CN105753828A - Method for quickly extracting vitis amurensis rupr seed procyanidin - Google Patents

Method for quickly extracting vitis amurensis rupr seed procyanidin Download PDF

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Publication number
CN105753828A
CN105753828A CN201610202857.0A CN201610202857A CN105753828A CN 105753828 A CN105753828 A CN 105753828A CN 201610202857 A CN201610202857 A CN 201610202857A CN 105753828 A CN105753828 A CN 105753828A
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CN
China
Prior art keywords
vitis amurensis
procyanidin
semen vitis
extraction
extracting
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Application number
CN201610202857.0A
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Chinese (zh)
Inventor
董周永
李明月
徐敏
周亚军
任辉
田刚
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吉林大学
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Application filed by 吉林大学 filed Critical 吉林大学
Priority to CN201610202857.0A priority Critical patent/CN105753828A/en
Publication of CN105753828A publication Critical patent/CN105753828A/en

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulfur atoms in positions 2 or 4
    • C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulfur atoms in positions 2 or 4 with aryl radicals attached in position 2
    • C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulfur atoms in positions 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins

Abstract

The invention discloses a method for quickly extracting vitis amurensis rupr seed procyanidin.The method mainly includes the steps that vitis amurensis rupr seeds are separated from pomace after wine making, vitis amurensis rupr seed powder is obtained through freezing drying, smashing, degreasing and screening, a 50-70% ethanol aqueous solution is added as an extraction solvent according to the material-liquid ratio (g/mL) of 1:(15-25), 0.3-0.5% (w/v) sodium hexametaphosphate is added at the same time as an assistant agent, the mixture is evenly stirred, passes a high-voltage pulse electric field and is centrifuged under the conditions that the number of pulses is 8-12 and the intensity of the electric field is 20-30kV/cm, supernatant is subjected to vacuum concentration and freezing drying, and a target product is obtained.Compared with a conventional extraction method, the technology can obviously increase the procyanidin field, shorten extraction time and reduce energy consumption, and the high-voltage pulse electric field serves as a non-heat-processing technology so that the activity of procyanidin can be well kept.

Description

A kind of rapid extracting method of Semen Vitis Amurensis procyanidin

Technical field

The invention belongs to natural product active substance and extract field, be specifically related to a kind of make wine the separating obtained Semen Vitis Amurensis of skin slag from Vitis Amurensis the method for rapid extraction procyanidin.

Background technology

China is the country of unique large area artificial culture Vitis Amurensis in the world, aboundresources.Vitis Amurensis cold tolerance is strong, fruit Wine-making quality is excellent, being the primary raw material of the Northeast's wine industry, but a large amount of skin slags produced after fruit wine brewing are taken as except small part except fertilizer, feedstuff, major part is directly discarded, not only waste resource, and contaminated environment.Still containing substantial amounts of nutrition and active component in skin slag after Vitis Amurensis wine brewing, especially seed procyanidins content is extremely abundant.Therefore, procyanidin is extracted in research from the seed of Vitis Amurensis liquor-making byproduct can be effectively improved the value of Vitis Amurensis, has important economic and social benefit.

Procyanidin is efficient cofactor, is the Natural antioxidant that can effectively remove human free radical generally acknowledged in the world at present.Procyanidin wide material sources, safety height, bioavailability are good, suffer from being widely applied in fields such as food, medicine, cosmetics.

The main extracting method of current procyanidin has solvent extraction method, ultrasonic method, microwave method, supercritical CO2Extraction etc., but mostly there is the problems such as length consuming time, energy consumption is high, extraction impurity is more.It is a kind of brand-new non-thermal technology technology that the high-pressure pulse electric that this test adopts extracts procyanidin, it is that food liquid is placed in container as electrolyte, producing, by high-tension current, the processing method that electric pulse carries out acting on two sparking electrodes of container insulation, its extraction time is short, energy consumption is low, efficiency is high.Procyanidin with metal ion-chelant can be cemented out by sodium hexameta phosphate as assisted extraction agent, can further improve the yield of procyanidin by adding a small amount of sodium hexameta phosphate additional high pressure impulse electric field.

Summary of the invention

It is an object of the invention to provide the method for Semen Vitis Amurensis procyanidins after the extraction of a kind of sodium hexameta phosphate additional high pressure impulse electric field is made wine.With extraction process provided by the present invention, can significantly shorten extraction required time, increase the yield of procyanidin, provide Technical Reference for effectively utilizing of Vitis Amurensis liquor-making byproduct.

The present invention realizes by techniques below scheme,

The rapid extracting method of a kind of Semen Vitis Amurensis procyanidin, comprises the steps:

(1) Semen Vitis Amurensis separates skin slag after wine brewing, freeze-dried, pulverizes, and defat, sieve to obtain Semen Vitis Amurensis powder；

(2) Semen Vitis Amurensis powder step (1) obtained adds ethanol water as Extraction solvent, add sodium hexameta phosphate as adjuvant simultaneously；

(3) feed liquid that step (2) obtains is stirred, through peristaltic pump, pumped high-pressure pulse electric extraction element with certain flow rate；

(4) the complete feed liquid of extracting step (3) obtained is centrifuged, and supernatant vacuum concentrates, and reclaims ethanol, and namely concentrated solution lyophilization obtains target product.

