CN101434973B - Process for extracting anthocyanidin in blackcurrant by aqueous enzymatic method - Google Patents
Process for extracting anthocyanidin in blackcurrant by aqueous enzymatic method Download PDFInfo
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Abstract
The invention discloses a process which uses an aqueous enzymatic method to extract anthocyanidin from blackcurrant. The fresh blackcurrant fruit is taken as raw material and then crushed, later purified water and pectinase are added into mashed fruit; by centrifugal separation after enzymatic hydrolysis, primary filtrate and peel residue are obtained; after the peel residue is extracted by acid solution and undergoes centrifugal separation, secondary filtrate is obtained; later the primary filtrate and the secondary filtrate are mixed and concentrated into concentration liquid under low temperature and vacuum state; and a resin column is attached on the concentration liquid, after elution with the acidic alcohol solution, low-temperature vacuum concentration and spray drying, a finished product of dry anthocyanidin powder is obtained. The invention effectively solves the problems of the existing extraction technology of the anthocyanidin of the blackcurrant that the process is complex, the energy consumption is large and the cost is high. The invention has the advantages of simple method, low cost, high anthocyanidin extraction rate, mild reaction condition, and low pollution degree to ecological environment, and is a new process for extracting the anthocyanidin from the blackcurrant, being worth of popularization.
Description
Technical field
The present invention relates to a kind of is the production technique that raw material extracts cyanidin(e) with the black currant, belongs to field of biochemical separation and purifying technology.
Background technology
Black currant (Ribes nigrum L.) has another name called black bean fruit, formal name used at school black-current (black currant), fruit for the sub-platymiscium in Saxifragaceae (saxifrage) the tea foot of a hill or mountain, belong to perennial undershrub, mainly be distributed in the more cold and cool area of Northern Hemisphere weather, have many countries to abound with black currant, China producing region mainly is distributed in the Northwest, northeast.Fruit black, subsphaeroidal, sweet and sour, delicate fragrance, nutritious, can be made into products such as refreshment drink, fruit wine, essence after the processing.Be rich in phenolic compound in the black currant fruit; main component is a cyanidin(e); anti-cancer, improve eyesight, control of diabetes, improvement circulation, control inflammation and comprise aspect the underdrive effect in the general astogeny process of disease, forgetful, acrobatics and tumblings effective in cure; especially to cardiovascular very strong provide protection arranged; and this cyanidin(e) is a water colo(u)r; can fully be absorbed by human body, thereby improve its bioavailability greatly.
The method that general cyanidin(e) extracts in the document is a lot, and extraction solvent commonly used has water, sour water, ethanol or methanol solution etc.But specific to the black currant cyanidin(e), research for black currant both at home and abroad focuses mostly in processing such as fruit juice, jam, or unsaturated fatty acids in the seed of black currant extracted, report to the black currant functional study is in the majority, few to the report that the separation of its functional component cyanidin(e) is purified, for example open day be that the patent document that November 16, publication number in 2005 are CN 1696261A discloses a kind of method with polyunsaturated fatty acid and carboxylate thereof in the urea inclusion method enrichment seed of black currant oil.Zhao Xinhuai etc. are to extract haematochrome with ethanol or water from the black currant pomace at " foodstuffs industry science and technology " 1998 the 2nd interim extraction and purifications of reporting black currant pomace haematochrome, through the absorption of ion exchange resin, recyclable about 86% pigment.Li Yanwei etc. " food and fermentation industries " nineteen ninety the 2nd interim the report from black currant juice and pomace extract haematochrome, then be with rare ethanol-extracted.
The problem that aforesaid method exists is: have a large amount of pectin substances in the black currant fruit, berry generally carries out the fragmentation back and extracts pigment, but the pulp material system viscosity after the Mechanical Crushing is very big, be difficult to by squeezing direct extraction fruit juice, because its crushing juice rate is very low, the operation easier of follow-up discharging and filtration operation is also very big, complex process; If use a large amount of organic solvent extraction, then can strengthen production cost; Extract and under the pyritous condition, carry out pigment, can strengthen energy consumption on the one hand, on the other hand the stability of destructible pigment again.
Summary of the invention
The present invention provides the technology of cyanidin(e) in the aqueous enzymatic extraction black currant that a kind of method is simple, with low cost, the cyanidin(e) extraction yield is high for the problem that solves present black currant cyanidin(e) extractive technique existence.
