CN109232230A - A method of extracting crocin from fresh gardenia - Google Patents
A method of extracting crocin from fresh gardenia Download PDFInfo
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- CN109232230A CN109232230A CN201811287625.5A CN201811287625A CN109232230A CN 109232230 A CN109232230 A CN 109232230A CN 201811287625 A CN201811287625 A CN 201811287625A CN 109232230 A CN109232230 A CN 109232230A
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- crocin
- fresh gardenia
- oscillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C57/00—Unsaturated compounds having carboxyl groups bound to acyclic carbon atoms
- C07C57/02—Unsaturated compounds having carboxyl groups bound to acyclic carbon atoms with only carbon-to-carbon double bonds as unsaturation
- C07C57/13—Dicarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G99/00—Subject matter not provided for in other groups of this subclass
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The method that the present invention provides a kind of to extract crocin from fresh gardenia, it is using fresh gardenia flower or fruit as raw material, using added with the sonic oscillation method for vibrating broken pearl, using its strong cavitation effect, mechanical oscillation, disturbance effect, high acceleration, emulsification, spreads, smashes and the multistage effect such as stirring action, increase molecular motion of material frequency and speed, increase solvent penetration power, to accelerate crocin to enter solvent, extraction is recycled, the mode of film purifying sufficiently extracts crocin.The beneficial effect is that, the present invention is using fresh cape jasmine explant as extraction raw material, it avoids currently used drying or process to adversely affect to crocin bring, this method step is few, easy to operate, whole process is without using complicated equipment and instrument, at low cost, purity is high is active good, Extracting temperature is low, recovery rate is high, extraction time is short, energy-saving and environmental protection.
Description
Technical field
The invention belongs to technical field of plant extraction, and crocin is extracted from fresh gardenia more particularly, to one kind
Method.
Background technique
Cape jasmine, evergreen shrubs are distributed in south China and middle part, the month at florescence 5-7 of cape jasmine, the fruiting period 8-11 month.Cape jasmine is
First dual-purpose of drug and food product of the Ministry of Public Health of China publication are the plants of a kind of great ornamental value, consumption and medical, each
Position finds there is application value under modern study.Contain there are many chemical component in fruit, flower, leaf, root position, and equal
There is biggish difference.Currently, the position that cape jasmine is most applied extensively is cape jasmine fruit.Cape jasmine fruit Gardenoside has liver protection benefit
Gallbladder, anti-inflammatory, analgesia, antitumor, prevention and treatment influenza and other effects, it is a lot of in terms of clinical application.The cape jasmine extracted in cape jasmine fruit
Pigment is for industry such as food, drug, dyestuffs.The fragrance extracted in gardenia is a kind of rare fragrance, and extraction is waved
Hair oil can be used for making perfumed soap, perfume, cosmetic etc..Cape jasmine leaf has activating blood circulation and reducing swelling, clearing heat and detoxicating effect, in recent years cape jasmine leaf
It is in food industry, cosmetics industry to have application more.Cape jasmine root medical value is high, is mainly used for clinic.
Crocin is in the fruit of cape jasmine and content is higher in spending, and the main component of its pigment is served as in cape jasmine, be from
A kind of unique water-soluble carotenoid, appearance are in rufous powder existing for right boundary, there is crocin, crocinWith
Crocin.Crocin has good water-soluble and alcohol-soluble, and alcoholic solution is bright-coloured yellow, is to confer to green bamboo snake
The principle active component of wine yellow.Crocin has the effect of tonifying Qi, activating microcirculation and removing stasis medicinal, cholagogue, can reduce cholesterol, simultaneously
Fat metabolism can be increased, have excitation to breathing, also there is immunoregulation effect, and study in modern age clinical science
In, crocin preparation also has a more apparent suppression cancer, antitumaous effect, and with other tumor Drugs partner treatment mistakes
Cheng Zhong can reduce the toxicity of anticarcinogen cis-platinum etc., improve curative effect.At present for the research table of crocin mechanism of tumor suppressor
Bright, there are many possible effect paths, and wherein apoptotic pathway has obtained more research support.
The dry fruit that raw material currently used for extracting cape jasmine crocin is from after dry or processing crushes in fact.
