CN104592324B - Gastrodin extraction and purification method - Google Patents
Gastrodin extraction and purification method Download PDFInfo
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- CN104592324B CN104592324B CN201510060466.5A CN201510060466A CN104592324B CN 104592324 B CN104592324 B CN 104592324B CN 201510060466 A CN201510060466 A CN 201510060466A CN 104592324 B CN104592324 B CN 104592324B
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- gastrodine
- extraction
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- ethanol
- ultrasonic atomization
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/203—Monocyclic carbocyclic rings other than cyclohexane rings; Bicyclic carbocyclic ring systems
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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Abstract
The invention relates to a gastrodin extraction and purification method, which obtains a pure gastrodin product through crushing treatment, ultrasonic atomization extraction, silica gel column adsorption elution and recrystallization, has mild overall process conditions and higher product yield, meets the control requirements of industrial production, and is beneficial to the actual operation of large-scale production.
Description
Technical field
The present invention relates to a kind of production method of gastrodine, and in particular to isolating and purifying for gastrodine is extracted in a kind of Rhizoma Gastrodiae
Method.
Background technology
Rhizoma Gastrodiae, is ground in the medicinal history that China has had more than 2,000 years at present both at home and abroad as a kind of famous and precious Chinese crude drug
Study carefully discovery, Rhizoma Gastrodiae main component gastrodine can be treated pain dizziness, numb limbs and tense tendons, frightened pain and be twitched, and clinically primary treatment is moved
Arteries and veins blood supply insufficiency, vestibular neuronitis, vertigo, coronary heart disease etc..
The traditional handicraft for extracting gastrodine at present mainly has：Alcohol extracting method, microwave loss mechanisms, ultrasonic extraction, enzyme extraction
And supercritical extraction etc..In prior art, the common problem paste-forming rate that predominantly gastrodine is extracted is relatively low, and product is produced
Go out content relatively low, while Processes and apparatus condition is complex, be unfavorable for amplifying the operation of production and the control of cost.Other one
Point be exactly gastrodine purification in terms of at present the resin column method of employing, adverse current extraction method etc..Use while product yield is relatively low
Organic solvent is complex, relatively costly.Liu Dongfeng et al. invention " a kind of method of purification of gastrodine " by supersound extraction,
The sterling yield 0.82 ~ 1.00% of the gastrodine that resin, silica column purification are finally obtained.
Ultrasonic atomization abstraction technique is that ultrasound wave is directly or indirectly acted on the solution containing dusty raw materials, one
" ultrasonic fountain " effect and aerosol are produced under fixed ultrasound condition, aerosol is wrapped in feed particles and does under this effect
Lower reciprocating motion, due to rupture of membranes effect caused by cavitation effect, the cost-effectively of raw material is dissolved, quilt when with aerosol exposure
Dissolving, and fallen back in liquid phase under gravity, reach good volume effect of extracting.
The content of the invention
To solve the problems, such as current production technology, the invention provides a kind of method for extraction and purification of gastrodine, the method will
Rhizoma Gastrodiae raw material is extracted by ultrasonic atomization after crushed, draws product extractum, is then separated and is recrystallized to give through silica gel
Gastrodine sterling.Integrated artistic mild condition, product yield are higher, meet industrial control and require, are conducive to big production
Practical operation.
The invention provides a kind of method for extraction and purification of gastrodine, comprises the steps：
（1）Pulverization process；（2）Extraction；（3）Silicagel column absorb-elute；（4）Recrystallization.
Preferably, the step（1）Dry Rhizoma Gastrodiae is crushed to into granularity in pulverization process and crosses 80 mesh sieves.
Preferably, the step（2）Extract and extract for ultrasonic atomization, its concrete steps includes：By the Rhizoma Gastrodiae after crushing
Raw material and ethanol press 1：2 ~ 5 weight ratios are mixed, and are then carried out ultrasonic atomization and are extracted 2 times, obtain day after extract concentration
Numb element extractum.
Preferably, ultrasonic atomization extraction conditionss be 25 ~ 40 DEG C of temperature, 1 ~ 2MHz of frequency, extraction time 20 ~ 40 minutes.
Preferably, the step（3）Silicagel column absorb-elute concrete steps include：By gastrodine extractum with 0.5 times of weight
Ethanol dissolving after loading silicagel column, with 10% ethanol water eluting, 3 ~ 5 times of silicagel column volumes after, change 50% ethanol water into
Eluting, collects fractional crystallization after eluent concentration.