The present invention reaches the concrete technical scheme that above-mentioned technical purpose adopts to be: the technology of cyanidin(e) in a kind of aqueous enzymatic extraction black currant comprises following steps:
A. be raw material with the black currant fresh fruit, through after the fragmentation, in pulp, add purified water and polygalacturonase, mix, centrifugation behind the enzymolysis gets just filtrate and peel residue, described purified water consumption is 20～100% of a pulp weight, the polygalacturonase consumption is 0.03～0.10% of a pulp weight, and hydrolysis temperature is 40～55 ℃, and enzymolysis time is 1.5～5h.The present invention uses enzyme solution, with the black currant fresh fruit is raw material, through broken back (then thawing earlier) as adopting freezing fruit, add polygalacturonase and carry out enzymolysis, pectin substance in the black currant pulp is effectively decomposed, reduced pulp viscosity, effective constituent is separated out to greatest extent, help operations such as the extraction of back and separation, for cyanidin(e) extracts the good condition of having created.Hydrolysis temperature is too high, though enzymolysis speed is accelerated, has accelerated the inactivation of polygalacturonase greatly, therefore should control suitable hydrolysis temperature.
B. peel residue is extracted the back centrifugation with acid solution, get time filtrate, described acid solution is 0.1%～0.3% aqueous citric acid solution, consumption is 4～20 times of described peel residue weight, the extraction time of peel residue is 2～4 times, and extraction time is each 1～3h, and extracting temperature is 40～50 ℃.It is more abundant to use acid solution that cyanidin(e) is extracted, thereby improves extraction yield, and peel residue can extract cyanidin(e) to greatest extent through extracting for several times, and simultaneously, remaining peel residue can be used as the raw material that extracts seed of black currant oil.
C. first filtrate is reached time filtrate mixing back cryogenic vacuum and concentrate, the temperature of described cryogenic vacuum concentration process is controlled at 55～60 ℃, gets concentrated solution, and the solid content of concentrated solution is controlled at 0.5～2% of its weight.Because cyanidin(e) easily decomposes during high temperature, therefore, here we adopt the spissated mode of cryogenic vacuum, and suitable low temperature can guarantee that cyanidin(e) can not be decomposed.Polymeric adsorbent has certain exchange capacity, under lower concentration, carries out usually, and cyanidin(e) excessive concentration in the upper prop liquid, then resin is revealed fast; Simultaneously, must make solid-liquid that arranged sufficient duration of contact mutually in the absorption exchange process, if flow velocity is too fast, resin and last fluid injection have little time exchange, also leakage phenomenon can take place, and consider the requirement of enhancing productivity, should select suitable last column liquid concentration, i.e. the suitable solid content of control.
D. with adsorption resin column on the concentrated solution, behind the acid purified water flushing resin column, use the acid ethanol solution wash-out, get elutriant, described polymeric adsorbent is a macroporous adsorbent resin, its model is D101, before using is 1.0～3.0 aqueous citric acid solution through post with the pH value, carries out acidification, column flow rate is 1～3 times of column volume per hour on the described concentrated solution, the pH value of described acid purified water is 1.0～3.0, and consumption is 2～6 times of column volumes, and flow velocity is 1～3 times of column volume per hour; Described acid ethanol solution is that the pH value is 1.0～3.0 60%～75% aqueous ethanolic solution, and elution flow rate is 0.5～2 times of column volume per hour, and elution volume is 1.5～3 times of column volumes.After the acidified processing of polymeric adsorbent, cyanidin(e) can be adsorbed in the resin column, thereby makes cyanidin(e) obtain wash-out in acid ethanol solution.Using acid purifying washing post, is the water-soluble impurity that adsorbs in the resin in order to remove.
E. the elutriant cryogenic vacuum is concentrated, get hyper-concentration liquid, the solid content of hyper-concentration liquid is controlled at 15～35% of its weight, with the hyper-concentration liquid spraying drying, cyanidin(e) dry powder gets product, during the hyper-concentration liquid spraying drying, its intake air temperature is controlled at 165～175 ℃, and the air outlet temperature is controlled at 85～95 ℃.The vacuum-drying required time is long, and temperature is higher, and cyanidin(e) can be destroyed, and therefore, we adopt spray-dired mode to prepare cyanidin(e) dry powder, can enhance productivity like this, guarantees quality product.The solid content of hyper-concentration liquid is low excessively, spraying drying length consuming time, and solid content is too high, is unfavorable for spray-dired feed operation, therefore should control suitable solid content.
Essence effect of the present invention is: complex process, energy consumption that it has solved present black currant cyanidin(e) extractive technique existence effectively reach the high problem of cost greatly, the inventive method is simple, with low cost, cyanidin(e) extraction yield height and reaction conditions gentleness, pollution level to ecotope is low, is the novel process of cyanidin(e) in a kind of extraction black currant that is worthy to be popularized.