Step of the present invention (1) is pulverize with mechanical crushing method, crosses 100 mesh sieves.

In step of the present invention (2), Semen Vitis Amurensis powder (g) is 1:(15～25 with the ratio of the ethanol water (mL) added), the volume fraction of ethanol water is 50～70%, and the addition of sodium hexameta phosphate is 0.3～0.5% (w/v).

In step of the present invention (3), flow velocity is 10mL/min, the condition of high-voltage pulse electric field device: umber of pulse is 8～12, and electric field intensity is 20～30kV/cm.

Centrifugal rotational speed in step of the present invention (4) is 4000r/min, time is 10～15min, and the temperature of centrifugal gained supernatant vacuum concentration is 40 DEG C, the solution lyophilization after concentration, drying condition: baking temperature is-80～-90 DEG C, vacuum is 5～15Pa.

Wherein, in described step (2), added sodium hexameta phosphate is the good adjuvant of extraction effect that the present invention filters out through the substantial amounts of institute of early stage.

Compared with prior art, the invention have the characteristics that:

(1) Vitis Amurensis is the primary raw material that the Northeast makes grape wine, and annual wine brewing produces substantial amounts of discarded Semen Vitis Amurensis, and its bioactive ingredients content is high, and cheap, steady sources, is the desirable feedstock extracting procyanidin；

(2) present invention adopts sodium hexameta phosphate additional high pressure impulse electric field to extract procyanidin first, it may be achieved the rapid extraction under room temperature condition, and technique is simple, safe and efficient；

(3) present invention is with Semen Vitis Amurensis after wine brewing for raw material, prepares procyanidin, can provide reference for the intensive processing of Vitis Amurensis liquor-making byproduct and higher value application.

Detailed description of the invention

Below in conjunction with embodiment, the present invention is described in further detail.

The rapid extracting method of a kind of Semen Vitis Amurensis procyanidin, flow process is as follows: vitis amurensis husk slag → pretreatment of raw material after wine brewing → sodium hexameta phosphate additional high pressure impulse electric field extracts → centrifugal → vacuum concentration → lyophilization → procyanidin crude extract.

Below for being embodied as step:

(1) pretreatment of raw material: separated from the skin slag after wine brewing by Semen Vitis Amurensis, lyophilization, pulverizes, defat, crosses 100 mesh sieves standby；

(2) sodium hexameta phosphate additional high pressure impulse electric field extracts: take a certain amount of Semen Vitis Amurensis powder, the ethanol water of 63% is added as Extraction solvent for 1:20 by solid-liquid ratio (g/mL), add the sodium hexameta phosphate of 0.4% (w/v) as adjuvant simultaneously, stir, through peristaltic pump, passing through umber of pulse for 10 with the flow pump of 10mL/min, the high-voltage pulse electric field device that electric field intensity is 25kV/cm extracts；

(3) centrifugal: by extracting feed liquid centrifugal 10min when 4000r/min, to take supernatant；

(4) vacuum concentration: by the vacuum concentration under 40 DEG C of conditions of centrifugal gained supernatant, be separately recovered ethanol and concentrated solution；

(5) lyophilization: by the solution after concentration under-18 DEG C of conditions after pre-freeze, temperature be-80～-90 DEG C, vacuum be 5～15Pa when lyophilization 12h, procyanidin yield is 9.5%.

The foregoing is only presently preferred embodiments of the present invention, invention is merely illustrative, not the spirit and scope of the present invention are defined.In this area, specialty artisans understand that, its technical scheme can be variously modified and revise without departing from the inventive concept of the premise, but broadly fall into protection scope of the present invention.

Claims (5)