Preferably, the step（4）Recrystallization concrete steps include：The gastrodine crystallization obtained after silicagel column is adsorbed adds
Enter the EtOH-EtOAc dissolving of 1 ~ 1.5 times of amount, wherein ethanol：The volume ratio of ethyl acetate is 1:5, solution temperature 50 ~ 60
DEG C, it is cooled to 20 ~ 25 DEG C and crystallizes 2 ~ 3 hours, separates, is drying to obtain gastrodine sterling.
The present invention is extracted by ultrasonic atomization, and substantially increase raw material extractum draws rate, while passing through silica gel adsorption
Be recrystallized to give gastrodine sterling, extraction time is short, and product yield is high, and technological operation is simple, is suitable for the scale of industry
Production.
Specific embodiment
The detailed content and its specific embodiment of the present invention is further illustrated below.It should be appreciated that described herein
Specific embodiment is only used for explaining the present invention, is not used to limit invention.
Embodiment 1：
A kind of method for extraction and purification of gastrodine, in turn includes the following steps：
（1）Pulverization process：10kg dry Rhizoma Gastrodiae is crushed to into granularity and crosses 80 mesh sieves.
（2）Ultrasonic atomization is extracted：Rhizoma Gastrodiae raw material and ethanol after crushing is pressed into 1：2 weight ratios are mixed, Ran Houjin
Row ultrasonic atomization extract 2 times, extraction conditionss be 25 DEG C of temperature, frequency 1MHZ, extraction time 20 minutes.After extract concentration
To gastrodine extractum 4.75kg.Based on raw material, yield of extract 47.5%.
（3）Silicagel column absorb-elute：By loading silicagel column after ethanol dissolving of the gastrodine extractum with 0.5 times of weight, 10% is used
After 3 times of silicagel column volumes of ethanol water eluting, 50% ethanol water eluting is changed into, collect fractional crystallization after eluent concentration
205g。
（4）Recrystallization：The gastrodine crystallization obtained after silicagel column is adsorbed adds the EtOH-EtOAc dissolving of 1 times of amount
（Volume ratio 1:5）, 50 DEG C of solution temperature, be cooled to 25 DEG C crystallize 2 hours, separate, be drying to obtain gastrodine sterling 157g, Jing
HPLC detection level is 98.4%, gastrodine yield 1.54%.
Embodiment 2：
A kind of method for extraction and purification of gastrodine, in turn includes the following steps：
（1）Pulverization process：10kg dry Rhizoma Gastrodiae is crushed to into granularity and crosses 80 mesh sieves.
（2）Ultrasonic atomization is extracted：Rhizoma Gastrodiae raw material and ethanol after crushing is pressed into 1：5 weight ratios are mixed, Ran Houjin
Row ultrasonic atomization extract 2 times, extraction conditionss be 40 DEG C of temperature, frequency 2MHZ, extraction time 40 minutes.After extract concentration
To gastrodine extractum 5.42kg.Based on raw material, yield of extract 54.2%.
（3）Silicagel column absorb-elute：By loading silicagel column after ethanol dissolving of the gastrodine extractum with 0.5 times of weight, 10% is used
After 5 times of silicagel column volumes of ethanol water eluting, 50% ethanol water eluting is changed into, collect fractional crystallization after eluent concentration
243g。
（4）Recrystallization：The gastrodine crystallization obtained after silicagel column is adsorbed adds the EtOH-EtOAc of 1.5 times of amounts molten
Solution（Volume ratio 1:5）, 60 DEG C of solution temperature, be cooled to 20 DEG C crystallize 3 hours, separate, be drying to obtain gastrodine sterling 174g, Jing
HPLC detection level is 97.3%, gastrodine yield 1.69%.
Embodiment 3：
A kind of method for extraction and purification of gastrodine, in turn includes the following steps：
（1）Pulverization process：10kg dry Rhizoma Gastrodiae is crushed to into granularity and crosses 80 mesh sieves.
（2）Ultrasonic atomization is extracted：Rhizoma Gastrodiae raw material and ethanol after crushing is pressed into 1：3 weight ratios are mixed, Ran Houjin
Row ultrasonic atomization extract 2 times, extraction conditionss be 35 DEG C of temperature, frequency 1.4MHZ, extraction time 25 minutes.After extract concentration
Obtain gastrodine extractum 5.16kg.Based on raw material, yield of extract 51.6%.
