CN105131052B - A kind of extracting method of crocin I - Google Patents
A kind of extracting method of crocin I Download PDFInfo
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- CN105131052B CN105131052B CN201510442096.1A CN201510442096A CN105131052B CN 105131052 B CN105131052 B CN 105131052B CN 201510442096 A CN201510442096 A CN 201510442096A CN 105131052 B CN105131052 B CN 105131052B
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Abstract
The present invention relates to medical separation and technical field of purification, more particularly to a kind of extracting method of crocin I.The extracting method includes：The medicinal part of the plant of the I containing crocin is subjected to alcohol extracting, extracting solution is made；Extracting solution obtains the first intermediate product through adsorbing separation；First intermediate product is purified using medium pressure chromatography system, obtains the second intermediate product；The chromatography agent of medium pressure chromatography system is polystyrene family macromolecule macroporous type polymeric material, and mobile phase is ethanol water；Second intermediate product is crystallized, obtains crocin I.Using extracting method provided by the invention can obtain high-purity, High color values crocin I crystal, purity is up to more than 95%, and color value is up to more than 950.
Description
Technical field
The present invention relates to medical separation and technical field of purification, more particularly to a kind of extracting method of crocin I.
Background technology
Crocin is the main pharmacodynamics component of Chinese medicine west safflower, is the sugar that crocetin is combined into different sugar base
Ester, mainly there is crocin I and crocin II.Crocin I and crocin II contents point in the west safflower of different sources
Not between 4.6%~11.0% and 1.1%~4.5%.Crocins compound has extensive pharmacological activity, such as reducing blood lipid
Effect, antioxidation activity, myocardial damage reparation etc., have preferable application prospect.West safflower is a kind of very expensive spices,
Its price has the title of " plant gold " about in 2000~4000 dollars/kg in the international market.International market about 70% at present
West safflower originate from Iran, also there are a large amount of plantations in other European countries.China is since nineteen sixty-five introduces a fine variety, successively in Shanghai, north
Capital, Jiangsu, zhejiang and other places successful introduction, and reach a certain scale, but yield is far from meeting medicinal demand.It is although western red
Spend it is not high to environmental requirement, but due to its yield is relatively low and investment it is larger, the Planting risk of west safflower is improved indirectly, in
State does not realize that industrialization is planted.Country's west safflower yield only accounts for 20% of demand or so at present, still needs to a large amount of imports every year
To fill up domestic demand.These factors seriously constrain the industry demand that separation crocin is extracted using west safflower as raw material.
Cape jasmine is the dry fruit of madder wort cape jasmine.Research shows that different cultivars, the cape jasmine Chinese and Western of different sources are red
The content of flower glycosides I is between 0.43%~1.2%.Moreover, cape jasmine yield is high, fresh fruit per mu yield is met up to 500~1000kg
Crocin extracts separated resource requirement, and the price of cape jasmine fruit is far below the price of west safflower again.Therefore carried from cape jasmine
Take crocin has significant practical significance to substitute west safflower.
Pigment part is mainly crocin class material in cape jasmine fruit, includes the degradation product of crocin class, the constituents
Middle crocin I accounts for main body, the accounting very little such as crocin II, III and crocetin.Crocin I is compared to other west
Carthamic acid component and crocetin, the water-soluble bigger of glycosides I, are highly soluble in water, and application operating is more convenient, the base in National Pharmacopeia
This is using crocin I as labeled component.
The prior art mainly adopts the method for macroporous absorbent resin absorption, the parsing of various concentrations alcohol gradient, or using silicon
The method of glue-line analysis continues to separate the different component of crocin.However, since crocin I hydrophilies are strong, compared to other
Component is more difficult to obtain high-purity crystals, and product purity known to related data and document known today and market exists mostly
50% or so, several crocin component mixabilities are larger, and color value is also substantially below 600.Therefore it is badly in need of providing a kind of pure
The extracting method of degree and the higher cape jasmine crocin I of color range.
