CN101658290A - Method for extracting crabapple polyphenols from crabapple skin dregs - Google Patents
Method for extracting crabapple polyphenols from crabapple skin dregs Download PDFInfo
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- CN101658290A CN101658290A CN200910072937A CN200910072937A CN101658290A CN 101658290 A CN101658290 A CN 101658290A CN 200910072937 A CN200910072937 A CN 200910072937A CN 200910072937 A CN200910072937 A CN 200910072937A CN 101658290 A CN101658290 A CN 101658290A
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Abstract
The invention relates to a method for extracting crabapple polyphenols from crabapple skin dregs, which comprises the procedures of soaking of the dried and smashed crabapple skin dregs in ethanol solution, ultrasonic extraction, column chromatography separation and purification, rotary evaporation concentration, vacuum drying and the like, wherein, the polyphenols are extracted from the crabappleskin dregs soaked in the ethanol solution in an ultrasonic extraction device, the ultrasonic power is 250W, and the AB-8 macroporous resin column chromatography method is adopted for separation and purification. The crabapple polyphenols are powder products, and the content of the polyphenols is 65%-80%. Raw materials used for extracting the crabapple polyphenols by adopting the method are the crabapple skin dregs, thereby not only utilizing wastes, but also reducing environmental pollution; and the method has the advantages of time-saving property, energy conservation, high extraction rate of the polyphenols and no solvent residue, and can greatly improve the additional value and the comprehensive utilization efficiency of agricultural and sideline products. The method can solve the problems of long extraction time and low purity of the conventional method, and is easy to realize the industrial production.
Description
One, technical field
What the present invention relates to is the development and use of crabapple skin dregs, particularly be to be raw material with the accessory substance crabapple skin dregs in the Chinese pear-leaved crabapple inspissated juice production process, extract the method for preparing crabapple polyphenols.
Two, background technology
Crabapple skin dregs is the accessory substance in the processing of Chinese pear-leaved crabapple fruit juice, contains abundant polyphenols.A large amount of pomaces is taken as rubbish and abandons in the Chinese pear-leaved crabapple inspissated juice processing at present, has not only wasted resource but also contaminated environment.Crabapple polyphenols plays a part very important as the native compound of a class biologically active to human beings'health.Many polyphenol that studies show that have plurality of health care functions, as caries prevention, prevention hypertension, antitumor, anti-sudden change, antibacterial, to remove free radical, antioxidation and anti-ageing waiting for a long time, particularly its oxidation resistance be ascorbic 50 times, 20 times of vitamin E.Polyphenol also have disappear smelly, fresh-keeping, protect fragrant, protect look, prevent effect such as vitamin loss, can prevent the bad change of food quality.More to the research of plant polyphenol both at home and abroad, patent mainly concentrates on the preparation of Tea Polyphenols, apple polyphenol and grape seed polyphenols and uses.But do not see the patent and the Related product research report of relevant crabapple skin dregs polyphenol as yet.Be rich in polyphenol substance in the crabapple skin dregs, utilize crabapple polyphenols to be soluble in the character of ethanol, extract by ultrasonic wave, adopt column chromatography purification, from crabapple skin dregs, extract crabapple polyphenols, have the recovery rate height, avoided the loss of active component, the advantage of no solvent residue has solved the problem that conventional method extraction time is long, purity is low, is easy to suitability for industrialized production.
Three, summary of the invention
Summary of the invention:
The purpose of this invention is to provide a kind of method for preparing crabapple polyphenols of from crabapple skin dregs, extracting.
Above-mentioned purpose realizes by following technical scheme:
The preparation method of crabapple polyphenols, its composition comprises: get crabapple skin dregs, dry or 50～55 ℃ of oven dry down, after the described drying process, be ground into 80～100 orders, crabapple skin dregs is sent in the ultrasonic wave extractor, extracted crabapple polyphenols under 250W, extractant is 50%～75% ethanol, extraction time 20～30min, extract 50～55 ℃ of temperature, solid-liquid ratio 1: 5～1: 10 extracts 1～2 time.Collect and leach liquid, preliminary concentrating.AB-8 macroporous resin column chromatography method is adopted in separation and purification, and the gained eluent is concentrated through rotary evaporation again, vacuum drying, can obtain the crabapple polyphenols powder, its crabapple polyphenols content 65%～80%.
The preparation method of described crabapple polyphenols, described AB-8 macroporous resin column chromatography method, adopt wet method dress post (1.0 * 40cm), post bed height 30cm, the leachate that adds crabapple polyphenols with the flow velocity of 1mL/min, adsorb saturated after, with the washing of 2BV (bed volume) distilled water, to remove impurity such as adsorbed sugar of resin and water-soluble hemicellulose.Then with 60% ethanolic solution be eluted to colourless till, elution flow rate is 0.5mL/min, collects eluent, adopts Rotary Evaporators to reclaim ethanol.
The preparation method of described crabapple polyphenols, described concentrated parameter is: vacuum 0.075～0.09MPa, 50～55 ℃ of evaporating temperatures.
