CN105712872A - Process for extracting 10-hydroxy-2-decenoic acid from royal jelly waste - Google Patents
Process for extracting 10-hydroxy-2-decenoic acid from royal jelly waste Download PDFInfo
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- CN105712872A CN105712872A CN201410730602.2A CN201410730602A CN105712872A CN 105712872 A CN105712872 A CN 105712872A CN 201410730602 A CN201410730602 A CN 201410730602A CN 105712872 A CN105712872 A CN 105712872A
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- decenoic acid
- decylenic acid
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Abstract
The invention discloses a process method for extracting 10-hydroxy-2-decenoic acid from royal jelly waste, wherein the process method comprises the following steps: (1) mixing the royal jelly waste with 95% edible alcohol according to the weight ratio of 1 to (8-10), adding the mixture into a reaction kettle, carrying out heating reflux for 40 minutes, then filtering while being hot, adding edible alcohol into the royal jelly waste, repeatedly extracting for 2-3 times, filtering, merging the filtrates, and carrying out reduced pressure recycling of ethyl alcohol; (2) concentrating the filtrate to 7-8 L, adding distilled water, heating to be transparent with steam, carrying out static filtration, washing the obtained crystal for three times with distilled water, and drying at the temperature of 50 DEG C, to obtain a crude product; and (3) adding a 50% methanol aqueous solution with the volume two times that of the crude product into the crude product, and recrystallizing for 3-4 times to obtain a 10-hydroxy-2-decenoic acid refined product. The process is simple, the cost is low, the 10-hydroxy-2-decenoic acid is extracted from the royal jelly waste, the maximum utilization rate of resources is achieved, the purity of the obtained 10-hydroxy-2-decenoic acid refined product reaches more than or equal to 99%, and the 10-hydroxy-2-decenoic acid can be used for production of antibacterial, anti-cancer and anti-radiation drugs.
Description
Technical field
The present invention relates to the preparation method technical field of E-10-hydroxy-2-decylenic acid, specifically a kind of process extracting E-10-hydroxy-2-decylenic acid from royal jelly slag.
Background technology
E-10-hydroxy-2-decylenic acid has pharmacological action widely, its energy enhancing body resistance to physical property, chemical and biological paathogenic factor, the immunologic function of enhancing body, promote that tissue is another to repair, adjust E&M function, improve the function of important organ, there are antibacterial and Inhibition test tumor growth etc..E-10-hydroxy-2-decylenic acid is fine as health food development future, and can increasingly be subject to people's attention, it may be said that its healthy lifespring that provides to the mankind, all too is important.The lack of standard clinical observation so far from 9 years, to renal failure, cholecystitis, diabetes, hyperlipemia, Senile disease, climacteric disfunction, immunologic hypofunction, promotes that children growth raw intelligence and dysplasia etc. truly have good effect.
Current E-10-hydroxy-2-decylenic acid is typically all and extracts from Lac regis apis.Extracting method Secondary Organic solvent extraction, secondary adjusts pH, by high performance liquid chromatography, 10-HDA is carried out qualitative analysis, the best extracting method generally acknowledged at present is that Lac regis apis aqueous solution pH is adjusted to 10, adds ether extraction impurity, then adjusts pH2 to add ether extraction 10-HAD, but this kind of method is to be made directly extraction with Lac regis apis, with high costs, complex process, it is unfavorable for large-scale promotion application and reduces E-10-hydroxy-2-decylenic acid cost.Royal jelly slag after at present extracting Lac regis apis is generally used as garbage and directly processes, serious waste resource, therefore, researches and develops a kind of process extracting E-10-hydroxy-2-decylenic acid from royal jelly slag, reaches maximally utilizing of resource very necessary.
Summary of the invention
Present invention aim to solve current E-10-hydroxy-2-decylenic acid is all extracting directly from Lac regis apis, and extraction process is complicated, with high costs, is unfavorable for the problem that the industrialization of E-10-hydroxy-2-decylenic acid uses, it is provided that a kind of process extracting E-10-hydroxy-2-decylenic acid from royal jelly slag.