（3）Silicagel column absorb-elute：By loading silicagel column after ethanol dissolving of the gastrodine extractum with 0.5 times of weight, 10% is used
After 4 times of silicagel column volumes of ethanol water eluting, 50% ethanol water eluting is changed into, collect fractional crystallization after eluent concentration
221g。
（4）Recrystallization：The gastrodine crystallization obtained after silicagel column is adsorbed adds the EtOH-EtOAc of 1.3 times of amounts molten
Solution（Volume ratio 1:5）, 52 DEG C of solution temperature, be cooled to 23 DEG C crystallize 3 hours, separate, be drying to obtain gastrodine sterling 175g, Jing
HPLC detection level is 99.2%, gastrodine yield 1.74%.
By present invention process method, the gastrodine product yield raising more than 50% in Rhizoma Gastrodiae can be made.Effectively improve
Product income, is suitable for the large-scale production of industry.
Claims (1)
1. a kind of method for extraction and purification of gastrodine, it is characterised in that：Comprise the steps：
(1) pulverization process；(2) extract；(3) silicagel column absorb-elute；(4) recrystallization；
Dry Rhizoma Gastrodiae is crushed to into granularity in step (1) pulverization process and crosses 80 mesh sieves；
Step (2) extraction is extracted for ultrasonic atomization, and its concrete steps includes：Rhizoma Gastrodiae raw material and ethanol after crushing is pressed
1：2～5 weight ratios are mixed, and are then carried out ultrasonic atomization and are extracted 2 times, and ultrasonic atomization extraction conditionss are temperature 25～40
DEG C, 1～2MHz of frequency, extraction time 20～40 minutes obtain gastrodine extractum after extract concentration；
Step (3) the silicagel column absorb-elute concrete steps include：After ethanol dissolving of the gastrodine extractum with 0.5 times of weight
Loading silicagel column, with 10% ethanol water eluting, 3～5 times of silicagel column volumes after, change 50% ethanol water eluting into, collect
Fractional crystallization after eluent concentration；
Step (4) the recrystallization concrete steps include：The gastrodine crystallization obtained after silicagel column is adsorbed adds 1～1.5 times
The EtOH-EtOAc dissolving of amount, wherein ethanol：The volume ratio of ethyl acetate is 1:5,50～60 DEG C of solution temperature is cooled to
20～25 DEG C crystallize 2～3 hours, separate, be drying to obtain gastrodine sterling.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105111258A (en) * | 2015-09-23 | 2015-12-02 | 成都艾比科生物科技有限公司 | Preparation method for extracting gastrodine from gastrodia elata |
| CN106496355B (en) * | 2016-11-07 | 2018-11-20 | 涟源康麓生物科技有限公司 | A kind of preparation method of pectin |
| CN106954840A (en) * | 2017-03-27 | 2017-07-18 | 湖北文理学院 | A kind of gingerol compound stabilizer containing Rhizoma Gastrodiae extract |
| CN108409808B (en) * | 2018-05-31 | 2021-04-06 | 中山大学 | Method for continuously extracting gastrodin from gastrodia elata through low-temperature high-pressure crushing |
| CN110845553A (en) * | 2019-11-25 | 2020-02-28 | 湖南省博世康中医药有限公司 | Method for extracting gastrodin by ultrasonic water bath heating |
| CN114573647A (en) * | 2020-11-30 | 2022-06-03 | 昆药集团股份有限公司 | Gastrodin anhydrous crystal form and preparation method thereof |
| CN114573649A (en) * | 2020-11-30 | 2022-06-03 | 昆药集团股份有限公司 | High-purity gastrodin crystal and preparation method and application thereof |
| CN114685576A (en) * | 2020-12-29 | 2022-07-01 | 昆药集团股份有限公司 | High-purity gastrodin unstable crystal form, preparation method thereof and preparation method of gastrodin crystal form FormA |
| CN114685575A (en) * | 2020-12-29 | 2022-07-01 | 昆药集团股份有限公司 | Gastrodin anhydrous crystal form and preparation method thereof |
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| CN101704855A (en) * | 2009-10-20 | 2010-05-12 | 南京荣世医药科技有限公司 | Method for preparing gastrodine |
| CN102250164A (en) * | 2011-08-09 | 2011-11-23 | 南京泽朗医药科技有限公司 | Purification method of gastrodin |
| CN104262424B (en) * | 2014-10-17 | 2016-04-13 | 神农架绿野食品开发有限责任公司 | The extracting method of Gastrodine |
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