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CN104876986B - A kind of method of anthocyanin in extraction purple sweetpotato - Google Patents

A kind of method of anthocyanin in extraction purple sweetpotato Download PDF

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CN104876986B
CN104876986B CN201510339783.0A CN201510339783A CN104876986B CN 104876986 B CN104876986 B CN 104876986B CN 201510339783 A CN201510339783 A CN 201510339783A CN 104876986 B CN104876986 B CN 104876986B
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vacuum
anthocyanin
purple sweetpotato
eluent
nanofiltration
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CN104876986A (en
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唐方华
黄华学
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Shaoyang Huacheng Green Fruit Biotechnology Co ltd
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Hunan Huacheng Biotech Inc
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Abstract

The method of anthocyanin, comprises the following steps in a kind of extraction purple sweetpotato:(1)Broken, squeezing:Purple sweetpotato is cleaned, crushed, normal temperature physical squeezing is carried out, squeezing juice and press residue are collected respectively;(2)Elution formula is extracted:Purple sweetpotato press residue is fitted into pressure-resistant chromatographic column, is compacted, is sealed, pressurization is eluted with hydrophilic solvent to purple sweetpotato slag press residue, collects eluent, eluent is merged with squeezing juice, mixed liquor is obtained;(3)Centrifugation, ultrafiltration:Mixed liquor is centrifuged, ultrafiltration is then carried out, obtains ultrafiltrate;(4)Nanofiltration, vacuum concentration:Ultrafiltrate is subjected to nanofiltration, nanofiltration liquid is concentrated in vacuo, concentrate is obtained;(5)Micro-wave vacuum:Concentrate is subjected to micro-wave vacuum, pattern glycoside product is obtained.The inventive method has that process is simple, the low feature of energy consumption, extracts the anthocyanin high income of product, anthocyanin yield >=75%, product purity >=40wt%, impurity is few, easy to maintain.

