CN1279049C - Extraction and purification of blue berry and its product - Google Patents
Extraction and purification of blue berry and its product Download PDFInfo
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- CN1279049C CN1279049C CN 200410022696 CN200410022696A CN1279049C CN 1279049 C CN1279049 C CN 1279049C CN 200410022696 CN200410022696 CN 200410022696 CN 200410022696 A CN200410022696 A CN 200410022696A CN 1279049 C CN1279049 C CN 1279049C
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Abstract
The present invention relates to an extraction and purification method for blue berries and a product thereof. The blue berries are extracted by reflux via acidified alcohol, treated by impurity removal, concentrated, hyperfiltrated and dried to obtain crude extracts, and blue berry anthocyanins with over 35% of anthocyanins can be obtained by adding an on-column woking procedure between hyperfiltration and drying. The method of the present invention has the advantages of simple operation, low cost, safe production, and can remarkably improve the purity of total anthocyanins in extracts; the product obtained by the method of the present invention has the advantages of high nutritive value, good pharmacological action and good bioactivity, and is precious raw material for producing health food and medicine.
Description
Technical field
The invention relates to the extraction and separation method of effective components in plants, be specifically related to a kind of method of from blue berry, extracting anthocyanin compound effective constituent, belong to biological pharmacy technical field.
Background technology
Blue berry (Vaccinium myrtillus L.) is the health fruit that a class is rich in multiple nutritional components, and its resistance of oxidation occupy first of fruit and the vegetables, is classified as one of human 5 big heath food by Food and Argriculture OrganizationFAO.At present, the multiple bioactive ingredients in the blue berry, particularly pattern glucoside material are the focuses of foreign study.
The pattern glucoside is one of best natural pigment that has been utilized up to now in the blue berry, and it has complied with the trend of green food as a kind of plant pigments.
In recent years, many bibliographical informations the nutritive value and the pharmacological action of blue berry anthocyanin, be mainly following some: 1. promote the resynthesis of erythrolabe on the retina, strengthen human eyesight; 2. delay the cranial nerve aging; 3. improve recycle system function; 4. the very strong function of removing active oxygen.So the research and development of blue berry anthocyanin are worth and are that not only it can be developed to additive or tinting material as a kind of high-quality natural pigment, the more important thing is that it can be used as a kind of new bioactive ingredients, is developed to health care, functional food and medicine.
The China that is extracted in of effective constituent studies considerably less in the blue berry, the foreign literature report also seldom, just in the document of being reported, the extraction process of blue berry effective constituent is, earlier with the not extraction using alcohol backflow of specified acid alkalescence, again through staticly settle, the chemical process removal of impurities, concentrate then, vacuum-drying obtains extract.The whole process complex procedures of described extracting method, the cost height, the extract purity that is obtained is lower.
Summary of the invention
The purpose of this invention is to provide and a kind ofly from blue berry pomace, extract useful medicinal ingredients, and make higher blue berry extracting and purifying method of its extract purity and products thereof.
The object of the present invention is achieved like this:
A kind of extracting and purifying method of blue berry comprises extraction, removal of impurities, concentrated, drying step, it is characterized in that also having the ultrafiltration operation between concentrated and drying, wherein:
A, extraction: with concentration is 30%-80%, PH be ethanol and the blue berry pomace powder of 2-6 with 1: 1-1: 10 solid-liquid ratio mixes, 30 ℃-90 ℃ following refluxing extraction 0.5-2 hour, filter and collect filtrate and residue, mix with residue and identical solid-liquid ratio with the acidifying ethanolic soln of concentration again, under uniform temp refluxing extraction 0.5-2 hour again, filter and also collect filtrate, merge twice filtrate;
B, removal of impurities: A step gained merging filtrate under 0 ℃ of-4 ℃ of low temperature, was placed 12-24 hour, filtered with B;
C, concentrated: filtrate is concentrated at 50 ℃ of following reduction vaporizations, concentrate 10-12 hour;
D, ultrafiltration: the millipore filtration that with concentrated solution by the aperture is 0.45um and 0.22um degerms and high molecular weight protein to remove;
E, drying: after filtrate or elutriant removed most of ethanol, dry in 50 ℃ of-60 ℃ of vacuum.
