CN103130629A - High-yield water-based curcumin extraction method - Google Patents

High-yield water-based curcumin extraction method Download PDF

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Publication number
CN103130629A
CN103130629A CN2013100889887A CN201310088988A CN103130629A CN 103130629 A CN103130629 A CN 103130629A CN 2013100889887 A CN2013100889887 A CN 2013100889887A CN 201310088988 A CN201310088988 A CN 201310088988A CN 103130629 A CN103130629 A CN 103130629A
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curcumine
high yield
water extraction
yield according
described step
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CN103130629B (en
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向怡卉
赵丽娟
董玲燕
左海兵
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NINGBO TRADITIONAL CHINESE PHARMACEUTICAL CO Ltd
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NINGBO TRADITIONAL CHINESE PHARMACEUTICAL CO Ltd
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Abstract

The invention relates to a high-yield water-based curcumin extraction method which comprises the following steps: (1) grinding curcuma, soaking with an alkaline water solution of 0-40 DEG C, stirring, extracting, then adding antioxidant, centrifuging, extracting 1-2 times, taking the supernatant, and adding acid to precipitate; and (2) adding an alcohol solution to dissolve the precipitate, centrifuging, adding water to obtain an alcohol dissolving liquid, purifying, concentrating, and drying to obtain curcumin. The curcumin content extracted by the invention can be up to 95%; the extraction and purification yield is more than 80%; and by taking water as extraction solvent, the method is economic, convenient and safe. Thus, the method provided by the invention is a high-yield and low-cost production process.