Description

A kind of method of anthocyanin in extraction purple sweetpotato
Technical field
The present invention relates to a kind of method for extracting anthocyanin in purple sweetpotato, and in particular to one kind extracts purple with elution formula method The method of anthocyanin in sweet potato.
Background technology
Purple sweetpotato, scientific name Solanum tuberdsm, English name purple sweet potato, alias purple potato, black potato. There is cultivation in China various regions.
Purple potato has various active composition, and nutritive value is higher, and it is rich in abundant anthocyanin class material, purple sweet potato anthocyanin It is a kind of natural pigment class material, with the various health care functions such as anti-oxidant, anticancer and protection eyesight, is widely used in food The fields such as product, drink and cosmetics.Because of the wide material sources of purple sweetpotato, and anthocyanin content is higher, and price is low, can be used as extraction A kind of good raw material of anthocyanin.
In recent years, the research that China researcher comes to extracting anthocyanin from purple sweetpotato is more.
CN104371351A discloses a kind of preparation method of Ipomoea batatas(L.)Lam, and this method is after purple sweetpotato is crushed, to make Extracted with sour water, then separate, concentrate through macroporous resin adsorption, drying etc. and obtain finished product, product yield is up to 3%, pattern Glycosides purity about 25%, this method technique is simple, meets industrialized production, but process power consumption is larger, and cost is of a relatively high.
CN101735646B discloses a kind of separating and extracting process of anthocyanins pigment from purple sweet potato, and this method is by fresh purple sweetpotato After mashing is broken, using ultrasound assisted extraction, recovered, macroporous resin adsorption separation, concentration and the obtained product, production such as dry Product anthocyanin content is about 30%, color value 146, and this method is adapted to plant operation, but the cycle is relatively long, during anthocyanin portion Divide degraded denaturation, product cost is high.
CN101735644B discloses a kind of extracting method of anthocyanins pigment from purple sweet potato, and this method is that purple sweetpotato is used into microwave After heat is ripe, extraction then is homogenized using sour water, through high speed centrifugation, concentration, dries, obtains product, yield is 34.96%, in product Anthocyanin content is about 10%.This method technique is simple, and product yield is higher, but the product impurity obtained is more, purity is low, unsuitable Preserve.
The content of the invention
The technical problems to be solved by the invention are that the drawbacks described above for overcoming prior art to exist is simple there is provided a kind of process The single, rate of recovery is high, energy consumption is low, and product purity is high, impurity is few, the method for extracting anthocyanin in purple sweetpotato easy to maintain.
The technical solution adopted for the present invention to solve the technical problems is as follows:The side of anthocyanin in a kind of extraction purple sweetpotato Method, comprises the following steps:
(1)Broken, squeezing:Purple sweetpotato is cleaned, crushed, normal temperature physical squeezing is carried out, squeezing juice and squeezing are collected respectively Slag, it is standby;
(2)Elution formula is extracted:By step(1)Gained purple sweetpotato press residue is fitted into pressure-resistant chromatographic column, is compacted, sealing, plus Pressure, is eluted with hydrophilic solvent as eluant, eluent to purple sweetpotato press residue, eluent is collected, by eluent and step(1)Institute Obtain squeezing juice to merge, obtain mixed liquor;
(3)Centrifugation, ultrafiltration:By step(2)Gained mixed liquor is centrifuged, and is then carried out ultrafiltration, is obtained ultrafiltrate;
(4)Nanofiltration, vacuum concentration:By step(3)Gained ultrafiltrate carries out nanofiltration, and it is dense that nanofiltration retentate fluid is carried out into vacuum Contracting, obtains concentrate;
(5)Micro-wave vacuum:By step(4)Gained concentrate carries out micro-wave vacuum, obtains pattern glycoside product.
Further, step(2)In, the pressure of the pressurization is 2.0~4.0Mpa.
Further, step(2)In, the hydrophilic solvent is the ethanol solution of volume fraction 50~70%.
Further, step(2)In, the flow velocity of the eluant, eluent is 3~5BV/h, the volume of the eluant, eluent used for 25~ 30BV。
Step(2)In, the elution formula extraction is that one kind crushes raw material after crushing, is fitted into pressure-resistant chromatographic column, is compacted Afterwards, the extraction mode that is then eluted under high pressure using solvent to the raw material in post, the relatively conventional method of this method is had Beneficial effect has:
1)The extraction of elution formula is that dress post replaces traditional extraction pot type device after raw material squeezing is crushed, and it is handled in guarantee While amount, extraction space is greatlyd save, the processing space of elution formula extraction is only the 1/8~1/ of extractor extraction space 10;
2)The extraction of elution formula is eluted using high pressure mode, during, the flow velocity of eluant, eluent is stablized relatively, its parameter control Digitization processed, become more meticulous, compared to traditional method for extracting, automaticity is high, efficiency high;
3)Elution formula extraction of the present invention is from 50~70% ethanol solutions as eluant, eluent, and main cause has at 2 points, and one is true Protecting eluant, eluent has good permeability to raw material, and two are to ensure that target component anthocyanin can be good at dissolution, while subtracting again Few polysaccharide(Mainly starch), protein, the dissolution of the macromolecular water-soluble substances such as tannin, the pattern in elution formula extraction solution The purity of glycosides is 10~12 times of traditional refluxing extraction;