The method for being currently used for extracting cape jasmine crocin is mainly neutral alumina impurity removal method, active carbon adsorption, overcritical dioxy
Change carbon flow body technique, gel chromatography, inoranic membrane extraction method etc..The final form of its product is ethanol solution, can be subtracted in this way
Few precipitating, moreover it is possible to anti-corrosion.
Summary of the invention
To solve the above problems, the present invention provides a kind of method that crocin is extracted from fresh gardenia, it is using super
Acoustic irradiation pressure generate strong cavitation effect, mechanical oscillation, disturbance effect, high acceleration, emulsification, spread, smash and
The multistage effect such as stirring action, and vibrate broken pearl and increase molecular motion of material frequency and speed, increase solvent penetration power, from
And target component crocin is accelerated to enter solvent, promote the progress extracted.The method comprises the following steps:
S1: it takes fresh gardenia explant to smash grinding to pieces, obtains abrasive material；
S2: 40% ~ 70% ethanol solution of 10 ~ 50 times of w/vs is added in abrasive material in step sl, and it is total to add solution
1/10 ~ 1/5 oscillation of volume is crushed pearl, must be crushed liquid after 1 ~ 2h of sonic oscillation, wherein amplitude is 100 ~ 500mm, oscillation frequency
Rate 5 ~ 10min/ times, every minor tick 2min, 400 ~ 600W of ultrasonic power, overall solution volume be abrasive material and volumes of aqueous ethanol it
With；
S3: being centrifuged 5 ~ 10min for liquid is crushed in step S2 under 4000 ~ 6000rpm revolving speed, take supernatant, and with 100 ~ 200mL
Aseptic water washing vibrates broken pearl, obtains flushing liquor, flushing liquor is merged with supernatant, obtains filtrate；
S4: filtrate in step S3 is extracted 2 ~ 3 times repeatedly with 1 ~ 3 times of organic solvent, is concentrated to give crocin crude extract；
S5: 40% ~ 70% ethyl alcohol of crocin crude extract in step S4 being redissolved, then is filtered with miillpore filter, collects filter
Liquid is simultaneously concentrated and dried, and obtains crocin.
The present invention avoids currently used drying or process using fresh cape jasmine explant as raw material is extracted
It is adversely affected to crocin bring, while using ultrasound plus the broken common auxiliary of pearl oscillation, so that extraction efficiency improves, and
Step is few, easy to operate, and whole process is without using complicated equipment and instrument.
Further, cape jasmine explant is one or both of fruit or flower in the step S1.
Further, it is the solid or hollow ball that partial size is 5 ~ 10mm, the material of ball that the step S2, which vibrates broken pearl,
For metal, stainless steel or polyethylene kind macromolecule can be obtained using commercially available material.
Further, oscillation is horizontal oscillations, one of vertical oscillation or the oscillation of horizontal spiral or more in the step S2
Kind.
Further, the aperture of miillpore filter is 0.45 μm in the step S5.
Further, organic solvent is one of ethyl acetate or butyl acetate in the step S5.
Further, the temperature for vibrating or being concentrated in the step S2, S4 and S5 is 30 ~ 50 DEG C.
Further, 40% ~ 70% ethanol solution of 10 ~ 20 times of w/vs is added in step S2 in abrasive material.
Compared with the existing technology, the present invention has the advantage that and effect:
1. Extracting temperature is low, recovery rate is high, extraction time is short, activity is high.
2. at low cost, purity is high, operating procedure is few, and process is simple.
3. energy-saving and environmental protection.
Specific embodiment
Further illustrate the present invention below in conjunction with specific embodiment, but embodiment the present invention is not done it is any type of
It limits.Unless stated otherwise, the present invention uses reagent, method and apparatus is the art conventional reagents, method and apparatus.
Unless stated otherwise, agents useful for same and material of the present invention are commercially available.
Embodiment 1:
S1: it takes fresh gardenia flower 200g to smash grinding to pieces, obtains abrasive material.
S2: being added 70% ethanol solution of 2000mL in abrasive material and adds the broken pearl of oscillation, after being crushed after pearl precipitating about
The 1/5 of total solution volume is accounted for, sonic oscillation 1h obtains broken liquid, wherein amplitude 200mm, frequency of oscillation 15min/ times, every time
It is spaced 2min, ultrasonic power 400W.
