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Method for preparing diosgenin by hydrolysis of ternary two-phase AlCl3

A technology of diosgenin and aluminum trichloride, which is applied in the directions of organic chemistry, steroids, etc., can solve the problems of low saponin yield, complicated process and mechanism, and many by-products, etc., so as to improve the saponin yield, The effect of shortening the extraction cycle and reducing the amount of acid

Active Publication Date: 2020-02-21
SOUTH CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some researchers used Aspergillus oryzae, Trichoderma harzianum, and Aspergillus awamori to inoculate and culture Dioscorea shield leaf to ferment and directly use saponin to convert and extract saponin. etc., the difference is significant, the process and mechanism of saponin hydrolysis in biotransformation are complicated, the yield of saponin is low, and there are many by-products generated
Although the biotransformation of saponin into diosgenin by the combination of biological method and enzymatic hydrolysis has attracted the attention of many researchers, compared with the traditional direct acid hydrolysis method, due to the uneconomical cost of the enzyme preparation and the biological The inefficiency of transformation leads to its limited application in the diosgenin industry
Because the traditional preparation technology saponin is faced with problems such as low yield, high acid consumption, large sewage discharge, unrecoverable starch waste residue and acidic waste liquid, or high resource consumption such as high recovery cost, it is urgent to find a saponin yield Preparation method of diosgenin with high acid consumption and low sewage discharge

Method used

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  • Method for preparing diosgenin by hydrolysis of ternary two-phase AlCl3
  • Method for preparing diosgenin by hydrolysis of ternary two-phase AlCl3
  • Method for preparing diosgenin by hydrolysis of ternary two-phase AlCl3

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Accurately weigh 5.0g Dioscorea chrysanthemum powder and put it into a 300mL Parr reactor, then add 80mL 4.0g / LAlCl 3 A ternary biphasic solution composed of aqueous solution, 75mL of ethanol and 100mL of petroleum ether was stirred evenly, and the reaction kettle was set at a rotation speed of 150rpm, and reacted at an extraction temperature of 150°C for 2.0h. After the end, the diosgenin extract in the petroleum ether organic phase was rotary evaporated, concentrated, crystallized, and dissolved in chromatographic grade methanol for sample preparation. Dioscin was then analyzed and quantified. The bottom wastewater solution is collected for subsequent COD analysis.

[0028] The analysis method of diosgenin is as follows: Dilute the above-mentioned diosgenin extract dissolved in constant volume in methanol to a certain number of times, filter it with a 0.22 μm filter membrane, collect it into a 1 mL sample bottle, and prepare a sample for later use. The saponin stand...

Embodiment 2

[0031] This example examines the influence of temperature on the yield of saponin in the ternary two-phase system. Accurately weigh 5.0g Dioscorea chrysanthemum powder and put it into a 300mL Parr reactor, then add 80mL 5.0g / L AlCl 3 The ternary biphasic solution composed of aqueous solution, 75mL ethanol and 100mL petroleum ether is stirred evenly, and the rotation speed of the reaction kettle is set to 150rpm. , 170°C, 180°C) and start timing, the reaction time is 2.0h. After the end, the diosgenin extract in the petroleum ether organic phase was rotary evaporated, concentrated, crystallized, and dissolved in chromatographic grade methanol for sample preparation. According to the method analyzed in Example 1, the yield of diosgenin from chrysanthemum leaf is calculated, and the effect of temperature on AlCl in the ternary two-phase system is investigated. 3 Influence of extraction yield of saponin. The results are shown in Table 1:

[0032] Table 1

[0033]

[0034] ...

Embodiment 3

[0036] This example examines the influence of extraction time on the yield of saponin in the ternary two-phase system. Accurately weigh 5.0g Dioscorea chrysanthemum powder and put it into a 300mL Parr reactor, then add 80mL 5.0g / L AlCl 3 The ternary biphasic solution composed of aqueous solution, 75mL ethanol and 100mL petroleum ether was stirred evenly, and the reaction kettle was set at a rotation speed of 150rpm, and reacted respectively at an extraction temperature of 150°C (0.5h, 1.0h, 1.5h, 2.0h, 2.5h, 3.0h). After the end, the diosgenin extract in the petroleum ether organic phase was rotary evaporated, concentrated, crystallized, and dissolved in chromatographic grade methanol for sample preparation. According to the method analyzed in Example 1, the yield of diosgenin from chrysanthemum leaf is calculated, and the effect of reaction time on AlCl in the ternary two-phase system is investigated. 3 Influence of extraction yield of saponin. The results are shown in Tab...

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Abstract

The invention discloses a method for preparing diosgenin by hydrolysis of ternary two-phase AlCl3. The method comprises the following steps: putting dried dioscorea powder into a reaction kettle, adding a ternary two-phase solution consisting of an aluminum trichloride aqueous solution, ethanol and petroleum ether, carrying out homogenizing, carrying out reacting for 0.5-3.0 hours at 130-180 DEG C, filtering the reaction solution, filtering out residues, separating out a petroleum ether layer, carrying out rotary evaporation, and carrying out recrystallizing to obtain the diosgenin. Accordingto the method for preparing diosgenin by acidolysis of non-traditional acid AlCl3 in the ternary two-phase system, the yield of diosgenin is improved, the extraction period is shortened, and meanwhile, the usage amount of the consumed acid is greatly reduced. More importantly, under a condition that concentrated sulfuric acid is not used, pollution to the environment is minimized, and the method has a large application prospect.

Description

technical field [0001] The invention relates to the technical field of plant extraction, in particular to extracting saponin from yam resources, and more specifically to a ternary two-phase AlCl 3 A method for preparing diosgenin by hydrolysis. Background technique [0002] Steroid hormone drugs are the second largest drug category in the world after antibiotics, and diosgenin is similar in structure to steroid hormone drugs, and is the most ideal precursor for the synthesis of steroid hormone drugs. There are as many as hundreds of three steroid hormone drugs synthesized from diosgenin, adrenocortical hormone, sex hormone and anabolic hormone. Therefore, the research and production of saponin extracted from yam resources has good market prospect and development value. [0003] Diosgenin is combined with different types and numbers of sugars through glycosidic bonds to form different diosgenins. Therefore, the hydrolysis of diosgenin is the key to extract and prepare diosg...

Claims

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Application Information

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IPC IPC(8): C07J71/00
CPCC07J71/0005
Inventor 谢君张帅帅毕桂灿
Owner SOUTH CHINA AGRI UNIV
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