4)The elution formula extraction of the present invention may be temperature controlled, and in the methods of the invention, use normal temperature Extraction, the time of whole elution formula extraction is only the 40~60% of traditional extraction process, and anthocyanin is protected well, is reduced Its probability degraded.
Further, step(3)In, the centrifugation is tubular type centrifugation, and the speed of centrifugation is 10000~14000r/min.Enter The main purpose of row centrifugation is to remove the deposit in mixed liquor, and particulate matter, reduces the pressure of follow-up membrane filtration.
Further, step(3)In, the ultrafiltration is second ultrafiltration, use for the first time molecular cut off for 20000~ The milipore filter of 40000 dalton, primarily to removing the macromolecular substances such as carbohydrate, albumen, uses molecular cut off for the second time For the milipore filter of 4000~6000 dalton, primarily to the material of the medium molecule size such as some polymers is removed, after being Continuous nanofiltration reduces pressure, improves the efficiency of membrane filtration, extends the service efficiency of film.
Further, step(4)In, the nanofiltration uses molecular cut off for the NF membrane of 100~200 dalton.Carry out The main purpose of nanofiltration is retention target anthocyanin class material, removes small molecule, salt and most of solvent.
Further, step(4)In, the temperature of the vacuum concentration is 50~60 DEG C, vacuum is -0.08~- 0.04Mpa, it is 25~30 to be concentrated into hundred profit degree.
Further, step(5)In, the vacuum of the micro-wave vacuum is -0.08~-0.06Mpa, the power of microwave For 8~12kw, dry to moisture≤5%.
The inventive method has advantages below:
(1)The inventive method technological process is simple, is easy to operation, adapts to the production of modern factories metaplasia;
(2)It is creative in the inventive method to replace traditional extraction mode, the extraction using ethanol elution formula extraction mode Mode is carried out in normal temperature, it is ensured that the stability of anthocyanin, in addition, while ensureing that anthocyanin extracts abundant, other impurities Dissolution reduce, direct purification extract;
(3)The filter type that the inventive method is combined using centrifugation with second ultrafiltration, is eliminated most miscellaneous well Matter, improves the efficiency of filtering;
(4)The inventive method uses nanofiltration, eliminates most solvent, reduces the pressure being subsequently concentrated in vacuo, energy Depletion few more than 30%;
(5)The whole technical process temperature of the inventive method be normal temperature, during traditional suction type need not be used to enter Row purifying, and processing time is short, loss is few, the anthocyanin high income of product, anthocyanin yield >=75%, and product purity >= 40wt%, its purity is significantly larger than the purity of anthocyanin about 30wt% obtained by general purifying resin technique;
(6)Pattern glycoside product obtained by the inventive method is placed under dry dark conditions, the shelf-life reaches 2 years.
Embodiment
With reference to embodiment, the invention will be further described.
Juice extractor used in the embodiment of the present invention is industrial spiral juice extractor, model LZ-2.5, manufacturer:Jingjiang City's spy's prestige mechanical equipment factory;Chromatographic column specification is 300 × 1200mm of Ф, and chromatographic column material is stainless steel, pressure-resistant≤10.0Mpa; Micro-wave vacuum equipment, model GW-WZ-20, manufacturer:Nanjing national strength and prestige heating equipment Co., Ltd;HPLC ultraviolet detections The wavelength of device detection is 540 nm;Used chemical reagent, unless otherwise specified, is obtained by routine business approach.
Embodiment 1
(1)Broken, squeezing:By the fresh purple sweetpotatos of 200kg(Anthocyanin content is 1.20%)Cleaning, crushes, uses juice extractor Normal temperature physical squeezing is carried out, squeezing juice and press residue are collected respectively, it is standby;
(2)Elution formula is extracted:By step(1)Gained purple sweetpotato press residue is fitted into pressure-resistant chromatographic column, is compacted, sealing, plus 2MPa is pressed, purple sweetpotato slag press residue is eluted as eluant, eluent with the ethanol solution of volume fraction 70%, eluant, eluent second is controlled The flow velocity of alcoholic solution is 3.25BV/h, and the volume of the eluant, eluent ethanol solution used is 25BV, collects eluent, by eluent with Step(1)Gained squeezing juice merges, and obtains mixed liquor;
(3)Centrifugation, ultrafiltration:By step(2)Gained mixed liquor carries out tubular type centrifugation under 14000r/min centrifugation rates, so After carry out second ultrafiltration, use molecular cut off for the milipore filter of 20000 dalton for the first time, molecular cut off used for the second time For the milipore filter of 5000 dalton, ultrafiltrate is obtained;
(4)Nanofiltration, vacuum concentration:By step(3)Gained ultrafiltrate uses molecular cut off for the NF membrane of 150 dalton Nanofiltration is carried out, then by nanofiltration retentate fluid at 50 DEG C, vacuum is under -0.08~-0.04Mpa, being concentrated in vacuo to hundred profit degree is 25, obtain concentrate;
(5)Micro-wave vacuum:By step(4)Gained concentrate is -0.08~-0.06Mpa, microwave power in vacuum Under 10 kw, micro-wave vacuum to moisture is 4.32%, obtains 4.35kg pattern glycoside products.
Gained pattern glycoside product detects that anthocyanin content is 42.73wt% through UV try and error methods, and anthocyanin yield is 77.45%; Gained pattern glycoside product is placed under dry dark conditions, the shelf-life reaches 2 years.
Embodiment 2
