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Preparation method of ergosterol

A technology of ergosterol and preparation steps, which is applied in the field of preparation of ergosterol, can solve problems such as affecting the yield and decreasing the extraction purity, and achieve the effect of increasing the extraction rate and mild production conditions

Active Publication Date: 2021-02-23
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When three recrystallizations are selected, not only the yield is greatly affected, but the extraction purity will decrease instead

Method used

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  • Preparation method of ergosterol
  • Preparation method of ergosterol
  • Preparation method of ergosterol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] 1. Ultrasonic wall breaking: Weigh 4.50 g of yeast powder and dissolve it in 20 mL of ethanol, place it in an ultrasonic cell grinder (parameters: 40%, 2s / 2s, 10 min), centrifuge (9000 r, 10 min), and take For the supernatant, the operation was repeated twice, and the supernatant was combined and concentrated to obtain ergosterol A, and the precipitate was saponified.

[0074] 2. Saponification extraction: put the above precipitate in a 250 mL eggplant-shaped bottle, add 22.5 mL 70% ethanol to it, then add 45 ml 30% NaOH, place it at 85 o In a C oil bath, react for 2.5 hrs.

[0075] 3. Extraction and concentration: after the reaction is completed, cool to 20-30 o C, add 100 mL ethyl acetate, mix well, let it stand still, take the upper layer; then add 100 ml ethyl acetate to the lower liquid, mix well, let stand, take the upper layer; then add 100 ml to the lower liquid Ethyl acetate, mix well, let stand, take the upper layer, combine the supernatant obtained by three...

Embodiment 2

[0111] The volume ratio of alcohol to alkali is 1:2, the ratio of material saponification agent (m:V) is 1:10, and the influencing factors of saponification conditions are the mass fraction of NaOH solution (A), the volume fraction of ethanol (B), and the saponification time (C), saponification temperature (D), the experimental results are shown in Table 5.

[0112] Table 5 Experimental arrangement and results of saponification conditions

[0113]

[0114] Note: A: mass fraction of NaOH solution; B: volume fraction of ethanol solution; C: saponification time; D: saponification temperature

[0115] From the experimental results of saponification conditions, RAo The saponification temperature of C can make the extraction rate of ergosterol the highest.

Embodiment 3

[0117] Determination of detection wavelength of ergosterol

[0118] Accurately weigh 10 mg of ergosterol standard substance in a 10 mL volumetric flask, add 3 mL of methanol to dissolve it completely, add methanol to the mark and shake well to make it a 1 mg / mL stock solution. Then precisely pipette 1 mL of the stock solution into a 10 mL volumetric flask, add methanol to the mark and shake well to obtain a 100 ug / mL sample solution. Take an appropriate amount of sample solution and blank methanol respectively in a quartz cuvette, and use a UV spectrophotometer to scan its full wavelength.

[0119] UV full-wavelength scan results (see Figure 5 ), the maximum absorption peaks appear at 270.97 nm, 281.38 nm, and 293.08 nm, and the absorption wavelength is selected as 281 nm in this paper.

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Abstract

The invention provides a preparation method of ergosterol, which comprises the following steps: carrying out ultrasonic treatment, saponification and column chromatography purification on a strain, and recrystallizing twice to obtain the ergosterol product. The extraction rate of ergosterol can reach 1.63%, the purity is highe r than 99%, and the content is higher than 95%. According to the method, the advantages of ultrasonic wall breaking and saponification extraction are combined, the two operations are innovatively carried out step by step, and the extraction rate is greatly increased. Inaddition, tests find that in the purification process, recrystallization is carried out twice after column chromatography is finished, and the product purity is the highest and is remarkably superiorto that of one or three times of recrystallization. According to the whole ergosterol preparation method, most of the used solvents can be recycled, the production conditions are mild, batch production is easy to realize in factories, the cost is low, the efficiency is high, and the product is high in quality.

Description

technical field [0001] The invention relates to a preparation method of ergosterol, which belongs to the technical field of biomedicine. Background technique [0002] Ergosterol, also known as ergosterol, is an important component of many microbial cell membranes. It plays an important role in ensuring cell viability, cell membrane fluidity, and cell membrane integrity. It is white needle-like or flaky crystals, insoluble in water, and easily Soluble in organic solvents such as ethyl acetate, benzene, ether, petroleum ether, etc., the chemical structure is as follows figure 1 shown. [0003] Ergosterol is an important pharmaceutical chemical raw material, which can produce medicines such as "cortisone", "progesterone", "hydrocortisone" and "vitamin D2". "Cortisone" is an adrenal cortex hormone used to treat Adrenal insufficiency, inflammation and allergic diseases; "Progesterone", also known as progesterone hormone, luteinizing hormone, is used to protect the endometrium o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
CPCC07J9/00
Inventor 李明媛李媛李萌贾琳
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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