The content of the invention
In view of this, the present invention provides a kind of extracting method of crocin I.Using extracting method provided by the invention
High-purity, the crocin I crystal of High color values can be obtained, purity is up to more than 95%, and color value is up to more than 950.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
The present invention provides a kind of extracting method of crocin I, include the following steps：
The plant medicinal part of the I containing crocin is subjected to alcohol extracting, extracting solution is made；
Extracting solution obtains the first intermediate product through adsorbing separation；
First intermediate product is purified using medium pressure chromatography system, obtains the second intermediate product；Medium pressure chromatography system
Chromatography agent is polystyrene family macromolecule macroporous type polymeric material, and mobile phase is ethanol water；
Second intermediate product is crystallized, obtains crocin I.
Preferably, the volumn concentration of ethanol water is 10%~60%.
Preferably, the volumn concentration of ethanol water is 30%~45%.
In some embodiments provided by the invention, the volumn concentration of ethanol water is 30%.
In other embodiments provided by the invention, the volumn concentration of ethanol water is 45%.
In other embodiments provided by the invention, the volumn concentration of ethanol water is 40%.
Preferably, the flow velocity of mobile phase is 0.2~0.5bv/h.
In some embodiments provided by the invention, the flow velocity of mobile phase is 0.2bv/h.
In other embodiments provided by the invention, the flow velocity of mobile phase is 0.3bv/h.
In other embodiments provided by the invention, the flow velocity of mobile phase is 0.5bv/h.
Preferably, the pressure of medium pressure chromatography system is 0.05~0.1MPa.
In some embodiments provided by the invention, the pressure of medium pressure chromatography system is 0.05MPa.
In other embodiments provided by the invention, the pressure of medium pressure chromatography system is 0.08MPa.
In other embodiments provided by the invention, the pressure of medium pressure chromatography system is 0.1MPa.
Preferably, the temperature of crystallization is -2~15 DEG C, the time is 15~40h.
In some embodiments provided by the invention, the temperature of crystallization is -2 DEG C, time 15h.
In other embodiments provided by the invention, the temperature of crystallization is 10 DEG C, time 30h.
In other embodiments provided by the invention, the temperature of crystallization is 15 DEG C, time 40h.
In some embodiments provided by the invention, the mixing speed of crystallization is 0~20rpm, and the cleaning solvent of crystallization is
Ethanol water.
Preferably, the volumn concentration of cleaning solvent ethanol water is 1%~50%.
Preferably, the volumn concentration of cleaning solvent ethanol water is 25%~50%.
In some embodiments provided by the invention, for temperature control at 0~25 DEG C, the speed of agitator of cleaning is 0 during cleaning
~20rpm, cleans 5~30min.
Preferably, adsorbing separation carries out adsorbing separation using macroporous absorbent resin.
In some embodiments provided by the invention, adsorbing separation carries out absorption point using HPD100 types macroporous absorbent resin
From.Preferably, alcohol extracting is extracted using 60%~70% ethanol water.
Preferably, the temperature of alcohol extracting is 20~30 DEG C, the number of alcohol extracting is 2~4 times.
Preferably, the grain fineness of polystyrene family macromolecule macroporous type polymeric material is 60~300 mesh, porosity is
10%~45%.
Preferably, chromatography agent chromatographs agent for LS-300 types or LS-350 types chromatograph agent.
In some embodiments provided by the invention, the plant of the I containing crocin is cape jasmine, its medicinal part is fruit.
But the raw material that extracting method provided by the invention uses is not limited to cape jasmine, as long as the plant containing crocin I components
Method provided by the invention extraction crocin I can be used.
The present invention provides a kind of extracting method of crocin I.The extracting method includes：By the plant of the I containing crocin
The medicinal part of thing carries out alcohol extracting, and extracting solution is made；Extracting solution obtains the first intermediate product through adsorbing separation；Production among first
Thing is purified using medium pressure chromatography system, obtains the second intermediate product；The chromatography agent of medium pressure chromatography system is polystyrene type
Macromolecule macroporous type polymeric material, mobile phase are ethanol water；Second intermediate product is crystallized, obtains crocin I.
Using extracting method provided by the invention can obtain high-purity, High color values crocin I crystal, purity up to more than 95%,
Color value is up to more than 950.