Description

A kind of method of water extraction curcumine of high yield
Technical field
The invention belongs to the preparation field of curcumine, particularly a kind of method of water extraction curcumine of high yield.
Background technology
Turmeric is the per nnial herb of Zingiber turmeric, and rhizome is flourishing, Cheng Cong, and branch ovalize or cylindric contains the number of chemical composition August at florescence, has good pharmaceutical use and economic outlook.Modern pharmacological research shows that one of the main component of turmeric curcumine has cholagogic, anti-inflammatory, reducing blood-fat, the effect such as antibiotic, anticancer.
Cholagogic: these product or its sodium salt have choleretic effect.During intravenous injection, can reduce the content of dog solids component and increase choleresis.But in the cycle, the absolute total amount of cholate, bilirubin, cholesterol excretion increases in its whole choleresis, and it is constant that fatty acid component keeps.Antibiotic: that streptococcus aureus is had stronger antibacterial effect.During oral 5~20mg/kg, can suppress the Guinea pig Gastric infringement that intramuscular injection 20mg/kg5-hydroxy-tryptamine causes.The hepatic injury that Paracetamol is caused has provide protection.
Find in the time of 2004 that curcumine is can Inhibition of HIV-1 integrase active and be used for the clinical trial of acquired immune deficiency syndrome (AIDS).
Anticancer is one of the main pharmacologically active of curcumine, and its effect that suppresses tumour confirmed in many experimentation on animalies repeatedly, and its concrete anticancer mechanism has become the recent research focus.2006, the researchist of NUS discovery, the curcumine in curry contains antioxygenation, can suppress the kind of starch patch and form at brain, thereby lower the chance of suffering from senile dementia.The ratio that this or soluble why Indian suffer from senile dementia is low than the west.In August, 2012, the researchist of U.S. George Mason University discovery, curcumine is the inhibitor of a series of virus infection healthy cells of a kind of prevention of wide spectrum.
Present factory extracts curcumine from turmeric method is mainly organic solvent extraction, and this method is not only brought the dissolvent residual problem to product, has simultaneously the high shortcoming of production cost.Extracting curcumine with water extraction not only reduces production costs greatly, and solved the problem of dissolvent residual in the curcumine, but the extract yield with water extraction extraction curcumine is very low at present, generally all below 10%, the present invention has well solved the problem that yield is low, finished product content is low in the water extraction curcumine.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of water extraction curcumine of high yield, and the curcumine content that the present invention extracts is up to 95%, and the yield of extraction purifying is more than 80%; The present invention do to extract solvent with water, and economical and convenient is safety again, is a kind of high yield, production technique cheaply.
The method of the water extraction curcumine of a kind of high yield of the present invention comprises:
(1) turmeric is pulverized the rear 0-40 ℃ of alkaline aqueous solution immersion of using, stir and extract, add antioxidant after extraction is completed, centrifugal, repeat 1-2 time, the merging supernatant liquor adds Acid precipitation;
(2) above-mentioned precipitation is added the alcoholic solution dissolving, the centrifugal residue that goes adds water and gets pure lysate, and then purifying, concentrate, and drying namely gets curcumine.
Described step (1) the neutral and alkali aqueous solution is that mass percentage concentration is sodium hydroxide or the potassium hydroxide aqueous solution of 0.5-5%.
In described step (1), the soaking and stirring time is 1-2h.
In described step (1), antioxidant is sodium sulfite solution, and mass percentage concentration is 0.5-1%.
Acid in described step (1) is that concentration of volume percent is aqueous acetic acid or the 1-10% aqueous hydrochloric acid of 20-50%.
In described step (2), alcoholic solution is ethanolic soln, and concentration expressed in percentage by volume is 80%-95%.
In described step (2), the concentration expressed in percentage by volume of pure lysate is 40%-60%.
In described step (2), purification process is the purification with macroreticular resin method.
Described purification with macroreticular resin method is, pure lysate is saturated with resin absorption, will be adsorbed to saturated resin and clean with the alcohol of 40-60%, and removal of impurities is the eluent wash-out with the 65-85% alcoholic solution, the collection elutriant.
Described macroreticular resin is D130.
In described step (2), the crystallization method elutriant is concentrated, and normal temperature is standing, separates out rear collection crystal until crystal.
Beneficial effect
(1) the curcumine content of the present invention's extraction is up to 95%(HPLC), extract the yield of purifying more than 80%;
(2) the present invention makes to extract solvent with water, economical and convenient, and safety is the production technique of a kind of low cost, high yield, high-content, meets energy-saving consumption-reducing production.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
1) curcuma powder 100g, in raw material, turmeric content is 3.43%, the water and the sodium hydroxide 10g that add 10 times of amounts (being 1000ml), 20 ℃ of lower lixiviates 2 hours, adding mass percentage concentration after lixiviate is 0.5% S-WAT, centrifugal, it is that 30% acetum to a large amount of precipitations occur that clear liquid adds concentration expressed in percentage by volume immediately.The gained filter residue adds water and the sodium hydroxide 5g of 10 times of amounts (being 1000ml), 20 ℃ of lower lixiviates 2 hours, adding mass percentage concentration after lixiviate is 0.5% S-WAT, centrifugal, and it is that acetum to a large amount of precipitations of 30% occur that clear liquid adds concentration expressed in percentage by volume immediately.
2) by centrifugal collecting precipitation, merge, be 95% dissolve with ethanol with concentration expressed in percentage by volume, adding suitable quantity of water pure concentration expressed in percentage by volume to the dissolve with ethanol liquid is 50% eventually.
3) dissolve with ethanol liquid is crossed D130 type macroporous resin chromatography column, is 50% washing with alcohol with concentration expressed in percentage by volume, then uses 3 times of column volume 70%(volume fractions) the aqueous ethanolic solution wash-out, collect elutriant.
4) elutriant is concentrated, crystallization, drying namely gets product 2.97g, and curcumine content is 94.7%, and yield is 82%.
Embodiment 2
1) curcuma powder 150g, in raw material, turmeric content is 3.51%, the water and the 25g sodium hydroxide that add 2000ml, 15 ℃ of lower lixiviates 1.5 hours, adding mass percentage concentration after lixiviate is 0.5% S-WAT, centrifugal, it is that 30% acetum to a large amount of precipitations occur that clear liquid adds concentration expressed in percentage by volume immediately.The gained filter residue adds water and the 10g sodium hydroxide of 1500ml, 15 ℃ of lower lixiviates 2 hours, and adding mass percentage concentration after lixiviate is 0.5% S-WAT, centrifugal, it is that acetum to a large amount of precipitations of 30% occur that clear liquid adds concentration expressed in percentage by volume immediately.
2) by centrifugal collecting precipitation, merge, be 80% dissolve with ethanol with concentration expressed in percentage by volume, adding suitable quantity of water pure concentration expressed in percentage by volume to the dissolve with ethanol liquid is 50% eventually.
3) dissolve with ethanol liquid is crossed D130 type macroporous resin chromatography column, is 55% washing with alcohol with concentration expressed in percentage by volume, then uses 3 times of column volume 70%(volume fractions) the aqueous ethanolic solution wash-out, collect elutriant.
4) with the elutriant concentrate drying, namely get product 4.36g, curcumine content is 95.1%, yield is 78.8%.
Embodiment 3
1) curcuma powder 250g, in raw material, turmeric content is 4.01%, adding is 3000ml water and 30g sodium hydroxide, 30 ℃ of lower lixiviates 2 hours, adding mass percentage concentration after lixiviate is 0.8% S-WAT, centrifugal, and it is that acetum to a large amount of precipitations of 50% occur that clear liquid adds concentration expressed in percentage by volume immediately.The gained filter residue adds 2500ml water and 25g sodium hydroxide, 30 ℃ of lower lixiviates 2 hours, and adding mass percentage concentration after lixiviate is 0.8% S-WAT, centrifugal, it is that acetum to a large amount of precipitations of 50% occur that clear liquid adds concentration expressed in percentage by volume immediately.
2) by centrifugal collecting precipitation, merge, be 85% dissolve with ethanol with concentration expressed in percentage by volume, adding suitable quantity of water pure concentration expressed in percentage by volume to the dissolve with ethanol liquid is 50% eventually.
3) dissolve with ethanol liquid is crossed D130 type macroporous resin chromatography column, is 50% washing with alcohol with concentration expressed in percentage by volume, then uses 3 times of column volume 70%(volume fractions) the aqueous ethanolic solution wash-out, collect elutriant.
4) with the elutriant concentrate drying, namely get product 8.63g, curcumine content is 95.8%, yield is 82.4%.