S3: being centrifuged 5min for broken liquid 4000rpm, takes supernatant, and vibrate broken pearl with 200mL aseptic water washing, stays
Flushing liquor is taken, and is merged with supernatant, filtrate is obtained.
S4: filtrate is extracted 3 times repeatedly with 1500mL ethyl acetate, 40 DEG C are concentrated to give crocin crude extract 20mL.
S5: 40% ethyl alcohol of crocin crude extract is redissolved, after filtered in 0.45um miillpore filter, collect filtrate simultaneously
It is concentrated and dried, obtains crocin alcoholic solution 1mL, surveying its content is 1.54mg/mL.
Embodiment 2:
S1: it takes fresh gardenia fruit 200g to smash grinding to pieces, obtains lapping liquid.
S2: being added 40% ethanol solution of 2500mL in lapping liquid and adds the broken pearl of oscillation, after being crushed after pearl precipitating about
The 1/5 of total solution volume is accounted for, sonic oscillation 2h obtains broken liquid, wherein amplitude 200mm, frequency of oscillation 15min/ times, every time
It is spaced 2min, ultrasonic power 600W.
S3: being centrifuged 5min for broken liquid 6000rpm, takes supernatant, and vibrate broken pearl with 200mL aseptic water washing, stays
Flushing liquor is taken, and is merged with supernatant, filtrate is obtained.
S4: filtrate is extracted 3 times repeatedly with 2000mL ethyl acetate, 40 DEG C are concentrated to give crocin crude extract 20mL.
S5: 70% ethyl alcohol of crocin crude extract is redissolved, after filtered in 0.45um miillpore filter, collect filtrate simultaneously
It is concentrated and dried, obtains crocin alcoholic solution 1mL, surveying its content is 2.85mg/mL.
Claims (8)
1. a kind of method for extracting crocin from fresh gardenia, which is characterized in that the method comprises the following steps:
S1: it takes fresh gardenia explant to smash grinding to pieces, obtains abrasive material；
S2: 40% ~ 70% ethanol solution of 10 ~ 50 times of w/vs is added in abrasive material in step sl, and it is total to add solution
1/10 ~ 1/5 oscillation of volume is crushed pearl, must be crushed liquid after 1 ~ 2h of sonic oscillation, wherein amplitude is 100 ~ 500mm, oscillation frequency
Rate 5 ~ 10min/ times, every minor tick 2min, 400 ~ 600W of ultrasonic power, overall solution volume be abrasive material and volumes of aqueous ethanol it
With；
S3: being centrifuged 5 ~ 10min for liquid is crushed in step S2 under 4000 ~ 6000rpm revolving speed, take supernatant, and with 100 ~ 200mL
Aseptic water washing vibrates broken pearl, obtains flushing liquor, flushing liquor is merged with supernatant, obtains filtrate；
S4: filtrate in step S3 is extracted 2 ~ 3 times repeatedly with 1 ~ 3 times of organic solvent, is concentrated to give crocin crude extract；
S5: 40% ~ 70% ethyl alcohol of crocin crude extract in step S4 being redissolved, then is filtered with miillpore filter, collects filter
Liquid is simultaneously concentrated and dried, and obtains crocin.
2. the method according to claim 1 for extracting crocin from fresh gardenia, which is characterized in that Cape jasmine in step S1
Sub- explant is one or both of fruit or flower.
3. the method according to claim 1 for extracting crocin from fresh gardenia, which is characterized in that the step S2
Vibrating broken pearl is the solid or hollow ball that partial size is 5 ~ 10mm, and the material of ball is metal, and stainless steel or polyethylene kind are high
Molecule.
4. the method according to claim 1 for extracting crocin from fresh gardenia, which is characterized in that the step S2
Middle oscillation is horizontal oscillations, one of vertical oscillation or the oscillation of horizontal spiral or a variety of.
5. the method according to claim 1 for extracting crocin from fresh gardenia, which is characterized in that the step S5
The aperture of middle miillpore filter is 0.45 μm.
6. the method according to claim 1 for extracting crocin from fresh gardenia, which is characterized in that the step S5
Middle organic solvent is one of ethyl acetate or butyl acetate.