Embodiment
Below by embodiment, the embodiment of technical solution of the present invention is further described.
Embodiment 1
With 2kg black currant fresh fruit is raw material, through after the fragmentation, adds the purified water of pulp weight 20% in pulp, is warming up to 40 ℃, adds the polygalacturonase of pulp weight 0.03% then, stir, and insulation 5h, centrifugation behind the enzymolysis gets just filtrate and peel residue.Peel residue repeats to extract 4 times through 0.1% aqueous citric acid solution, and the consumption of aqueous citric acid solution is 4 times of peel residue weight, and extraction time is each 1h, and extracting temperature is 40 ℃.The extracting solution centrifugation gets time filtrate.First filtrate and time filtrate mixing back cryogenic vacuum are concentrated, and its temperature is controlled at 55～60 ℃, and being concentrated into solid content is 2% concentrated solution.Adopting the D101 macroporous adsorptive resins, before using is 1.0 aqueous citric acid solution through post with the pH value, carries out acidification.With the concentrated solution upper prop, flow velocity is 1 times of column volume per hour, with the pH value 2 times of column volumes of acid purified water flushing of 1.0, flow velocity is 1 times of column volume per hour, use then that the pH value is 1.0, the acidic ethanol aqueous solution wash-out of ethanol content 60%, elution flow rate is 2 times of column volumes per hour, and elution volume is 3 times of column volumes.Elutriant concentrates through cryogenic vacuum, and its temperature is controlled at 55～60 ℃, is concentrated into solid content and is 15% hyper-concentration liquid, and with the hyper-concentration liquid spraying drying, its intake air temperature is controlled at 165 ℃, and the air outlet temperature is controlled at 85 ℃, cyanidin(e) powder 25.0g.After testing, cyanidin(e) content is 25.3%, and it is 90.4% that cyanidin(e) extracts refining transformation efficiency.
Embodiment 2
Get black currant fresh fruit 20kg,, pulp is put in the extraction flask, add the purified water of pulp weight 60% through after the fragmentation, be warming up to 45 ℃, add the polygalacturonase of pulp weight 0.06% then, stir, insulation 3h, centrifugation behind the enzymolysis gets just filtrate and peel residue.Peel residue repeats to extract 3 times through 0.2% aqueous citric acid solution, and the consumption of aqueous citric acid solution is 12 times of peel residue weight, and extraction time is 2h, and extracting temperature is 45 ℃.The extracting solution centrifugation gets time filtrate.First filtrate and time filtrate are mixed the back cryogenic vacuum concentrate, its temperature is controlled at 55～60 ℃, is concentrated into solid content and is 1% concentrated solution.Adopting the D101 macroporous adsorptive resins, before using is 2.0 aqueous citric acid solution through post with the pH value, carries out acidification.With the concentrated solution upper prop, flow velocity is 2 times of column volumes per hour, with the pH value 4 times of column volumes of acid purified water flushing of 2.0, flow velocity is 2 times of column volumes per hour, use that the pH value is 2.0, the acidic ethanol aqueous solution wash-out of ethanol content 70%, elution flow rate is 1 times of column volume per hour, and elution volume is 2 times of column volumes.Elutriant concentrates through cryogenic vacuum, and its temperature is controlled at 55～60 ℃, is concentrated into solid content and is 25% hyper-concentration liquid, and with the hyper-concentration liquid spraying drying, its intake air temperature is controlled at 170 ℃, and the air outlet temperature is controlled at 90 ℃, cyanidin(e) powder 245g.After testing, cyanidin(e) content is 25.8%, and it is 90.3% that cyanidin(e) extracts refining transformation efficiency.
Embodiment 3
Get the freezing fruit 100kg of black currant,, add the purified water of pulp weight 100% through thawing, after the fragmentation, pulp being put in the extraction flask, be warming up to 50 ℃, add the polygalacturonase of pulp weight 0.1% then, stir, insulation 1.5h, centrifugation behind the enzymolysis gets just filtrate and peel residue.Peel residue repeats to extract 2 times through 0.3% aqueous citric acid solution, and the consumption of aqueous citric acid solution is 20 times of peel residue, and extraction time is each 3h, and extracting temperature is 50 ℃.The extracting solution centrifugation gets time filtrate.First filtrate and time filtrate are mixed the back cryogenic vacuum concentrate, its temperature is controlled at 55～60 ℃, is concentrated into solid content and is 0.5% concentrated solution.Adopting the D101 macroporous adsorptive resins, before using is 3.0 aqueous citric acid solution through post with the pH value, carries out acidification.With the concentrated solution upper prop, flow velocity is 3 times of column volumes per hour, with the pH value 6 times of column volumes of acid purified water flushing of 3.0, flow velocity is 3 times of column volumes per hour, use that the pH value is 3, the acidic ethanol aqueous solution wash-out of ethanol content 75%, elution flow rate is 0.5 times of column volume per hour, and elution volume is 1.5 times of column volumes.Elutriant concentrates through cryogenic vacuum, and its temperature is controlled at 55～60 ℃, is concentrated into solid content and is 35% hyper-concentration liquid, and with the hyper-concentration liquid spraying drying, its intake air temperature is controlled at 175 ℃, and the air outlet temperature is controlled at 95 ℃, cyanidin(e) powder 1.25kg.After testing, cyanidin(e) content is 25.2%, and it is 90.0% that cyanidin(e) extracts refining transformation efficiency.