Brief description of the drawings
Fig. 1 shows the HPLC collection of illustrative plates of crocin I in embodiment 1；
Fig. 2 shows the HPLC collection of illustrative plates of crocin I in embodiment 2；
Fig. 3 shows the HPLC collection of illustrative plates of crocin I in embodiment 3.
Embodiment
The invention discloses a kind of extracting method of crocin I, those skilled in the art can use for reference present disclosure, fit
When modified technique parameter is realized.In particular, all similar substitutions and modifications are for a person skilled in the art
It is it will be apparent that they are considered as being included in the present invention.The present invention method and application by preferred embodiment into
Gone description, related personnel substantially can not depart from present invention, in spirit and scope to method described herein and application
It is modified or suitably changes with combining, realizes and using the technology of the present invention.
Raw materials used, reagent, instrument can be bought by market in the extracting method of crocin I provided by the invention.
With reference to embodiment, the present invention is further explained：
The extraction of 1 crocin I of embodiment
Dried cape jasmine fruit is crushed to 10~20 mesh through rotary vane type pulverizer, the raw material after 100kg crushing is taken, adds
Add 60% ethanol solution, extracted three times under the conditions of 30 DEG C.Vacuum-concentrcted is carried out to feed liquid ethanol after merging extracting solution
Content is less than 2%, and cooling, obtains feed liquid 27Kg.
4.5 times of deionized water dilution feed liquids of addition, filtering, gained filtrate are adsorbed through macroporous absorbent resin HPD100,5 times of trees
The clear water of fat volume rinses resin bed.Parsed with 75% ethanol, gained desorbed solution is less than through being concentrated under reduced pressure into ethanol content
2%, obtain 5kg concentrates.
30% ethanol of gained solution analysis of material concentrate is diluted 2 times, medium pressure chromatography is carried out through the chromatography agent of LS-300 types, with
30% ethanol is mobile phase, flow velocity 0.2bv/h, pressure 0.1MPa.
The part of the I containing crocin is collected, temperature control, mixing speed 10rpm are carried out at -2 DEG C, holding 15 is tied when small
Crystalline substance, crystallization are cleaned using 40% ethanol water, and for temperature control at 25 DEG C, the speed of agitator of cleaning be 20rpm during cleaning, is cleaned
30min.Drying is performed under reduced pressure after collecting crystal, final gained 820g peony crystallographic powder, color value 973,
HPLC detection crocin I contents are 95.7%, and collection of illustrative plates is shown in Fig. 1.
The extraction of 2 crocin I of embodiment
Dried cape jasmine fruit is crushed to 10~20 mesh through rotary vane type pulverizer, the raw material after 100kg crushing is taken, adds
Add 70% ethanol solution, extracted three times under the conditions of 25 DEG C.Vacuum-concentrcted is carried out to feed liquid ethanol after merging extracting solution
Content is less than 2%, and cooling, obtains feed liquid 28Kg.
4.5 times of deionized water dilution feed liquids of addition, filtering, gained filtrate are adsorbed through macroporous absorbent resin HPD300,5 times of trees
The clear water of fat volume rinses resin bed.Parsed with 75% ethanol, gained desorbed solution is less than through being concentrated under reduced pressure into ethanol content
2%, obtain 4.8kg concentrates.
45% ethanol of gained solution analysis of material concentrate is diluted 2 times, medium pressure chromatography is carried out through the chromatography agent of LS-350 types, with
45% ethanol is mobile phase, flow velocity 0.3bv/h, pressure 0.08MPa.
The part of the I containing crocin is collected, temperature control, mixing speed 15rpm are carried out at 10 DEG C, holding 15 is tied when small
Crystalline substance, crystallization are cleaned using 25% ethanol water, and for temperature control at 15 DEG C, the speed of agitator of cleaning be 10rpm during cleaning, is cleaned
20min.Drying is performed under reduced pressure after collecting crystal, final gained 797g peony crystallographic powder, color value 989,
HPLC detection crocin I contents are 96.4%, and collection of illustrative plates is shown in Fig. 2.
