CN107936083A - A kind of purification process that tigogenin is extracted from sisal dregs - Google Patents
A kind of purification process that tigogenin is extracted from sisal dregs Download PDFInfo
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- CN107936083A CN107936083A CN201711254991.6A CN201711254991A CN107936083A CN 107936083 A CN107936083 A CN 107936083A CN 201711254991 A CN201711254991 A CN 201711254991A CN 107936083 A CN107936083 A CN 107936083A
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- CN
- China
- Prior art keywords
- tigogenin
- extracted
- hexamethylene
- purification process
- sisal dregs
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J71/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton is condensed with a heterocyclic ring
- C07J71/0005—Oxygen-containing hetero ring
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of purification process that tigogenin is extracted from sisal dregs, is the tigogenin crude product that will be extracted from sisal dregs, is recrystallized with hexamethylene and alcohol mixed solvent, centrifuges, obtains tigogenin sterling.The present invention changes traditional method recrystallized with modes such as ethanol, and uses hexamethylene and alcohol mixed solvent to recrystallize, and product purity can reach more than 93%.
Description
Technical field
The present invention relates to tigogenin, more particularly to a kind of purification process that tigogenin is extracted from sisal dregs.
Background technology
Tigogenin, also referred to as Tigogenin, sisalagenin etc., are the base stocks of synthesizing steroid hormone medicine, plain
There are " medical gold " and the title of " hormone is female ".The downstream product monoene produced using tigogenin, can synthesize his rice again
More than the 120 kinds of hormone medicines such as pine.Tigogenin is also widely used for the industries such as food, cosmetics and animal husbandry, is biological doctor
Medicine chemical field is most universal, most important basic material.It is more universal using sisal dregs extraction tigogenin.But the prior art
Mostly isolated and purified with ethyl alcohol recrystallization, generally require three times more than recrystallize, but product purity be extremely difficult to 90% with
On.As disclosed in Chinese patent " a kind of method for extraction tigogenin of squeezing the juice from sisal dregs "（CN103087143A）, it is purified
Tigogenin in thick saponin is extracted using hot ethanol, filtering, through being concentrated in vacuo, standing, is collected by centrifugation saponin crystal, heated
Tigogenin finished product is obtained after drying.Its tigogenin extracted has good quality, less energy consumption, technique is simple, the rate of recovery is high, section
Can be environmentally friendly the advantages that, but do not refer to product purity is how many.
The content of the invention
It is an object of the invention to provide a kind of purification process that tigogenin is extracted from sisal dregs, it can be effectively improved
Product purity.
Embodiment of the present invention is：A kind of purification process that tigogenin is extracted from sisal dregs, is by from sisal dregs
The tigogenin crude product of middle extraction, is recrystallized with hexamethylene and alcohol mixed solvent, is centrifuged, is obtained tigogenin sterling.
Embodiment as an optimization, the matter of tigogenin crude product and hexamethylene and alcohol mixed solvent during the recrystallization
Amount proportioning is 1:8~12；More optimize, tigogenin crude product is 1 with the quality proportioning of hexamethylene and alcohol mixed solvent:
1。
Embodiment as an optimization, the temperature of the recrystallization is 70-80 DEG C.The temperature of the recrystallization more optimized is
75℃。
Embodiment as an optimization, the quality proportioning of the hexamethylene and ethanol is 1：0.5~1.5.More optimize
It is that the quality proportioning of the hexamethylene and ethanol is 1：1.
The present invention changes traditional method recrystallized with modes such as ethanol, and uses hexamethylene and ethanol to mix
Solvent recrystallization, product purity can reach more than 93%.
Embodiment
The embodiment of the present invention is given below, the present invention will be described in detail.
Embodiment 1：A kind of extraction of tigogenin and purification process, specific method and step are as follows：
（1）The sisal dregs for removing fiber are added into water, are fermented 10~20 days, it is dry；
（2）Dry sisal dregs are put into concentration as in 15~25% aqueous hydrochloric acid solutions, with being steam heated to temperature 150~200
DEG C, and in 2.5~3.5kg/cm2When hydrolysis 2.5~3.5 is small under pressure；
（3）Press filtration, filter residue add lime calcification, then press filtration, filter residue are dried, obtains hydrolysate；
（4）It is 95% alcohol steep by hydrolysate purity, 60~100 DEG C, 50~80min of time of extraction temperature, feed liquid weight ratio
1:15~25；
（5）Leaching liquor is concentrated into postcooling to room temperature, crystal centrifugation is dried, obtains tigogenin crude product；
（6）By tigogenin crude product hexamethylene and alcohol mixed solvent recrystallization purification, centrifuge, it is pure to obtain tigogenin
Product.75 DEG C of recrystallization temperature, tigogenin crude product are 1 with the quality proportioning of hexamethylene and alcohol mixed solvent:10, hexamethylene and
The quality proportioning of ethanol is 1：1.Second alcohol concentration≤95% used.
Tigogenin product purity 95.16% obtained by the above method.
