10, 1:20, 1:30, 1:40, 1:50) (n-hexane, petroleum ether, ethyl acetate) , presoak (0, 0.5, 1, 1.5, 2h), extract (0.5, 1, 1.5, 2, 2.5h) under (20, 30, 40, 50, 60°C) conditions, extract (1, 2, 3 times. Suction filtration, draw 2mL extract, add 2mL 4% sodium hydroxide methanol aqueous solution, ultrasonic 1h, the solution is concentrated to dryness by rotation, add 2mL n-hexane, enter high-performance liquid chromatography, measure the content of polyprenol, and select out relatively best factor level. The results are shown in Table 1:

...

Embodiment 2

[0034] Example 2 Orthogonal optimization test of polyprenyl alcohol extraction

[0035] Taking the particle size, presoaking time, extraction time and extraction temperature of Ginkgo biloba raw material as the investigation factors, the optimal extraction scheme was determined through orthogonal experiments.

[0036] Table 2 Arrangement and results of polyprenyl alcohol extraction process test

[0037]

[0038] Table 3 polyprenol extraction analysis of variance results

[0039]

[0040]The results of range R showed that the degree of extraction process affecting polyprenol in Ginkgo biloba dregs was as follows: D (particle size) > A (presoaking time) > C (extraction temperature) > B (extraction time), A, The two factors D (P2 B 1 C 1 D. 2 , that is, the raw material of ginkgo biloba leaves is passed through a No. 3 sieve, the presoaking time is 0.5h, the extraction temperature is 40°C, and the extraction time is 1h.

Embodiment 3

[0041] Embodiment 3 The optimization of polyprenol hydrolysis single factor

[0042] Ginkgo biloba dregs produced during the production of ginkgolide injection were crushed through a No. 3 sieve, and petroleum ether with a ratio of raw material weight to solvent volume of 1:30 was added, presoaked for 0.5 h, extracted at 40°C for 1 h, and extracted twice . Suction filtration, draw 2mL extract, add 2mL (mass concentration 1%, 2%, 4%, 6%, 8%) sodium hydroxide (methanol, ethanol) water (alcohol water volume ratio is 1:4, 2 :3, 3:2, 4:1, 0:1) solution, ultrasonic (10, 20, 30, 40, 50, 60min), ultrasonic frequency (60, 70, 80, 90, 100KHz), solution rotary concentration To dryness, add 2mL of n-hexane, enter the high-performance liquid chromatography, and optimize the optimal factor level. The results are shown in Table 4:

[0043] Table 4 polyprenol hydrolysis single factor preferred experimental results

[0044]

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Abstract

The invention discloses a method of extracting refined polyprenol from ginkgo leaf residue. Through a lot of experiments, optimal ethyl ether extraction process, sodium hydroxide hydrolysis process, acetone impurity-removing process and silica gel column chromatography and C18 column chromatography impurity-removing process are screened out. Waste ginkgo leaf residue is used as a raw material, so that waste is recycled; the whole method is reasonable in design and high in operability; purity of polyprenol prepared by the method can reach higher than 95%, the method is supportive of industrial production and has important application value, and the defect that polyprenol prepared by the prior art is low in purity and application value can be overcome.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a method for extracting and refining polyprenol from ginkgo biloba dregs of ginkgolide injection. Background technique [0002] Ginkgo biloba polyprenol is a betulin alcohol polyprenol composed of 14-24 (mainly 17-19) isopentenyl units. Alcohol is close in structure and can be metabolized into dolichyl phosphate in the human body as a carrier for glycoprotein biosynthesis. The analysis of the content of polyprenol in Ginkgo biloba leaves shows that the content of polyprenol in green leaves or yellow leaves is relatively high, as high as 1.0% to 1.5%, and some even reach 1.96%. [0003] A large amount of solid waste is produced in the production process of ginkgolide injection, which contains many types of non-lactone resource chemical substances, including rich polyprenol and flavonoid resource chemical substances. The traditional treatment methods of medicinal residues, su...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C27/02C07C29/74C07C29/76C07C29/86C07C33/02
CPCC07C29/095C07C29/74C07C29/76C07C29/86C07C33/02
Inventor 刘培段金廒钱大玮江曙
Owner NANJING UNIVERSITY OF TRADITIONAL CHINESE MEDICINE
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