CN103130629B - A kind of method of water extraction curcumin of high yield - Google Patents

A kind of method of water extraction curcumin of high yield Download PDF

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CN103130629B
CN103130629B CN201310088988.7A CN201310088988A CN103130629B CN 103130629 B CN103130629 B CN 103130629B CN 201310088988 A CN201310088988 A CN 201310088988A CN 103130629 B CN103130629 B CN 103130629B
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curcumin
high yield
water extraction
concentration
volume
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CN103130629A (en
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向怡卉
赵丽娟
董玲燕
左海兵
方明
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NINGBO CHINESE MEDICINE PHARMACEUTICAL CO Ltd
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NINGBO CHINESE MEDICINE PHARMACEUTICAL CO Ltd
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Abstract

A kind of method that the present invention relates to water extraction curcumin of high yield, comprising: (1) uses 0-40 DEG C of alkaline aqueous solution to soak after turmeric is pulverized, and stirs, and after having extracted, adds antioxidant, centrifugal, extracts 1-2 time, gets supernatant, acid adding precipitation; (2) above-mentioned precipitation is added to alcoholic solution and dissolve, centrifugal, the alcohol lysate that adds water to obtain, then purifying, concentrated, dry, obtain curcumin. The curcumin content that the present invention extracts can reach 95%, and extracts the yield of purifying more than 80%, and taking water as extracting solvent, economical and convenient is safety again simultaneously, is a kind of high yield, production technology cheaply.

