CN103044569B - Wolfberry fruit extract containing matrimony vine acid and preparation method thereof - Google Patents
Wolfberry fruit extract containing matrimony vine acid and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of wolfberry fruit extract containing matrimony vine acid.Containing the matrimony vine acid of 1% ~ 10% and 2% ~ 20% lycium barbarum polysaccharide in described wolfberry fruit extract, the invention provides preparation method, comprise matrimony vine raw material reverse osmosis purified drinking water washed away floating dust, the lixiviate of reverse osmosis purified drinking water or heating extractions, filtration, absorption, wash-out, ultrafiltration, concentrate, sterilizing, spraying dry.The present invention is that the deep processing production of matrimony vine provides new qualifying point, to matrimony vine deep processed product Quality advance, and differentiates that the true and false quality band of product is helped, can produce far-reaching influence.Not only be conducive to Cleaning market but also be conducive to the interests of human consumer, promote the well-being of mankind health.The inventive method is suitable for suitability for industrialized production, has very large using value and social benefit.
Description
Technical field
The present invention relates to plant milk extract, be specifically related to the preparation method of plant milk extract, particularly relate to a kind of wolfberry fruit extract and the method thereof that contain matrimony vine acid from matrimony vine (Lycium chinense) extraction preparation.
Background technology
The healthy food that is beneficial to man is a lot, but matrimony vine is a kind of good vegetalitas protective foods, and the long property that its Clinical efficacy historifies is well-known.The traditional definition of China to matrimony vine function: invigorating the liver and kidney, beneficial vital essence, longue meat, improve complexion, improving eyesight is calmed the nerves, dispel the wind control void, promote longevity, effect of hard muscles and bones.Along with the development of modern science, scientists utilizes advanced science and technology to disclose the basic substance of matrimony vine validity.Find that it also has carotenoid, oligose, polymer glycopeptide, VITAMIN containing flavones, matrimony vine acid, taurine, trimethyl-glycine: B1, B2, C and E, protein, fat, amino acid, robust fibre and trace element etc.In today that people's living standard improves day by day, the health-care effect of matrimony vine widely receive by current masses, therefore, the deep processed product of relevant matrimony vine is also increasing in recent years.Matrimony vine originates in the northwest wide geographic area of China.The quality of deep processed product and the place of production and preserving type have very large relation, the inevitable quality that also can have influence on its deep processed product.But, at present for the requirement of wolfberry fruit extract, only using the polysaccharide component in wolfberry fruit extract as quality index, obviously with such one simply and not have a quality index of Enzyme specificity be the quality that is not enough to ensure matrimony vine deep processed product.The present inventor successfully invents the method for the exclusive chemical composition " matrimony vine acid " in preparation matrimony vine, and applied for Chinese patent (application number 2012105328009, a kind of method preparing high-purity lycium barbarum acid), and propose the Detection job index one of of matrimony vine acid composition as matrimony vine deep processed product.The present inventor has done further research on this basis and has found to have carried out content control to the matrimony vine acid in extract, can differentiate the index of true and false quality as matrimony vine deep processed product.Far-reaching influence will be played to matrimony vine process deeply industry.
Summary of the invention
Technical problem to be solved by this invention is in research and design wolfberry fruit extract except also containing matrimony vine acid containing except lycium barbarum polysaccharide.
The invention provides a kind of wolfberry fruit extract containing matrimony vine acid, containing the matrimony vine acid of 1% ~ 10% and 2% ~ 20% lycium barbarum polysaccharide in described wolfberry fruit extract.