Claims (11)

1. the method for the water extraction curcumine of a high yield comprises:
(1) turmeric is pulverized the rear 0-40 ℃ of alkaline aqueous solution immersion of using, stir and extract, add antioxidant after extraction is completed, centrifugal, repeat 1-2 time, the merging supernatant liquor adds Acid precipitation;
(2) above-mentioned precipitation is added the alcoholic solution dissolving, centrifugal, add water and get pure lysate, then purifying, concentrated, crystallization, drying namely gets curcumine.
2. the method for the water extraction curcumine of a kind of high yield according to claim 1, it is characterized in that: described step (1) the neutral and alkali aqueous solution is that mass percentage concentration is sodium hydroxide or the potassium hydroxide aqueous solution of 0.5-5%.
3. the method for the water extraction curcumine of a kind of high yield according to claim 1 is characterized in that: in described step (1), the soaking and stirring time is 1-2h.
4. the method for the water extraction curcumine of a kind of high yield according to claim 1 is characterized in that: in described step (1), antioxidant is sodium sulfite solution, and mass percentage concentration is 0.5-1%.
5. the method for the water extraction curcumine of a kind of high yield according to claim 1, it is characterized in that: the acid in described step (1) is that concentration of volume percent is aqueous acetic acid or the 1-10% aqueous hydrochloric acid of 20-50%.
6. the method for the water extraction curcumine of a kind of high yield according to claim 1 is characterized in that: in described step (2), alcoholic solution is ethanolic soln, and concentration expressed in percentage by volume is 80%-95%.
7. the method for the water extraction curcumine of a kind of high yield according to claim 1, it is characterized in that: in described step (2), the concentration expressed in percentage by volume of pure lysate is 40%-60%.
8. the method for the water extraction curcumine of a kind of high yield according to claim 1 is characterized in that: in described step (2), purification process is the purification with macroreticular resin method.
9. the method for the water extraction curcumine of a kind of high yield according to claim 8, it is characterized in that: described purification with macroreticular resin method is, the alcohol lysate is saturated with resin absorption, clean being adsorbed to the alcohol of saturated resin with 40-60%, removal of impurities, be the eluent wash-out with the 65-85% alcoholic solution, collect elutriant.
10. the method for the water extraction curcumine of a kind of high yield according to claim 9, it is characterized in that: described macroreticular resin is D130.
11. the method for the water extraction curcumine of a kind of high yield according to claim 1 is characterized in that: in described step (2), the crystallization method elutriant is concentrated, and normal temperature is standing, separates out rear collection crystal until crystal.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105341144A (en) * 2015-10-01 2016-02-24 常州市奥普泰科光电有限公司 Preparation method of fruit fresh keeping agent made in manner that silkworm cocoon casings are coated with curcumin
CN105360690A (en) * 2015-11-27 2016-03-02 全椒县王震家禽养殖专业合作社 High-nutrient goose fattening feed
JP2016199491A (en) * 2015-04-09 2016-12-01 ハウスウェルネスフーズ株式会社 Mood state improver
CN112521259A (en) * 2020-12-24 2021-03-19 晨光生物科技集团股份有限公司 Preparation method of natural curcumin without vanillin

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CN101468944A (en) * 2007-12-24 2009-07-01 北京琥珀光华医药科技开发有限公司 Method for extracting and separating turmeric effective ingredient curcumin
CN101445440A (en) * 2008-12-23 2009-06-03 晨光天然色素集团有限公司 Method for extracting refined curcumin and curcuma oil from curcuma

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2016199491A (en) * 2015-04-09 2016-12-01 ハウスウェルネスフーズ株式会社 Mood state improver
CN105341144A (en) * 2015-10-01 2016-02-24 常州市奥普泰科光电有限公司 Preparation method of fruit fresh keeping agent made in manner that silkworm cocoon casings are coated with curcumin
CN105360690A (en) * 2015-11-27 2016-03-02 全椒县王震家禽养殖专业合作社 High-nutrient goose fattening feed
CN112521259A (en) * 2020-12-24 2021-03-19 晨光生物科技集团股份有限公司 Preparation method of natural curcumin without vanillin

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