1. the rapid extracting method of a Semen Vitis Amurensis procyanidin, it is characterised in that: step is as follows
(1) Semen Vitis Amurensis separates skin slag after wine brewing, freeze-dried, pulverizes, and defat, sieve to obtain Semen Vitis Amurensis powder；
(2) Semen Vitis Amurensis powder step (1) obtained adds ethanol water as Extraction solvent, add sodium hexameta phosphate as adjuvant simultaneously；
(3) feed liquid that step (2) obtains is stirred, through peristaltic pump, pumped high-pressure pulse electric extraction element with certain flow rate；
(4) the complete feed liquid of extracting step (3) obtained is centrifuged, and supernatant vacuum concentrates, and reclaims ethanol, and namely concentrated solution lyophilization obtains target product.
2. the rapid extracting method of a kind of Semen Vitis Amurensis procyanidin according to claim 1, it is characterised in that: step (1) is pulverize with mechanical crushing method, crosses 100 mesh sieves.
3. the rapid extracting method of a kind of Semen Vitis Amurensis procyanidin according to claim 1, it is characterized in that: in step (2), Semen Vitis Amurensis powder (g) is 1:(15～25 with the ratio of the ethanol water (mL) added), the volume fraction of ethanol water is 50～70%, and the addition of sodium hexameta phosphate is 0.3～0.5% (w/v).
4. the rapid extracting method of a kind of Semen Vitis Amurensis procyanidin according to claim 1, it is characterized in that: in step (3), flow velocity is 10mL/min, the condition of high-voltage pulse electric field device: umber of pulse is 8～12, electric field intensity is 20～30kV/cm.
5. the rapid extracting method of a kind of Semen Vitis Amurensis procyanidin according to claim 1, it is characterized in that: the centrifugal rotational speed in step (4) is 4000r/min, time is 10～15min, the temperature of centrifugal gained supernatant vacuum concentration is 40 DEG C, solution lyophilization after concentration, drying condition: baking temperature is-80～-90 DEG C, vacuum is 5～15Pa.
CN201610202857.0A 2016-04-01 2016-04-01 Method for quickly extracting vitis amurensis rupr seed procyanidin CN105753828A (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106614969A (en) * 2016-12-22 2017-05-10 李程程 Appetite stimulating fermented tea walnut cakes and preparation method thereof
CN106689305A (en) * 2016-12-22 2017-05-24 李程程 Bone paste and fresh milk walnut sweet cakes with decorative patterns, for promoting digestion, and making method of bone paste and fresh milk walnut sweet cakes
CN106720047A (en) * 2016-12-22 2017-05-31 李程程 A kind of enriching yin beauty treatment strong bone walnut cake and preparation method thereof
CN106720046A (en) * 2016-12-22 2017-05-31 李程程 A kind of nourishing the stomach appetizing the ancient philosophers's walnut cake and preparation method thereof
CN106720049A (en) * 2016-12-22 2017-05-31 李程程 One kind appetizing fermentation bone mud walnut cake and preparation method thereof
CN106720048A (en) * 2016-12-22 2017-05-31 李程程 A kind of anti-oxidant cheese's walnut cake and preparation method thereof of replenishing the calcium
CN106819021A (en) * 2016-12-22 2017-06-13 李程程 A kind of micro- sugared low fat shredded coconut stuffing walnut cake of beauty treatment and preparation method thereof
CN106819023A (en) * 2016-12-22 2017-06-13 李程程 A kind of milk fermentation honey walnut cake and preparation method thereof
CN106819022A (en) * 2016-12-22 2017-06-13 李程程 A kind of heat-clearing beauty treatment bone mud walnut cake and preparation method thereof
CN106857759A (en) * 2016-12-22 2017-06-20 李程程 A kind of stomach invigorating beauty treatment bone mud decorative pattern walnut cake and preparation method thereof
CN107552536A (en) * 2017-09-05 2018-01-09 贵州慧静生物科技有限公司 Grape wine waste residue integrated extraction technique

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105294636A (en) * 2015-11-16 2016-02-03 大兴安岭林格贝寒带生物科技股份有限公司 Preparation method of oligomeric proanthocyanidin

Patent Citations (1)

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CN105294636A (en) * 2015-11-16 2016-02-03 大兴安岭林格贝寒带生物科技股份有限公司 Preparation method of oligomeric proanthocyanidin

Non-Patent Citations (1)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106614969A (en) * 2016-12-22 2017-05-10 李程程 Appetite stimulating fermented tea walnut cakes and preparation method thereof
CN106689305A (en) * 2016-12-22 2017-05-24 李程程 Bone paste and fresh milk walnut sweet cakes with decorative patterns, for promoting digestion, and making method of bone paste and fresh milk walnut sweet cakes
CN106720047A (en) * 2016-12-22 2017-05-31 李程程 A kind of enriching yin beauty treatment strong bone walnut cake and preparation method thereof
CN106720046A (en) * 2016-12-22 2017-05-31 李程程 A kind of nourishing the stomach appetizing the ancient philosophers's walnut cake and preparation method thereof
CN106720049A (en) * 2016-12-22 2017-05-31 李程程 One kind appetizing fermentation bone mud walnut cake and preparation method thereof
CN106720048A (en) * 2016-12-22 2017-05-31 李程程 A kind of anti-oxidant cheese's walnut cake and preparation method thereof of replenishing the calcium
CN106819021A (en) * 2016-12-22 2017-06-13 李程程 A kind of micro- sugared low fat shredded coconut stuffing walnut cake of beauty treatment and preparation method thereof
CN106819023A (en) * 2016-12-22 2017-06-13 李程程 A kind of milk fermentation honey walnut cake and preparation method thereof
CN106819022A (en) * 2016-12-22 2017-06-13 李程程 A kind of heat-clearing beauty treatment bone mud walnut cake and preparation method thereof
CN106857759A (en) * 2016-12-22 2017-06-20 李程程 A kind of stomach invigorating beauty treatment bone mud decorative pattern walnut cake and preparation method thereof
CN107552536A (en) * 2017-09-05 2018-01-09 贵州慧静生物科技有限公司 Grape wine waste residue integrated extraction technique

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Application publication date: 20160713