The extraction of 3 crocin I of embodiment
Dried cape jasmine fruit is crushed to 10~20 mesh through rotary vane type pulverizer, the raw material after 100kg crushing is taken, adds
Add 65% ethanol solution, extracted three times under the conditions of 20 DEG C.Vacuum-concentrcted is carried out to feed liquid ethanol after merging extracting solution
Content is less than 2%, and cooling, obtains feed liquid 35Kg.
4.5 times of deionized water dilution feed liquids of addition, filtering, gained filtrate are adsorbed through macroporous absorbent resin HPD300,5 times of trees
The clear water of fat volume rinses resin bed.Parsed with 75% ethanol, gained desorbed solution is less than through being concentrated under reduced pressure into ethanol content
2%, obtain 5.6kg concentrates.
40% ethanol of gained solution analysis of material concentrate is diluted 2 times, medium pressure chromatography is carried out through the chromatography agent of LS-350 types, with
40% ethanol is mobile phase, flow velocity 0.5bv/h, pressure 0.05MPa.
The part of the I containing crocin is collected, temperature control, mixing speed 20rpm are carried out at 15 DEG C, holding 15 is tied when small
Crystalline substance, crystallization are cleaned using 50% ethanol water, and for temperature control at 10 DEG C, the speed of agitator of cleaning be 5rpm during cleaning, is cleaned
5min.Drying is performed under reduced pressure after collecting crystal, final gained 766g peony crystallographic powder, color value 977.8,
HPLC detection crocin I contents are 95.7%, and collection of illustrative plates is shown in Fig. 3.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of extracting method of crocin I, it is characterised in that include the following steps：
The plant medicinal part of the I containing crocin is subjected to alcohol extracting, extracting solution is made；
The extracting solution obtains the first intermediate product through adsorbing separation；The adsorbing separation is inhaled using macroporous absorbent resin
Fufen from；
First intermediate product is purified using medium pressure chromatography system, obtains the second intermediate product；Medium pressure chromatography system
The chromatography agent of system is polystyrene family macromolecule macroporous type polymeric material, and mobile phase is ethanol water, the ethanol water
Volumn concentration be 10%~60%；The pressure of medium pressure tomographic system is 0.05~0.1MPa；
Second intermediate product is crystallized, obtains crocin I.
2. extracting method according to claim 1, it is characterised in that the flow velocity of the mobile phase is 0.2~0.5bv/h.
3. extracting method according to claim 1, it is characterised in that the temperature of the crystallization is -2~15 DEG C, and the time is
15~40h.
4. extracting method according to claim 1, it is characterised in that the mixing speed of the crystallization is 0~20rpm, knot
Brilliant cleaning solvent is ethanol water.
5. extracting method according to claim 1, it is characterised in that the alcohol extracting is water-soluble using 60%~70% ethanol
Liquid extracts.
6. extracting method according to claim 1, it is characterised in that the temperature of the alcohol extracting is 20~30 DEG C, alcohol extracting
Number is 2~4 times.
7. extracting method according to claim 1, it is characterised in that the polystyrene family macromolecule macroporous type polymerize material
The grain fineness of material is 60~300 mesh, and porosity is 10%~45%.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108383884B (en) * | 2018-02-28 | 2021-06-18 | 上海诗丹德标准技术服务有限公司 | Separation and purification method of unstable crocin |
| CN109400660B (en) * | 2018-11-19 | 2021-11-09 | 江苏史蒂文生物科技有限公司 | Crocin standard prepared from fructus Gardeniae by using novel filler, and its preparation method |
| CN110156847A (en) * | 2019-05-14 | 2019-08-23 | 浙江工业大学 | A kind of extracting method of crocin |
| CN110330537B (en) * | 2019-08-23 | 2020-08-21 | 郑州中科新兴产业技术研究院 | Process for extracting high-purity crocin from gardenia fruit |
| CN111171087B (en) * | 2020-02-17 | 2023-09-08 | 天津理工大学 | Purification method and application of high-purity crocin I |
| CN112552169B (en) * | 2020-12-08 | 2023-03-14 | 江西省科学院应用化学研究所 | Crocetin diester compound and preparation method and application thereof |
| CN113144057B (en) * | 2021-06-03 | 2022-09-16 | 上海瀛洲西红花种植专业合作社 | Stigma croci extract and preparation method and application thereof |
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