According to the extracting and purifying method of above-mentioned blue berry, can obtain crude extract, anthocyanin content is greater than 5% in the crude extract.If between ultrafiltration and drying step, increase the upper prop operation, can obtain highly purified extract, anthocyanin content is greater than 35% in this extract.Described upper prop is meant: earlier filtrate is crossed macroporous adsorbent resin with the velocity flow of 1-3 times of column volume per hour, cross resin with the distilled water of 2-5 times of column volume with identical velocity flow then, the most of impurity of flush away; Cross resin with the ethanolic soln of the 60%-90% of 1-3 column volume with identical velocity flow again, the anthocyanin that adsorbs on the resin is eluted, collect elutriant.
The present invention adopts the acidifying ethanol (PH=2-6) that is different from traditional technology to carry out refluxing extraction, can fully improve the solubility rate of anthocyanin in ethanol, thereby stripping anthocyanin as much as possible, and anthocyanin is more stable in sour environment, suppresses the degraded of anthocyanin.
The present invention introduces the ultrafiltration operation that does not have in the traditional technology, has simplified loaded down with trivial details step in the chemical subtraction process greatly like this, has reduced the loss of anthocyanin in the removal of impurities process, has saved cost; Ultrafiltration removal of impurities simultaneously can be held back high molecular weight protein and most of bacterium, and this is more thorough than chemical subtraction, improved the purity of total anthocyanin in the product more completely, is that following process has been established aseptic basis and hold back most of bacterium.
Extracting and purifying method of the present invention compared with prior art, and is simple to operate, cost is low, production safety, can improve the purity of total anthocyanin in the extract significantly.Have nutritive value and pharmacological action with the product that the inventive method obtained, it is the valuable raw material of protective foods and pharmaceutical production.Proof uses the inventive method extract obtained through ultraviolet spectrophotometry and efficient liquid phase chromatographic analysis by experiment, and total anthocyanin purity has reached 35%, and traditional technology can only reach 20%; And has higher biological activity.
Embodiment
Embodiment 1:
With blue berry pomace 20 grams is raw material, after moisture is removed in oven dry in aeration cabinet, the Florence flask of packing into, add 2 times of volumes, PH and be 2, concentration is 30% ethanolic soln, place on the water-bath, refluxing extraction is 0.5 hour under 30 ℃ of conditions, collects filtrate and residue respectively after filtering with B.Residue is packed in the Florence flask, add 2 times of volumes, PH and be 2, concentration is 30% ethanolic soln, 0.5 hour after-filtration of refluxing extraction under identical condition merges in twice filtrate and the Florence flask of packing into, put into temperature again and be 0 ℃ refrigerator, left standstill 10 hours.Then, take out refrigerator, filter, filtrate is placed on the rotatory evaporator, concentrate 10 hours down, obtain 50 milliliters of concentrated solutions at 50 ℃ with B.After concentrated solution is 0.45 micron millipore filtration by the aperture, carry out ultrafiltration with 0.22 micron film again, collect wash-out filtrate.Elutriant is placed vacuum drying oven, and at 50 ℃ of following dry blue berry crude extracts that get, its anthocyanin content is 15%.This extract can be used as the raw material that protective foods is produced.
Embodiment 2:
With blue berry pomace 20 grams is raw material, after moisture is removed in oven dry in aeration cabinet, the Florence flask of packing into, add 5 times of volumes, PH and be 3, concentration is 80% ethanolic soln, place on the water-bath, refluxing extraction is 1 hour under 50 ℃ of conditions, collects filtrate and residue respectively after filtering with B.Residue is packed in the Florence flask, add 5 times of volumes, PH and be 3, concentration is 80% ethanolic soln, at 1 hour after-filtration of identical condition refluxing extraction, merges filtrate twice.Filtrate is placed on the rotatory evaporator, concentrate 12 hours down, obtain 150 milliliters of concentrated solutions in 50 ℃.Concentrated solution is packed in the Florence flask, put into temperature again and be 4 ℃ refrigerator, left standstill 12 hours.Then, take out refrigerator, filter with B, filtrate is 0.45 micron millipore filtration by the aperture after, carry out ultrafiltration, collection filtrate with 0.22 micron film again.The adsorption column of packing into after the AB-8 macroporous adsorbent resin cleaned.150 milliliters of filtrates are crossed resin with the velocity flow of 2 times of column volumes per hour, after treating that resin fully absorbs anthocyanin, distilled water with 4 times of column volumes is crossed resin with identical velocity flow, with the most of impurity of flush away, again 70% ethanolic soln of 2 times of column volumes is crossed resin with identical velocity flow, anthocyanin is eluted, collect elutriant.Elutriant is placed vacuum drying oven, be drying to obtain purity and be 35% blue berry anthocyanin under 50 ℃, it is as the raw material of pharmaceutical production.