Another object of the present invention there is provided the preparation method of the above-mentioned wolfberry fruit extract containing matrimony vine acid, and the method comprises the following steps:
(1) extract: matrimony vine (Lycium chinense) raw material reverse osmosis purified drinking water is washed away floating dust, then extract with reverse osmosis purified drinking water cold soaking or heating;
(2) original position is filtered or is assisted centrifugal clarification: lixiviate completes, and material filters through original position or centrifugal slagging-off obtains lixiviate feed liquid;
(3) filter of feed liquid essence or Plate Filtration: use secondary filter to filter or flame filter press filtering original position filtration or centrifugal auxiliary slagging-off gained feed liquid;
(4) ultrafiltration: cleaner liquid ultra-filtration membrane ultrafiltration is obtained by liquid and trapped fluid;
(5) by ion-exchange fiber post: by adding ion-exchange fiber post by liquid and cleaning with reverse osmosis purified drinking water after ultrafiltration;
(6) wash-out of ion-exchange fiber post: the ion-exchange fiber post elution that reverse osmosis purified drinking water is cleaned;
(7) concentrated: after collection step (5) elutriant is concentrated, then to merge vacuum concentration with the trapped fluid after step (4) ultrafiltration;
(8) ultra high temperature sterilization (UHTS): by above-mentioned concentrated solution by the sterilizing of ultra high temperature sterilization (UHTS) equipment;
(9) spraying dry: will above by ultrapasteurized concentrated solution with being spray dried to powder and get final product.
The weight ratio of described step (1) reverse osmosis purified drinking water and matrimony vine raw material is 8:1 ~ 16:1(W/W), preferred 12:1(W/W).Each 1 ~ 3 hour, preferably 1.5 hours.Extracting temperature 30 DEG C ~ 90 DEG C, preferably 80 DEG C.Extract twice under the same conditions.
Described reverse osmosis purified drinking water obtains by reverse osmosis purified drinking water is machine-processed, unit type is KYRO025TH-1, equipment meets (China national industry standard) HY/T068-2002 " tap water preparation system SRO series reverse osmosis equipment " standard, requirement that GB17324-2003 " bottle (bucket) fills purified drinking water hygienic standard " specifies that quality meets (CNS).
Step (2) is as obtained lixiviate feed liquid through centrifugal slagging-off, and centrifugal rotational speed is 1000 revs/min.
Step (3) as with Plate Filtration, then adds filtration medium talcum powder (consumption is one of percentage of raw material charging capacity) with 10 μm of filter clothes; Secondary filter filter sizes is 0.1 μm.
Step (4) is as obtained by liquid and trapped fluid with ultra-filtration membrane ultrafiltration; The aperture of ultra-filtration membrane is 5000D ~ 10000D, preferred 8000D.
Step (5) uses ion exchange column to be ZB-2 strongly basic anion ion exchange fibre post, described anion-exchange fibre post, before use, after the 1 molar sodium hydroxide solution process with one times of column volume, then spends reverse osmosis purified drinking water and cleans to neutrality; Step (4) gained filtrate with 1 cylinder accumulated amount/hour flow velocity add the anion-exchange fibre post after process, ion exchange column being washed till the limpid and pH of water outlet with reverse osmosis purified drinking water after adding feed liquid is 6 ~ 7.
0.2% hydrochloric acid soln, 0.5% formic acid solution or 0.5% acetum wash-out that step (6) ion-exchange fiber post adopts the reverse osmose pure-water of 1.2 ~ 1.5 times of column volumes to prepare, with 0.2 ~ 0.5 cylinder accumulated amount/hour flow velocity, preferably 0.2% hydrochloric acid soln was with the flow velocity of 0.2/ hour.
Step (6) elutriant is adopted vacuum concentration by step (7), repeatedly adds the operation of reverse osmosis purified drinking water reconcentration at-90 ~-95 MPa 50 ~ 60 DEG C.Add water three times, when being concentrated to Brix12, namely add reverse osmosis purified drinking water at every turn, amount of water is 1/2nd of original doses; Completing add water for three times concentrated after, when material is concentrated to Brix15, the trapped fluid adding step (4) continues to be concentrated into Brix20 ~ 26 and stops concentrated.
The concentrated solution of step (8) is by ultra high temperature sterilization (UHTS) equipment (120 ± 1 DEG C, motor frequency of utilization 25Hz) sterilizing.
The aseptic feed liquid spray drying device of step (9) is dry, and inlet temperature controls at 110 ~ 120 DEG C, and air outlet temperature controls at 85 ~ 90 DEG C.
The product that the inventive method obtains is tested the lycium barbarum polysaccharide testing method in the detection of matrimony vine acid and employing GB/T18672-2002 through HPLC external standard method respectively.Matrimony vine acid and 2% ~ 20% lycium barbarum polysaccharide of 1% ~ 10% should be contained in described wolfberry fruit extract.
