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Method for preparing diosgenin by hydrolysis of ternary two-phase aluminum chloride

A technology of aluminum trichloride and diosgenin, applied in organic chemistry, steroidal compounds, etc., can solve the problems of complex process and mechanism, low yield of saponin, and many by-products, shorten the extraction cycle, improve the quality of soap Effect of reduction in yield and acid consumption

Active Publication Date: 2022-04-29
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 aluminum chloride
  • Method for preparing diosgenin by hydrolysis of ternary two-phase aluminum chloride
  • Method for preparing diosgenin by hydrolysis of ternary two-phase aluminum chloride

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 ternary two-phase AlCl 3 The method of preparing diosgenin by hydrolysis, put the dried dioscin powder into the reaction kettle, then add the ternary biphasic solution composed of aluminum trichloride aqueous solution, ethanol and petroleum ether, evenly, react at 130-180°C for 0.5 ~3.0h, the reaction solution was filtered, the residue was filtered off, the petroleum ether layer was separated and rotary evaporated, and diosgenin was obtained after recrystallization. The present invention adopts the Lewis acid AlCl of non-traditional acid 3 The preparation of diosgenin from chrysanthemum leaf by acid hydrolysis in the ternary two-phase system not only improves the yield of saponin, shortens the extraction period, but also greatly reduces the amount of acid consumed. More importantly, without using concentrated sulfuric acid, The pollution to the environment will also become minimal, and it has great application prospects.

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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Patent Type & Authority Patents(China)
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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