Description

A kind of method of water extraction curcumin of high yield
Technical field
The invention belongs to the preparation field of curcumin, particularly a kind of method of water extraction curcumin of high yield.
Background technology
Turmeric is the herbaceos perennial of Zingiber turmeric, rhizome prosperity, Cheng Cong, branch ovalize or cylindric, flowerAugust phase, contain number of chemical composition, there is good medical value and economic outlook. Modern pharmacological research shows turmericOne of main component curcumin has cholagogic, anti-inflammatory, reducing blood lipid, the effect such as antibacterial, anticancer.
Cholagogic: these product or its sodium salt have choleretic effect. When intravenous injection, can reduce the content of dog solid constituent and increase bileSecretory volume. But in its whole choleresis cycle, the absolute total amount of cholate, bilirubin, cholesterine excretion increases, fatAcid composition keeps constant. Antibacterial: staphylococcus aureus is had to stronger antibacterial effect. When oral 5~20mg/kg, energySuppress the Guinea pig Gastric infringement that intramuscular injection 20mg/kg5-hydroxytryptamine causes. The hepatic lesion that paracetamol is caused has protective effect.
2004 time, find that curcumin energy Inhibition of HIV-1 integrase is active and for the clinical testing of AIDS.
Anticancer is one of the main pharmacologically active of curcumin, and its effect that suppresses tumour obtains repeatedly in many zooperiesConfirm, its concrete anticancer mechanism has become recent research focus. 2006, the researcher of NUS found, coffeeCurcumin in curry, containing antioxidation, can suppress kind of starch patch and form at brain, thereby lowers the machine of suffering from senile dementiaMeeting. The ratio that this or soluble why Indian suffer from senile dementia is low compared with west. In August, 2012, George Mason is large in the U.S.Learn researcher and find, curcumin is the inhibitor of a series of virus infections healthy cells of a kind of prevention of wide spectrum.
The method that current factory extracts curcumin from turmeric is mainly organic solvent and extracts, and this method is not only brought to product, there is the shortcoming that production cost is high in dissolvent residual problem simultaneously. Extracting curcumin with water extraction not only greatly reduces and is produced intoThis, and solved the problem of dissolvent residual in curcumin, but the current extract yield with water extraction extraction curcumin is veryLow, generally all below 10%, the present invention has well solved the problem that yield is low, finished product content is low in water extraction curcumin.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of water extraction curcumin of high yield, the ginger that the present invention extractsFlavine content is up to 95%, and the yield that extracts purifying is more than 80%; The present invention makes to extract solvent, economical and convenient with waterSafety is again a kind of high yield, production technology cheaply.
The method of the water extraction curcumin of a kind of high yield of the present invention, comprising:
(1) turmeric is pulverized to the rear 0-40 DEG C of alkaline aqueous solution immersion of using, stir and extract, after having extracted, add antioxidant, fromThe heart, repeats 1-2 time, merges supernatant, acid adding precipitation;
(2) above-mentioned precipitation is added to alcoholic solution and dissolve, the centrifugal residue that goes, the alcohol lysate that adds water to obtain, then purifying, concentrated, dry,Obtain curcumin.
Described step (1) the neutral and alkali aqueous solution is that mass percentage concentration is NaOH 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 solution of 20-50%.
In described step (2), alcoholic solution is ethanolic solution, and concentration expressed in percentage by volume is 80%-95%.
In described step (2), the concentration expressed in percentage by volume of alcohol lysate is 40%-60%.
In described step (2), purification process is purification with macroreticular resin method.
Described purification with macroreticular resin method is that alcohol lysate is saturated by resin adsorption, uses being adsorbed to saturated resinThe alcohol of 40-60% cleans, removal of impurities, with 65-85% alcoholic solution be eluant, eluent wash-out, collection eluent.
Described macroreticular resin is D130.
In described step (2), method for crystallising eluent is concentrated, and normal temperature leaves standstill, and collects crystal after crystal is separated out.
Beneficial effect
(1) the curcumin content that the present invention extracts 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 a kind of low cost, high yield, high-loadProduction technology, meets energy-saving consumption-reducing and produces.
Detailed description of the invention
Below in conjunction with specific embodiment, further set forth the present invention. Should be understood that these embodiment are only for illustrating the present inventionBe not used in and limit the scope of the invention. In addition should be understood that after having read the content of the present invention's instruction art technology peopleMember can make various changes or modifications the present invention, and these equivalent form of values fall within equally the application's appended claims and limitScope.
Embodiment 1
1) curcuma powder 100g, in raw material, turmeric content is 3.43%, adds water and the hydroxide of 10 times of amounts (being 1000ml)Sodium 10g, lixiviate 2 hours at 20 DEG C, after lixiviate, adding mass percentage concentration is 0.5% sodium sulfite, centrifugal, clear liquid is verticalAdding concentration expressed in percentage by volume is that 30% acetum to a large amount of precipitations occur. Gained filter residue adds 10 times of amounts (being 1000ml)Water and NaOH 5g, lixiviate 2 hours at 20 DEG C, after lixiviate, adding mass percentage concentration is 0.5% sodium sulfite,Centrifugal, it is that 30% acetum to a large amount of precipitations occur that clear liquid adds concentration expressed in percentage by volume immediately.
2) by centrifugal collecting precipitation, merge, the ethanol that is 95% by concentration expressed in percentage by volume dissolves, and adds suitable quantity of water to ethanolIn lysate, alcohol concentration expressed in percentage by volume is 50% eventually.
3) ethanol lysate is crossed D130 type macroreticular resin chromatographic column, is that 50% ethanol washs, then uses 3 by concentration expressed in percentage by volumeTimes column volume 70%(volume fraction) ethanol water wash-out, collect eluent.
4) eluent is concentrated, crystallization, dry, obtain product 2.97g, curcumin content is 94.7%, yield is 82%.
Embodiment 2
1) curcuma powder 150g, in raw material, turmeric content is 3.51%, adds water and the 25g NaOH of 2000ml, 15 DEG CLower lixiviate 1.5 hours, after lixiviate, adding mass percentage concentration is 0.5% sodium sulfite, centrifugal, clear liquid adds volume immediatelyPercentage concentration is 30% the extremely a large amount of precipitation appearance of acetum. Gained filter residue adds water and the 10g NaOH of 1500ml,Lixiviate 2 hours at 15 DEG C, after lixiviate, adding mass percentage concentration is 0.5% sodium sulfite, centrifugal, clear liquid adds body immediatelyLong-pending percentage concentration is 30% the extremely a large amount of precipitation appearance of acetum.
2) by centrifugal collecting precipitation, merge, the ethanol that is 80% by concentration expressed in percentage by volume dissolves, and adds suitable quantity of water to ethanolIn lysate, alcohol concentration expressed in percentage by volume is 50% eventually.
3) ethanol lysate is crossed D130 type macroreticular resin chromatographic column, is that 55% ethanol washs, then uses 3 by concentration expressed in percentage by volumeTimes column volume 70%(volume fraction) ethanol water wash-out, collect eluent.
4) by eluent concentrate drying, obtain product 4.36g, curcumin 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 NaOH, 30Lixiviate 2 hours at DEG C, after lixiviate, adding mass percentage concentration is 0.8% sodium sulfite, centrifugal, clear liquid adds volume immediatelyPercentage concentration is 50% the extremely a large amount of precipitation appearance of acetum. Gained filter residue adds 2500ml water and 25g NaOH,Lixiviate 2 hours at 30 DEG C, after lixiviate, adding mass percentage concentration is 0.8% sodium sulfite, centrifugal, clear liquid adds body immediatelyLong-pending percentage concentration is 50% the extremely a large amount of precipitation appearance of acetum.
2) by centrifugal collecting precipitation, merge, the ethanol that is 85% by concentration expressed in percentage by volume dissolves, and adds suitable quantity of water to ethanolIn lysate, alcohol concentration expressed in percentage by volume is 50% eventually.
3) ethanol lysate is crossed D130 type macroreticular resin chromatographic column, is that 50% ethanol washs, then uses 3 by concentration expressed in percentage by volumeTimes column volume 70%(volume fraction) ethanol water wash-out, collect eluent.
4) by eluent concentrate drying, obtain product 8.63g, curcumin content is 95.8%, yield is 82.4%.