Embodiment 2：A kind of tigogenin purification process, by 1 step of embodiment（5）The tigogenin crude product hexamethylene of gained
Alkane and alcohol mixed solvent recrystallization purification, centrifuge, obtain tigogenin sterling.80 DEG C of recrystallization temperature, tigogenin is thick
Product are 1 with the quality proportioning of hexamethylene and alcohol mixed solvent:8, the quality proportioning of hexamethylene and ethanol is 1：0.5.
Tigogenin product purity 93.08% obtained by the above method.
Embodiment 3：A kind of tigogenin purification process, by 1 step of embodiment（5）The tigogenin crude product hexamethylene of gained
Alkane and alcohol mixed solvent recrystallization purification, centrifuge, obtain tigogenin sterling.Recrystallization temperature:70 DEG C, tigogenin is thick
Product are 1 with the quality proportioning of hexamethylene and alcohol mixed solvent:12, the quality proportioning of hexamethylene and ethanol is 1：1.5.
Tigogenin product purity 93.32% obtained by the above method.
Embodiment 4：A kind of tigogenin purification process, by 1 step of embodiment（5）The tigogenin crude product ethanol of gained
Recrystallization purification, centrifuges, obtains tigogenin sterling.75 DEG C of recrystallization temperature, tigogenin crude product and ethanol quality proportioning
For 1:10, second alcohol concentration≤95%.
Tigogenin product purity 89.86% obtained by the above method.
From above-described embodiment as can be seen that the present invention is recrystallized using hexamethylene and alcohol mixed solution, product is pure
Degree can reach more than 93%, and be recrystallized using ethanol under the conditions of same as Example 1, and product purity is only
89.86%.In addition, the proportioning and hexamethylene and second of recrystallization temperature, tigogenin crude product and hexamethylene and alcohol mixed solvent
The proportioning of alcohol all has a direct impact product purity.Find out from embodiment 1-3, the product purity highest of embodiment 1, reaches
95.16%.Therefore, the technical parameter of embodiment 1 is the embodiment optimized the most, is preferred solution.
Claims (7)
- A kind of 1. purification process that tigogenin is extracted from sisal dregs, it is characterised in that the sisal hemp that will be extracted from sisal dregs Saponin crude product, is recrystallized with hexamethylene and alcohol mixed solvent, is centrifuged, is obtained tigogenin sterling.
- 2. the purification process according to claim 1 that tigogenin is extracted from sisal dregs, it is characterised in that the heavy knot Tigogenin crude product is with being 1 with the quality proportioning of hexamethylene and alcohol mixed solvent when brilliant:8~12.
- 3. the purification process according to claim 1 or 2 that tigogenin is extracted from sisal dregs, it is characterised in that sisal hemp Saponin crude product is with being 1 with the quality proportioning of hexamethylene and alcohol mixed solvent:1.
- 4. the purification process according to claim 1 that tigogenin is extracted from sisal dregs, it is characterised in that the heavy knot Brilliant temperature is 70~80 DEG C.
- 5. the purification process of tigogenin is extracted in the slave sisal dregs according to claim 1 or 4, it is characterised in that described The temperature of recrystallization is 75 DEG C.
- 6. the purification process according to claim 1 that tigogenin is extracted from sisal dregs, it is characterised in that the hexamethylene The quality proportioning of alkane and ethanol is 1：0.5~1.5.
- 7. the purification process of tigogenin is extracted from sisal dregs according to claim 1 or 5, it is characterised in that described The quality proportioning of hexamethylene and ethanol is 1：1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711254991.6A CN107936083A (en) | 2017-12-02 | 2017-12-02 | A kind of purification process that tigogenin is extracted from sisal dregs |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711254991.6A CN107936083A (en) | 2017-12-02 | 2017-12-02 | A kind of purification process that tigogenin is extracted from sisal dregs |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107936083A true CN107936083A (en) | 2018-04-20 |
Family
ID=61947511
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711254991.6A Pending CN107936083A (en) | 2017-12-02 | 2017-12-02 | A kind of purification process that tigogenin is extracted from sisal dregs |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109293731A (en) * | 2018-11-22 | 2019-02-01 | 莫伟文 | A kind of preparation method of safe synthetic reaction sisal hemp saponin(e methylation product |
| CN110590900A (en) * | 2019-09-29 | 2019-12-20 | 石门红太阳生物科技有限公司 | Dewaxing method in sisal hemp saponin production |
-
2017
- 2017-12-02 CN CN201711254991.6A patent/CN107936083A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109293731A (en) * | 2018-11-22 | 2019-02-01 | 莫伟文 | A kind of preparation method of safe synthetic reaction sisal hemp saponin(e methylation product |
| CN110590900A (en) * | 2019-09-29 | 2019-12-20 | 石门红太阳生物科技有限公司 | Dewaxing method in sisal hemp saponin production |
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Legal Events
| Date | Code | Title | Description |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180420 |
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| WD01 | Invention patent application deemed withdrawn after publication |