Claims (1)
1. the technology of cyanidin(e) in the aqueous enzymatic extraction black currant, its feature comprises following steps:
A. be raw material with the black currant fresh fruit, through after the fragmentation, in pulp, add purified water and polygalacturonase, mix, centrifugation behind the enzymolysis gets just filtrate and peel residue, described purified water consumption is 20～100% of a pulp weight, the polygalacturonase consumption is 0.03～0.10% of a pulp weight, and hydrolysis temperature is 40～55 ℃, and enzymolysis time is 1.5～5h;
B. peel residue is extracted the back centrifugation with acid solution, get time filtrate, described acid solution is 0.1%～0.3% aqueous citric acid solution, consumption is 4～20 times of described peel residue weight, the extraction time of peel residue is 2～4 times, and extraction time is each 1～3h, and extracting temperature is 40～50 ℃;
C. first filtrate is reached time filtrate mixing back cryogenic vacuum and concentrate, the temperature of described cryogenic vacuum concentration process is controlled at 55～60 ℃, gets concentrated solution, and the solid content of concentrated solution is controlled at 0.5～2% of its weight;
D. with adsorption resin column on the concentrated solution, behind the acid purified water flushing resin column, use the acid ethanol solution wash-out, get elutriant, described polymeric adsorbent is a macroporous adsorbent resin, its model is D101, before using is 1.0～3.0 aqueous citric acid solution through post with the pH value, carries out acidification, column flow rate is 1～3 times of column volume per hour on the described concentrated solution, the pH value of described acid purified water is 1.0～3.0, and consumption is 2～6 times of column volumes, and flow velocity is 1～3 times of column volume per hour; Described acid ethanol solution is that the pH value is 1.0～3.0 60%～75% aqueous ethanolic solution, and elution flow rate is 0.5～2 times of column volume per hour, and elution volume is 1.5～3 times of column volumes;
E. the elutriant cryogenic vacuum is concentrated, get hyper-concentration liquid, the solid content of hyper-concentration liquid is controlled at 15～35% of its weight, with the hyper-concentration liquid spraying drying, cyanidin(e) dry powder gets product, during the hyper-concentration liquid spraying drying, its intake air temperature is controlled at 165～175 ℃, and the air outlet temperature is controlled at 85～95 ℃.
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| CN102731463B (en) * | 2011-12-25 | 2014-11-19 | 大兴安岭林格贝有机食品有限责任公司 | Method for purifying anthocyanins in ribes nigrum |
| CN102775454A (en) * | 2012-08-06 | 2012-11-14 | 宁波杰顺生物科技有限公司 | Extractive of blackcurrant fruit anthocyanin |
| CN102993768B (en) * | 2012-12-21 | 2014-12-24 | 新疆科宇科技有限公司 | Blackcurrant pigment extract and production method thereof |
| CN104961783B (en) * | 2015-04-17 | 2018-07-10 | 浙江惠松制药有限公司 | A kind of effective extraction anthocyanidin and the method for anthocyanin |
| CN106616131B (en) * | 2016-11-16 | 2020-03-13 | 沈阳农业大学 | Preparation method of aronia melanocarpa non-concentrated reduced fruit juice |
| CN112314945A (en) * | 2020-10-29 | 2021-02-05 | 安徽卡伦拜瑞健康科技有限公司 | Method for preparing high-activity cranberry extract by sectional extraction method |
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| CN101037702A (en) * | 2007-02-16 | 2007-09-19 | 北京市农林科学院 | Method for manufacturing purple corn anthocyanin |
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| US20020055471A1 (en) * | 2000-08-31 | 2002-05-09 | Bailey David T. | Efficient method for producing compositions enriched in anthocyanins |
| CN101037702A (en) * | 2007-02-16 | 2007-09-19 | 北京市农林科学院 | Method for manufacturing purple corn anthocyanin |
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