The preparation method of described crabapple polyphenols, described vacuum drying parameter is: vacuum 0.09MPa, 50～55 ℃ of temperature.
This technical scheme has following beneficial effect:
1. the present invention takes ultrasonic wave to extract, and ultrasonic extraction is compared with conventional solvent extraction, has short, advantages such as productive rate is high, mild condition of extraction time, helps suitability for industrialized production.
2. present technique is all carried out at low temperatures to extraction, purifying and the concentrated overall process of polyphenol in the crabapple skin dregs, and the chemical constitution of polyphenol is not had destruction.
3. technology of the present invention can obtain higher degree crabapple polyphenols product.Adopted macroreticular resin AB-8 that the crude extract of crabapple polyphenols is carried out separation and purification in the separation and purification process, it is good that it has selectivity, and adsorption rate is fast, is easy to resolve, and regeneration is handled simple, characteristics such as product purity height.Also comprised the optimal separation conditional parameter among the present invention: absorption and wash-out at normal temperatures, add the leachate of crabapple polyphenols with the flow velocity of 1mL/min, adsorb saturated after, wash with 2BV (bed volume) distilled water.Use 60% ethanol elution then, elution flow rate is 0.5mL/min.Test and improve through hundreds of inferior groping, the special process parameter that the present invention adopts improves the purity of crabapple polyphenols greatly.
4. technical costs of the present invention is lower, and the solvent that uses can all reclaim, and the product no solvent residue, for the suitability for industrialized production of crabapple polyphenols provides can be for the process route of implementing.
5. to extract the used raw material of polyphenol be crabapple skin dregs in the present invention, and these crabapple skin dregs usually can only be as feed or fertilizer, and its higher added value is not brought into play.The present invention provides new way for the utilization of crabapple skin dregs, and discarded object is fully utilized, and has reduced environmental pollution, brings bigger economic benefit also can for relevant processing enterprise.
Four, the specific embodiment
Embodiment 1: be the feedstock production crabapple polyphenols with the crabapple skin dregs.
Get the dried crabapple skin dregs of 80 orders, in the ultrasonic wave extractor, extract crabapple polyphenols down in the 250W ultrasonic power, extractant is 50% ethanol, and extraction time 30min extracts 50 ℃ of temperature, and solid-liquid ratio 1: 5 extracts 2 times.Collect and leach liquid, preliminary concentrating.
AB-8 macroporous resin column chromatography method is adopted in separation and purification, adopt wet method dress post (1.0 * 40cm), post bed height 30cm adds the leachate of crabapple polyphenols with the flow velocity of 1mL/min, adsorb saturated after, with 2
The washing of BV (bed volume) distilled water is to remove impurity such as adsorbed sugar of resin and water-soluble hemicellulose.Then with 60% ethanolic solution be eluted to colourless till, elution flow rate is 0.5mL/min, collects eluent.
The gained eluent after 50 ℃ of rotary evaporations of evaporating temperature concentrate, adopts vacuum 0.09MPa again through vacuum 0.09MPa, and 50 ℃ of vacuum drying of temperature can obtain the crabapple polyphenols powder, and its crabapple polyphenols content is 65%.
Embodiment 2: be the feedstock production crabapple polyphenols with the crabapple skin dregs.
Get the dried crabapple skin dregs of 100 orders, in the ultrasonic wave extractor, extract crabapple polyphenols down in the 250W ultrasonic power, extractant is 60% ethanol, and extraction time 25min extracts 55 ℃ of temperature, and solid-liquid ratio 1: 8 extracts 2 times.Collect and leach liquid, preliminary concentrating.
Separation and purification is with embodiment 1.
The gained eluent after 55 ℃ of rotary evaporations of evaporating temperature concentrate, adopts vacuum 0.09MPa again through vacuum 0.09MPa, and 55 ℃ of vacuum drying of temperature can obtain the crabapple polyphenols powder, and its crabapple polyphenols content is 72%.
Embodiment 3: be the feedstock production crabapple polyphenols with the crabapple skin dregs.
Get the dried crabapple skin dregs of 80 orders, in the ultrasonic wave extractor, extract crabapple polyphenols down in the 250W ultrasonic power, extractant is 75% ethanol, and extraction time 30min extracts 50 ℃ of temperature, and solid-liquid ratio 1: 10 extracts 1 time.Collect and leach liquid, preliminary concentrating.
Separation and purification is with embodiment 1.
The gained eluent after 55 ℃ of rotary evaporations of evaporating temperature concentrate, adopts vacuum 0.09MPa again through vacuum 0.075MPa, and 50 ℃ of vacuum drying of temperature can obtain the crabapple polyphenols powder, and its crabapple polyphenols content is 80%.