The present invention has used the beneficiation technologies of matrimony vine acid, discloses the brand-new wolfberry fruit extract containing matrimony vine acid.Deep processing for matrimony vine is produced and is provided new quality control, to matrimony vine deep processed product Quality advance, and differentiates that the true and false quality of product brings very large help, produces far-reaching influence.The present invention had both been conducive to purifying wolfberry fruit extract market, and be conducive to again the interests of human consumer, promote the well-being of mankind health.Method provided by the invention is suitable for suitability for industrialized production, has very large using value and social benefit.
Embodiment
Embodiment 1.
Take Ningxia and produce dried fruit of lycium barbarum 10 kilograms, wash away floating dust by reverse osmosis purified drinking water shower.With reverse osmosis purified drinking water lixiviate twice, each 80KG of consumption, each static lixiviate 2 hours, extraction temperature 80 DEG C.The feed liquid that lixiviate obtains is filtered through original position.Merge the vat liquor smart filter membrane filtering of 0.1 μm.Cleaner liquid adopt 10000D ultrafiltration membrane treatment obtain after the trapped fluid after ultrafiltration and ultrafiltration by liquid two parts.Being added with after the process of one times of column volume 1 molar sodium hydroxide solution by liquid after ultrafiltration, then clean the OH to neutrality with reverse osmosis purified drinking water
-type ZB-2 strongly basic anion ion exchange fibre filling pillar, add flow velocity be 1 cylinder accumulated amount/hour.Ion exchange column is washed till water outlet with reverse osmosis purified drinking water after adding feed liquid limpid and and reach pH6 ~ 7.This ion-exchange fiber post again with 0.2% hydrochloric acid soln wash-out of 1.2 column volume reverse osmosis purified drinking waters preparation, flow rate control 0.2 cylinder accumulated amount/hour.Collect acidic effluent liquid and adopt vacuum concentration, vacuum concentration parameter is-90 ~-95 MPa 50 ~ 60 DEG C.Just add reverse osmosis purified drinking water when being concentrated to Brix12 at every turn, each amount of water is 1/2nd of original doses.After such repetitive operation three times, when material is finally concentrated to about Brix15, then add the trapped fluid after above-mentioned ultrafiltration, continue to be concentrated into Brix20 ~ 26 and stop concentrated releasing feed liquid.The material concentrated adopts the sterilizing of ultra high temperature sterilization (UHTS) equipment, then becomes the finished product with spray drying device spraying dry.Spraying dry inlet temperature controls at 110 ~ 120 DEG C, and air outlet temperature controls at 85 ~ 90 DEG C.Obtain dried powder 740g.
Detection content of medlar acid is: 9.3%; Lycium barbarum polysaccharide content is: 19.4%.(HPLC external standard method is to the lycium barbarum polysaccharide testing method in the detection of matrimony vine acid and employing GB/T18672-2002.）
Illustrate: the reverse osmosis purified drinking water that the present invention is used, be that the reverse osmosis purified drinking water of KYRO025TH-1 is machine-processed by unit type, equipment meets (China national industry standard) HY/T068-2002 " tap water preparation system SRO series reverse osmosis equipment " standard, requirement that GB17324-2003 " bottle (bucket) fills purified drinking water hygienic standard " specifies that quality meets (CNS).