A kind of process extracting E-10-hydroxy-2-decylenic acid from royal jelly slag of the present invention, comprises the following steps:
(1) edible ethanol of royal jelly slag and 95% is mixed by weight the ratio for 1:8-10, add in reactor, be heated to reflux 40 minutes, filtered while hot, then in royal jelly slag, add the edible ethanol of royal jelly slag weight 4-5 times, repeat to extract 2-3 time, filter, merge each filtrate, recovered under reduced pressure ethanol；
(2) concentrate the filtrate to 7-8L, add distilled water, with steam (or water-bath) heating to transparent, stands 10-12 hour, filter, obtain E-10-hydroxy-2-decylenic acid crystal, with distilled water wash three times, then drying at 50 DEG C, obtain crude product；
(3) crude product that step (2) prepares adds 50% methanol aqueous solution of two volumes, and recrystallization obtains E-10-hydroxy-2-decylenic acid fine work, E-10-hydroxy-2-decylenic acid content >=99% in this E-10-hydroxy-2-decylenic acid fine work 3-4 time.
Extracting, by the inventive method, the E-10-hydroxy-2-decylenic acid fine work that obtains with low cost, preparation technology is simple, and has reached the resource peak use rate of Lac regis apis pharmacy, it is to avoid the wasting of resources, develops condition of providing convenience further for E-10-hydroxy-2-decylenic acid simultaneously.
Detailed description of the invention
Embodiment 1
A kind of process extracting E-10-hydroxy-2-decylenic acid from royal jelly slag of the present embodiment, comprises the following steps:
(1) edible ethanol of royal jelly slag and 95% is mixed by weight the ratio for 1:9, add in reactor, be heated to reflux 40 minutes, filtered while hot, then in royal jelly slag, add the edible ethanol of royal jelly slag weight 5 times, repeat to extract 3 times, filter, merge 4 filtrates, recovered under reduced pressure ethanol；
(2) concentrate the filtrate to 7L, add distilled water, with steam (or water-bath) heating to transparent, stands 10 hours, filter, obtain E-10-hydroxy-2-decylenic acid crystal, with distilled water wash three times, then drying at 50 DEG C, obtain crude product；
(3) crude product that step (2) prepares adds 50% methanol aqueous solution of two volumes, and recrystallization obtains E-10-hydroxy-2-decylenic acid fine work, E-10-hydroxy-2-decylenic acid content >=99% in this E-10-hydroxy-2-decylenic acid fine work 4 times.
Claims (1)
1. the process extracting E-10-hydroxy-2-decylenic acid from royal jelly slag, it is characterised in that comprise the following steps:
(1) edible ethanol of royal jelly slag and 95% is mixed by weight the ratio for 1:8-10, add in reactor, be heated to reflux 40 minutes, filtered while hot, then in royal jelly slag, add the edible ethanol of royal jelly slag weight 4-5 times, repeat to extract 2-3 time, filter, merge each filtrate, recovered under reduced pressure ethanol；
(2) concentrate the filtrate to 7-8L, add distilled water, with steam (or water-bath) heating to transparent, stands 10-12 hour, filter, obtain E-10-hydroxy-2-decylenic acid crystal, with distilled water wash three times, then drying at 50 DEG C, obtain crude product；
(3) crude product that step (2) prepares adds 50% methanol aqueous solution of two volumes, and recrystallization obtains E-10-hydroxy-2-decylenic acid fine work, E-10-hydroxy-2-decylenic acid content >=99% in this E-10-hydroxy-2-decylenic acid fine work 3-4 time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410730602.2A CN105712872A (en) | 2014-12-05 | 2014-12-05 | Process for extracting 10-hydroxy-2-decenoic acid from royal jelly waste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410730602.2A CN105712872A (en) | 2014-12-05 | 2014-12-05 | Process for extracting 10-hydroxy-2-decenoic acid from royal jelly waste |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105712872A true CN105712872A (en) | 2016-06-29 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410730602.2A Pending CN105712872A (en) | 2014-12-05 | 2014-12-05 | Process for extracting 10-hydroxy-2-decenoic acid from royal jelly waste |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106929231A (en) * | 2017-03-08 | 2017-07-07 | 蔡颖欣 | A kind of transparent amino acid crystal soap of Cinnamomum kanahirai hay and preparation method thereof |
| CN113575898A (en) * | 2021-08-11 | 2021-11-02 | 杭州碧于天保健品有限公司 | Method for removing foreign matters in royal jelly slurry residue based on crystallization technology |
-
2014
- 2014-12-05 CN CN201410730602.2A patent/CN105712872A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106929231A (en) * | 2017-03-08 | 2017-07-07 | 蔡颖欣 | A kind of transparent amino acid crystal soap of Cinnamomum kanahirai hay and preparation method thereof |
| CN113575898A (en) * | 2021-08-11 | 2021-11-02 | 杭州碧于天保健品有限公司 | Method for removing foreign matters in royal jelly slurry residue based on crystallization technology |
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160629 |
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| WD01 | Invention patent application deemed withdrawn after publication |