Embodiment 3:
With blue berry pomace 20 grams is raw material, after moisture is removed in oven dry in aeration cabinet, the Florence flask of packing into, add 10 times of volumes, PH and be 6, concentration is 60% ethanolic soln, place on the water-bath, refluxing extraction is 2 hours under 90 ℃ of conditions, collects filtrate and residue respectively after filtering with B.Residue is packed in the Florence flask, add 10 times of volumes, PH and be 6, concentration is 60% ethanolic soln, at 2 hours after-filtration of identical condition refluxing extraction, merges filtrate twice.Merging filtrate is packed in the Florence flask, put into temperature again and be 2 ℃ refrigerator, left standstill 11 hours.Then, take out refrigerator, filter, filtrate is placed on the rotatory evaporator, concentrate 10-12 hour down, obtain 200 milliliters of concentrated solutions in 50 ℃ with B.After concentrated solution is 0.45 micron millipore filtration by the aperture, carry out ultrafiltration with 0.22 micron film again, collect filtrate.The adsorption column of packing into after the AB-8 macroporous adsorbent resin cleaned.200 milliliters of filtrates are crossed resin with the velocity flow of 3 times of column volumes per hour, after treating that resin fully absorbs anthocyanin, distilled water with 6 times of column volumes is crossed resin with identical velocity flow, with the most of impurity of flush away, again 80% ethanolic soln of 3 times of column volumes is crossed resin with identical velocity flow, anthocyanin is eluted, collect elutriant.Elutriant is placed vacuum drying oven, be drying to obtain purity and be 30% blue berry anthocyanin under 50 ℃, it is as the raw material of pharmaceutical production.
Claims (2)
1. the extracting and purifying method of a blue berry comprises extraction, removal of impurities, concentrated, drying step, it is characterized in that also having the ultrafiltration operation between concentrated and drying, wherein:
A, extraction: with concentration is 30%-80%, PH be ethanol and the blue berry pomace powder of 2-6 with 1: 1-1: 10 solid-liquid ratio mixes, 30 ℃-90 ℃ following refluxing extraction 0.5-2 hour, filter and collect filtrate and residue, mix with residue and identical solid-liquid ratio with the acidifying ethanolic soln of concentration again, under uniform temp refluxing extraction 0.5-2 hour again, filter and also collect filtrate, merge twice filtrate;
B, removal of impurities: A step gained merging filtrate under 0 ℃ of-4 ℃ of low temperature, was placed 12-24 hour, filtered with B;
C, concentrated: filtrate is concentrated at 50 ℃ of following reduction vaporizations, concentrate 10-12 hour;
D, ultrafiltration: the millipore filtration that with concentrated solution by the aperture is 0.45um and 0.22um degerms and high molecular weight protein to remove;
E, drying: after filtrate or elutriant removed most of ethanol, dry in 50 ℃ of-60 ℃ of vacuum.
2. the extracting and purifying method of blue berry according to claim 1, it is characterized in that: between ultrafiltration and drying step, also has the upper prop operation, described upper prop is meant: earlier filtrate is crossed macroporous adsorbent resin with the velocity flow of 1-3 times of column volume per hour, cross resin with the distilled water of 2-5 times of column volume with identical velocity flow then, the most of impurity of flush away; Cross resin with the ethanolic soln of the 60%-90% of 1-3 column volume with identical velocity flow again, the anthocyanin that adsorbs on the resin is eluted, collect elutriant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410022696 CN1279049C (en) | 2004-06-02 | 2004-06-02 | Extraction and purification of blue berry and its product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410022696 CN1279049C (en) | 2004-06-02 | 2004-06-02 | Extraction and purification of blue berry and its product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1583774A CN1583774A (en) | 2005-02-23 |
| CN1279049C true CN1279049C (en) | 2006-10-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200410022696 Expired - Fee Related CN1279049C (en) | 2004-06-02 | 2004-06-02 | Extraction and purification of blue berry and its product |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9969707B2 (en) | 2011-12-16 | 2018-05-15 | CENTRE DE RECHERCHE INDUSTRIELLE DU QUéBEC | Method for extracting anthocyanin derivatives from a plant source |
| CN114870427B (en) * | 2021-12-04 | 2023-11-03 | 黑龙江邦超生物科技有限公司 | Technological method and equipment for extracting and purifying blue berry functional substances by anaerobic method and supercharging method |
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- 2004-06-02 CN CN 200410022696 patent/CN1279049C/en not_active Expired - Fee Related
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Granted publication date: 20061011 Termination date: 20120602 |