Embodiment 2
Take Ningxia and produce dried fruit of lycium barbarum 10 kilograms, wash away floating dust by reverse osmosis purified drinking water shower.With reverse osmosis purified drinking water lixiviate twice, each 120KG of consumption, each static lixiviate 1.5 hours, extraction temperature 50 DEG C.The feed liquid that lixiviate obtains is all that original position filters gained.Merge vat liquor flame filter press filtering and use flocculating aids talcum powder 0.1 kilogram.Cleaner liquid adopt 5000D ultrafiltration membrane treatment obtain after the trapped fluid after ultrafiltration and ultrafiltration by liquid two parts.After ultrafiltration by liquid add processed one-tenth OH-type ZB-2 strongly basic anion ion exchange fibre filling pillar (the method process according to embodiment 1), pass into flow velocity be 1 cylinder accumulated amount/hour.Ion exchange column is washed till water outlet with reverse osmosis purified drinking water after adding feed liquid limpid and and reach pH6 ~ 7.The 0.5% formic acid solution wash-out that the ion-exchange fiber post adding feed liquid afterwash is prepared with 1.5 column volume reverse osmosis purified drinking waters, flow rate control 0.2 cylinder accumulated amount/hour.Acid de-liquid is washed in collection.Acidic effluent liquid adopts vacuum concentration, and vacuum concentration parameter is-90 ~-95 MPa 50 ~ 60 DEG C.Just add reverse osmosis purified drinking water when being concentrated to Brix12 at every turn, each amount of water is 1/2nd of original doses.After such repetitive operation three times, be mixed into previous ultra-filter retentate when material is finally concentrated to about Brix15 and continue to be concentrated into Brix20 ~ 26 stopping concentrated releasing feed liquid.The material concentrated adopts the sterilizing of ultra high temperature sterilization (UHTS) equipment, then becomes the finished product with spray drying device spraying dry.Spraying dry inlet temperature controls at 110 ~ 120 DEG C, and air outlet temperature controls at 85 ~ 90 DEG C.Obtain dried powder 1970g.Detection content of medlar acid is: 3.1%; Lycium barbarum polysaccharide content is: 6.8%.(HPLC is to the lycium barbarum polysaccharide testing method in the detection of matrimony vine acid and employing GB/T18672-2002.）
Embodiment 3.
Take Ningxia and produce dried fruit of lycium barbarum 10 kilograms, wash away floating dust by reverse osmosis purified drinking water shower.With reverse osmosis purified drinking water lixiviate twice, each 150KG of consumption, each static lixiviate 3 hours, extraction temperature 30 DEG C.The feed liquid that lixiviate obtains filters gained through original position.Merge the soaked extracting solution smart filter membrane filtering of 0.1 μm.Cleaner liquid adopt 8000D ultrafiltration membrane treatment obtain after the trapped fluid after ultrafiltration and ultrafiltration by liquid two parts.After ultrafiltration by liquid add processed one-tenth OH-type ZB-2 strongly basic anion ion exchange fibre filling pillar (the method process according to embodiment 1), pass into flow velocity be 1 cylinder accumulated amount/hour.Ion exchange column is washed till water outlet with reverse osmosis purified drinking water after adding feed liquid pure and and reach pH6 ~ 7.The 0.5% acetum wash-out that the logical ion-exchange fiber post adding feed liquid afterwash is prepared with 1.2 column volume reverse osmosis purified drinking waters, flow rate control 0.2 cylinder accumulated amount/hour.Acid de-liquid is washed in collection.Acidic effluent liquid adopts vacuum concentration, and vacuum concentration parameter is-90 ~-95 MPa 50 ~ 60 DEG C.Just add reverse osmosis purified drinking water when being concentrated to Brix12 at every turn, each amount of water is 1/2nd of original doses.After such repetitive operation three times, be mixed into previous ultra-filter retentate when material is finally concentrated to about Brix15 and continue to be concentrated into Brix20 ~ 26 stopping concentrated releasing feed liquid.The material concentrated adopts the sterilizing of ultra high temperature sterilization (UHTS) equipment, then becomes the finished product with spray drying device spraying dry.Spraying dry inlet temperature controls at 110 ~ 120 DEG C, and air outlet temperature controls at 85 ~ 90 DEG C.Obtain dried powder 945g.Detection content of medlar acid is: 6.8%; Lycium barbarum polysaccharide content is: 13.5%(HPLC is to the lycium barbarum polysaccharide testing method in the detection of matrimony vine acid and employing GB/T18672-2002).