Claims (4)

1. a method for the water extraction curcumin of high yield, comprising:
(1) turmeric is pulverized to the rear 0-40 DEG C of alkaline aqueous solution immersion of using, stir and extract, after having extracted, add antioxidant, centrifugal,Repeat 1-2 time, merge supernatant, acid adding precipitation; Alkaline aqueous solution is that mass percentage concentration is the hydroxide of 0.5-5%Sodium or potassium hydroxide aqueous solution; The aqueous acetic acid that acid is 20-50% for concentration of volume percent; Antioxidant is sulfurousAcid sodium solution, mass percentage concentration is 0.5%
(2) above-mentioned precipitation is added to alcoholic solution and dissolve, centrifugal, the alcohol lysate that adds water to obtain, then purifying, concentrated, crystallization, dry,Obtain curcumin; Wherein alcoholic solution is ethanolic solution, and concentration expressed in percentage by volume is 80%-95%; Purification process is that macropore is inhaledAttached purifying resin method, purification with macroreticular resin method is that alcohol lysate is saturated by resin adsorption, saturated by being adsorbed toResin cleans with the alcohol of 40-60%, removal of impurities, with 65-85% alcoholic solution be eluant, eluent wash-out, collection eluent; WhereinMacroreticular resin is D130.
2. the method for the water extraction curcumin 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.
3. the method for the water extraction curcumin of a kind of high yield according to claim 1, is characterized in that: in described step (2)The concentration expressed in percentage by volume of alcohol lysate is 40%-60%.
4. the method for the water extraction curcumin of a kind of high yield according to claim 1, is characterized in that: in described step (2)Method for crystallising eluent is concentrated, and normal temperature leaves standstill, and collects crystal after crystal is separated out.
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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
CN112521259B (en) * 2020-12-24 2022-11-18 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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