7. the method according to claim 1 for extracting crocin from fresh gardenia, which is characterized in that the step
The temperature for vibrating or being concentrated in S2, S4 and S5 is 30 ~ 50 DEG C.
8. the method according to claim 1 for extracting crocin from fresh gardenia, which is characterized in that ground in step S2
Grind 40% ~ 70% ethanol solution that 10 ~ 20 times of w/vs are added in object.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811287625.5A CN109232230A (en) | 2018-10-31 | 2018-10-31 | A method of extracting crocin from fresh gardenia |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811287625.5A CN109232230A (en) | 2018-10-31 | 2018-10-31 | A method of extracting crocin from fresh gardenia |
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| Publication Number | Publication Date |
|---|---|
| CN109232230A true CN109232230A (en) | 2019-01-18 |
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ID=65079762
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| Application Number | Title | Priority Date | Filing Date |
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| CN201811287625.5A Withdrawn CN109232230A (en) | 2018-10-31 | 2018-10-31 | A method of extracting crocin from fresh gardenia |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113180277A (en) * | 2021-06-02 | 2021-07-30 | 西南林业大学 | Application of saffron natural pigment in novel tobacco and preparation method thereof |
Citations (7)
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|---|---|---|---|---|
| WO2004078695A1 (en) * | 2003-03-07 | 2004-09-16 | Riken Vitamin Co., Ltd. | Method for the purification of crocetin |
| CN102432455A (en) * | 2011-12-14 | 2012-05-02 | 广西大学 | Method for preparing crocetin and crocin |
| CN102914462A (en) * | 2012-11-22 | 2013-02-06 | 上海化工研究院 | High-throughput method for extracting carotene in biological sample |
| CN103203265A (en) * | 2012-01-13 | 2013-07-17 | 谢小飞 | Ultrasonic high-energy density bead mill for biological cell wall breaking |
| CN104327133A (en) * | 2014-10-15 | 2015-02-04 | 浙江天露生物科技有限公司 | Gardenia jasminoides effective component comprehensive extraction technology |
| CN105176137A (en) * | 2015-09-11 | 2015-12-23 | 福建恒康生态农业发展有限公司 | Separation preparation method of gardenia oil, water-soluble gardenia pigment and gardenin |
| WO2017042257A1 (en) * | 2015-09-09 | 2017-03-16 | Pierre Fabre Medicament | Gardenia extract for colouring the skin |
-
2018
- 2018-10-31 CN CN201811287625.5A patent/CN109232230A/en not_active Withdrawn
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004078695A1 (en) * | 2003-03-07 | 2004-09-16 | Riken Vitamin Co., Ltd. | Method for the purification of crocetin |
| CN102432455A (en) * | 2011-12-14 | 2012-05-02 | 广西大学 | Method for preparing crocetin and crocin |
| CN103203265A (en) * | 2012-01-13 | 2013-07-17 | 谢小飞 | Ultrasonic high-energy density bead mill for biological cell wall breaking |
| CN102914462A (en) * | 2012-11-22 | 2013-02-06 | 上海化工研究院 | High-throughput method for extracting carotene in biological sample |
| CN104327133A (en) * | 2014-10-15 | 2015-02-04 | 浙江天露生物科技有限公司 | Gardenia jasminoides effective component comprehensive extraction technology |
| WO2017042257A1 (en) * | 2015-09-09 | 2017-03-16 | Pierre Fabre Medicament | Gardenia extract for colouring the skin |
| CN105176137A (en) * | 2015-09-11 | 2015-12-23 | 福建恒康生态农业发展有限公司 | Separation preparation method of gardenia oil, water-soluble gardenia pigment and gardenin |
Non-Patent Citations (3)
| Title |
|---|
| 姚立霞: ""栀子黄色素提取及精制工艺的研究"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 徐洁等: "《芳香植物研究与应用》", 30 April 2017, 昆明：云南科技出版社 * |
| 黄弦等: ""多指标评价栀子超声提取工艺"", 《时珍国医国药》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113180277A (en) * | 2021-06-02 | 2021-07-30 | 西南林业大学 | Application of saffron natural pigment in novel tobacco and preparation method thereof |
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Application publication date: 20190118 |