Claims (13)
1. the wolfberry fruit extract containing matrimony vine acid, is characterized in that, containing the matrimony vine acid of 1% ~ 10% and 2% ~ 20% lycium barbarum polysaccharide in described wolfberry fruit extract; Described wolfberry fruit extract is prepared by following method: (1) extracts: matrimony vine raw material reverse osmosis purified drinking water is washed away floating dust, then extracts with reverse osmosis purified drinking water cold soaking or heating;
(2) original position is filtered or is assisted centrifugal clarification: lixiviate completes, and material filters through original position or centrifugal slagging-off obtains lixiviate feed liquid;
(3) filter of feed liquid essence or Plate Filtration: use secondary filter to filter or flame filter press filtering original position filtration or centrifugal auxiliary slagging-off gained feed liquid;
(4) ultrafiltration: cleaner liquid ultra-filtration membrane ultrafiltration is obtained by liquid and trapped fluid;
(5) by ion-exchange fiber post: ultrafiltration is joined ion-exchange fiber post by liquid and cleans with reverse osmosis purified drinking water;
(6) wash-out of ion-exchange fiber post: the ion-exchange fiber post elution that reverse osmosis purified drinking water is cleaned;
(7) concentrated: after collection step (5) elutriant is concentrated, then to merge vacuum concentration with the trapped fluid after step (4) ultrafiltration;
(8) ultra high temperature sterilization (UHTS): by above-mentioned concentrated solution by the sterilizing of ultra high temperature sterilization (UHTS) equipment;
(9) spraying dry: will above by ultrapasteurized concentrated solution with being spray dried to powder and get final product.
2. the method for the wolfberry fruit extract of preparation as claimed in claim 1 containing matrimony vine acid, it is characterized in that, the method comprises the following steps:
(1) extract: matrimony vine raw material reverse osmosis purified drinking water is washed away floating dust, then extract with reverse osmosis purified drinking water cold soaking or heating;
(2) original position is filtered or is assisted centrifugal clarification: lixiviate completes, and material filters through original position or centrifugal slagging-off obtains lixiviate feed liquid;
(3) filter of feed liquid essence or Plate Filtration: use secondary filter to filter or flame filter press filtering original position filtration or centrifugal auxiliary slagging-off gained feed liquid;
(4) ultrafiltration: cleaner liquid ultra-filtration membrane ultrafiltration is obtained by liquid and trapped fluid;
(5) by ion-exchange fiber post: ultrafiltration is joined ion-exchange fiber post by liquid and cleans with reverse osmosis purified drinking water;
(6) wash-out of ion-exchange fiber post: the ion-exchange fiber post elution that reverse osmosis purified drinking water is cleaned;
(7) concentrated: after collection step (5) elutriant is concentrated, then to merge vacuum concentration with the trapped fluid after step (4) ultrafiltration;
(8) ultra high temperature sterilization (UHTS): by above-mentioned concentrated solution by the sterilizing of ultra high temperature sterilization (UHTS) equipment;
(9) spraying dry: will above by ultrapasteurized concentrated solution with being spray dried to powder and get final product.
3. preparation contains the method for the wolfberry fruit extract of matrimony vine acid according to claim 2, and it is characterized in that, the weight ratio of described step (1) reverse osmosis purified drinking water and matrimony vine raw material is 8:1 ~ 16:1; Each 1 ~ 3 hour; Extracting temperature 30 DEG C ~ 90 DEG C, extracts twice under the same conditions.
4. preparation contains the method for the wolfberry fruit extract of matrimony vine acid according to claim 3, and it is characterized in that, the weight ratio of described step (1) reverse osmosis purified drinking water and matrimony vine raw material is 12:1; Each 1.5 hours; Extracting temperature 80 DEG C, extracts twice under the same conditions.
5. preparation contains the method for the wolfberry fruit extract of matrimony vine acid according to claim 2, it is characterized in that, described step (2) obtains lixiviate feed liquid through centrifugal slagging-off, and centrifugal rotational speed is 1000 revs/min; When step (3) uses Plate Filtration, then use 10 μm of filter clothes, add filtration medium talcum powder; Amount of talc is one of percentage of matrimony vine acid starting material weight; Secondary filter filter sizes is 0.1 μm.
6. preparation contains the method for the wolfberry fruit extract of matrimony vine acid according to claim 2, it is characterized in that, described step (4) is as obtained by liquid and trapped fluid with ultra-filtration membrane ultrafiltration; The aperture of ultra-filtration membrane is 5000D ~ 10000D.