Claims (4)
1. the preparation method of a crabapple polyphenols, its composition comprises: crabapple skin dregs, dry or 50～55 ℃ of oven dry down, and it is characterized in that: after the described drying process, be ground into 80～100 orders, crabapple skin dregs is sent in the ultrasonic wave extractor, extracted crabapple polyphenols under 250W, extractant is 50%～75% ethanol, extraction time 20～30min, extract 50～55 ℃ of temperature, solid-liquid ratio 1: 5～1: 10 extracts 1～2 time.Collect and leach liquid, preliminary concentrating.AB-8 macroporous resin column chromatography method is adopted in separation and purification, and the gained eluent is concentrated through rotary evaporation again, vacuum drying, can obtain the crabapple polyphenols powder, its polyphenol content 65%～80%.
2. the preparation method of crabapple polyphenols according to claim 1, it is characterized in that: described AB-8 macroporous resin column chromatography method, adopt wet method dress post (1.0 * 40cm), post bed height 30cm, the leachate that adds crabapple polyphenols with the flow velocity of 1mL/min, adsorb saturated after, with the washing of 2BV (bed volume) distilled water, to remove impurity such as adsorbed sugar of resin and water-soluble hemicellulose.Then with 60% ethanolic solution be eluted to colourless till, elution flow rate is 0.5mL/min, collects eluent, adopts Rotary Evaporators to concentrate and reclaims ethanol.
3. the preparation method of crabapple polyphenols according to claim 1 and 2, it is characterized in that: described concentrated parameter is: vacuum 0.075～0.09MPa, 50～55 ℃ of evaporating temperatures.
4. the preparation method of crabapple polyphenols according to claim 1, it is characterized in that: described vacuum drying parameter is: vacuum 0.09MPa, 50～55 ℃ of temperature.
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| CN2009100729379A CN101658290B (en) | 2009-09-21 | 2009-09-21 | Method for extracting crabapple polyphenols from crabapple skin dregs |
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| CN2009100729379A CN101658290B (en) | 2009-09-21 | 2009-09-21 | Method for extracting crabapple polyphenols from crabapple skin dregs |
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| CN101658290A true CN101658290A (en) | 2010-03-03 |
| CN101658290B CN101658290B (en) | 2012-07-04 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102178140A (en) * | 2010-12-01 | 2011-09-14 | 李良 | Fresh crab granatum health care fruit jelly |
| CN103169033A (en) * | 2013-04-17 | 2013-06-26 | 江苏省农业科学院 | Extraction process of strawberry phenol substances |
| CN103224538A (en) * | 2013-04-22 | 2013-07-31 | 华南理工大学 | Method for extracting grape skin residue polyphenols by synergy of ultrasound and pulsed electric field |
| CN104906154A (en) * | 2015-05-16 | 2015-09-16 | 吉林大学 | Method for ultrasonic-assisted extraction of polyphenol substances from new zealand spinach |
| CN113416739A (en) * | 2021-06-24 | 2021-09-21 | 黑龙江八一农垦大学 | Application of Saccharomyces rouxii gene in improving yield of HDMF (high-density multi-ferule) produced by microorganisms |
| CN115363214A (en) * | 2022-09-22 | 2022-11-22 | 江西省蚕桑茶叶研究所(江西省经济作物研究所) | Preparation method of honey-fried mulberry leaves |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1095616A (en) * | 1993-10-24 | 1994-11-30 | 李伟 | Fructus Mali Asiaticae diarrhea and preparation method thereof |
| CN1270627C (en) * | 2002-04-04 | 2006-08-23 | 林开中 | Freeze dried and antistaled multi-taste fruit and its preparing process |
-
2009
- 2009-09-21 CN CN2009100729379A patent/CN101658290B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102178140A (en) * | 2010-12-01 | 2011-09-14 | 李良 | Fresh crab granatum health care fruit jelly |
| CN102178140B (en) * | 2010-12-01 | 2013-01-16 | 李良 | Fresh crab granatum health care fruit jelly |
| CN103169033A (en) * | 2013-04-17 | 2013-06-26 | 江苏省农业科学院 | Extraction process of strawberry phenol substances |
| CN103224538A (en) * | 2013-04-22 | 2013-07-31 | 华南理工大学 | Method for extracting grape skin residue polyphenols by synergy of ultrasound and pulsed electric field |
| CN103224538B (en) * | 2013-04-22 | 2016-01-20 | 华南理工大学 | A kind of supersonic synergic pulsed electrical field extracts the method for grape skin polyphenol |
| CN104906154A (en) * | 2015-05-16 | 2015-09-16 | 吉林大学 | Method for ultrasonic-assisted extraction of polyphenol substances from new zealand spinach |
| CN104906154B (en) * | 2015-05-16 | 2018-04-03 | 吉林大学 | The method that ultrasonic assistant extracts polyphenols from New Zealand spinach |
| CN113416739A (en) * | 2021-06-24 | 2021-09-21 | 黑龙江八一农垦大学 | Application of Saccharomyces rouxii gene in improving yield of HDMF (high-density multi-ferule) produced by microorganisms |
| CN115363214A (en) * | 2022-09-22 | 2022-11-22 | 江西省蚕桑茶叶研究所(江西省经济作物研究所) | Preparation method of honey-fried mulberry leaves |
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| CN101658290B (en) | 2012-07-04 |
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