7. preparation contains the method for the wolfberry fruit extract of matrimony vine acid according to claim 6, it is characterized in that, described step (4) is as obtained by liquid and trapped fluid with ultra-filtration membrane ultrafiltration; The aperture of ultra-filtration membrane is 8000D.
8. preparation contains the method for the wolfberry fruit extract of matrimony vine acid according to claim 2, it is characterized in that, described step (5) uses ion exchange column to be ZB-2 strongly basic anion ion exchange fibre post, described anion-exchange fibre post, before use, after the 1 molar sodium hydroxide solution process with one times of column volume, then clean to neutrality with reverse osmosis purified drinking water; Step (4) gained filtrate with 1 cylinder accumulated amount/hour flow velocity add the anion-exchange fibre post after process, ion exchange column being washed till the limpid and pH of water outlet with reverse osmosis purified drinking water after adding feed liquid is 6 ~ 7.
9. preparation contains the method for the wolfberry fruit extract of matrimony vine acid according to claim 2, it is characterized in that, described step (6) ion-exchange fiber post adopts 0.2% hydrochloric acid soln, 0.5% formic acid solution or the 0.5% acetum wash-out of the reverse osmosis purified drinking water preparation of 1.2 ~ 1.5 times of column volumes, with 0.2 ~ 0.5 cylinder accumulated amount/hour flow velocity.
10. preparation contains the method for the wolfberry fruit extract of matrimony vine acid according to claim 9, it is characterized in that, described step (6) ion-exchange fiber post adopt 1.2 ~ 1.5 times of column volumes reverse osmosis purified drinking water preparation 0.2% hydrochloric acid soln wash-out, with 0.2 cylinder accumulated amount/hour flow velocity.
11. methods of wolfberry fruit extract of preparation containing matrimony vine acid according to claim 2, it is characterized in that, described step (7) adopts vacuum concentration step (6) elutriant, the operation of reverse osmosis purified drinking water reconcentration is added in triplicate at-90 ~-95 MPa 50 ~ 60 DEG C, when being concentrated to Brix12 at every turn, namely add reverse osmosis purified drinking water, amount of water is 1/2nd of original doses; After completing, when material is concentrated to Brix15, the trapped fluid adding step (4) continues to be concentrated into Brix20 ~ 26 and stops concentrated.
12. methods of wolfberry fruit extract of preparation containing matrimony vine acid according to claim 2, is characterized in that, the concentrated solution of described step (8) by the sterilizing of ultra high temperature sterilization (UHTS) equipment, temperature 120 ± 1 DEG C, motor frequency of utilization 25Hz.
13. methods of wolfberry fruit extract of preparation containing matrimony vine acid according to claim 2, it is characterized in that, the aseptic feed liquid spray drying device of described step (9) is dry, and inlet temperature controls at 110 ~ 120 DEG C, and air outlet temperature controls at 85 ~ 90 DEG C.
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| CN103323551A (en) * | 2013-06-25 | 2013-09-25 | 上海诺德生物实业有限公司 | Method for detecting content of medlar acid |
| CN106380498B (en) * | 2016-08-12 | 2018-11-23 | 上海诺德生物实业有限公司 | The preparation method of fructus lycii acid |
| CN108186797A (en) * | 2018-01-03 | 2018-06-22 | 上海诺德生物实业有限公司 | Remove wolfberry fruit extract of low-melting impurities and preparation method thereof |
| CN112370494A (en) * | 2020-11-23 | 2021-02-19 | 湖南金农生物资源股份有限公司 | Method for preparing medlar extract by combined fermentation |
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| CN1546054A (en) * | 2003-12-15 | 2004-11-17 | 上海中医药大学 | Application of wolfberry polyose in the preparation process of gastric ulcer treating medicine |
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| CN1546054A (en) * | 2003-12-15 | 2004-11-17 | 上海中医药大学 | Application of wolfberry polyose in the preparation process of gastric ulcer treating medicine |
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| Title |
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| Hypoglycemic and hypolipidemic effects and antioxidant activity of fruit extracts from Lycium barbarum;Qiong Luo et al.;《Life Sciences》;20041126;第76卷(第2期);第137–149页 * |
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