(1)Broken, squeezing:By the fresh purple sweetpotatos of 200kg(Anthocyanin content is 1.20%)Cleaning, crushes, uses juice extractor Normal temperature physical squeezing is carried out, squeezing juice and press residue are collected respectively, it is standby;
(2)Elution formula is extracted:By step(1)Gained purple sweetpotato press residue is fitted into pressure-resistant chromatographic column, is compacted, sealing, plus 4MPa is pressed, purple sweetpotato slag press residue is eluted as eluant, eluent with the ethanol solution of volume fraction 50%, eluant, eluent second is controlled The flow velocity of alcoholic solution is 4.97BV/h, and the volume of the eluant, eluent ethanol solution used is 30BV, collects eluent, by eluent with Step(1)Gained squeezing juice merges, and obtains mixed liquor;
(3)Centrifugation, ultrafiltration:By step(2)Gained mixed liquor carries out tubular type centrifugation under 12000r/min centrifugation rates, so After carry out second ultrafiltration, use molecular cut off for the milipore filter of 20000 dalton for the first time, molecular cut off used for the second time For the milipore filter of 4000 dalton, ultrafiltrate is obtained;
(4)Nanofiltration, vacuum concentration:By step(3)Gained ultrafiltrate uses molecular cut off for the NF membrane of 150 dalton Nanofiltration is carried out, then by nanofiltration retentate fluid at 60 DEG C, vacuum is under -0.08~-0.04Mpa, being concentrated in vacuo to hundred profit degree is 30, obtain concentrate;
(5)Micro-wave vacuum:By step(4)Gained concentrate is -0.08~-0.06Mpa, microwave power in vacuum For under 10kw, micro-wave vacuum to moisture is 4.73%, obtains 4.53kg pattern glycoside products.
Gained pattern glycoside product detects that anthocyanin content is 40.12wt% through UV try and error methods, and anthocyanin yield is 75.73%; Gained pattern glycoside product is placed under dry dark conditions, the shelf-life reaches 2 years.
Embodiment 3
(1)Broken, squeezing:By the fresh purple sweetpotatos of 200kg(Anthocyanin content is 1.20%)Cleaning, crushes, uses juice extractor Normal temperature physical squeezing is carried out, squeezing juice and press residue are collected respectively, it is standby;
(2)Elution formula is extracted:By step(1)Gained purple sweetpotato press residue is fitted into pressure-resistant chromatographic column, is compacted, sealing, plus 3MPa is pressed, purple sweetpotato slag press residue is eluted as eluant, eluent with the ethanol solution of volume fraction 60%, eluant, eluent second is controlled The flow velocity of alcoholic solution is 3.93BV/h, and the volume of the eluant, eluent ethanol solution used is 28BV, collects eluent, by eluent with Step(1)Gained squeezing juice merges, and obtains mixed liquor;
(3)Centrifugation, ultrafiltration:By step(2)Gained mixed liquor carries out tubular type centrifugation under 13000r/min centrifugation rates, so After carry out second ultrafiltration, use molecular cut off for the milipore filter of 40000 dalton for the first time, molecular cut off used for the second time For the milipore filter of 6000 dalton, ultrafiltrate is obtained;
(4)Nanofiltration, vacuum concentration:By step(3)Gained ultrafiltrate uses molecular cut off for the NF membrane of 200 dalton Nanofiltration is carried out, then by nanofiltration retentate fluid at 55 DEG C, vacuum is under -0.08~-0.04Mpa, being concentrated in vacuo to hundred profit degree is 27, obtain concentrate;
(5)Micro-wave vacuum:By step(4)Gained concentrate is -0.08~-0.06Mpa, microwave power in vacuum For under 10kw, micro-wave vacuum to moisture is 3.94%, obtains 4.39kg pattern glycoside products.
Gained pattern glycoside product is through HPLC ultraviolet detections, and anthocyanin content is 41.56wt%, and anthocyanin yield is 76.02%; Gained pattern glycoside product is placed under dry dark conditions, the shelf-life reaches 2 years.
Embodiment 4
(1)Broken, squeezing:By the fresh purple sweetpotatos of 200kg(Anthocyanin content is 1.20%)Cleaning, crushes, uses juice extractor Normal temperature physical squeezing is carried out, squeezing juice and press residue are collected respectively, it is standby;
(2)Elution formula is extracted:By step(1)Gained purple sweetpotato press residue is fitted into pressure-resistant chromatographic column, is compacted, sealing, plus 2.5MPa is pressed, purple sweetpotato slag press residue is eluted as eluant, eluent with the ethanol solution of volume fraction 65%, eluant, eluent is controlled The flow velocity of ethanol solution is 3.63BV/h, and the volume of the eluant, eluent ethanol solution used is 26BV, eluent is collected, by eluent With step(1)Gained squeezing juice merges, and obtains mixed liquor;
(3)Centrifugation, ultrafiltration:By step(2)Gained mixed liquor carries out tubular type centrifugation under 10000r/min centrifugation rates, so After carry out second ultrafiltration, use molecular cut off for the milipore filter of 40000 dalton for the first time, molecular cut off used for the second time For the milipore filter of 5000 dalton, ultrafiltrate is obtained;
(4)Nanofiltration, vacuum concentration:By step(3)Gained ultrafiltrate uses molecular cut off for the NF membrane of 150 dalton Nanofiltration is carried out, then by nanofiltration retentate fluid at 57 DEG C, vacuum is under -0.08~-0.04Mpa, being concentrated in vacuo to hundred profit degree is 26, obtain concentrate;
(5)Micro-wave vacuum:By step(4)Gained concentrate is -0.08~-0.06Mpa, microwave power in vacuum For under 10kw, micro-wave vacuum to moisture is 4.11%, obtains 4.48kg pattern glycoside products.
Gained pattern glycoside product is through HPLC ultraviolet detections, and anthocyanin content is 40.95wt%, and anthocyanin yield is 76.44%; Gained pattern glycoside product is placed under dry dark conditions, the shelf-life reaches 2 years.

Claims (12)

1. a kind of method for extracting anthocyanin in purple sweetpotato, it is characterised in that:Comprise the following steps:
(1)Broken, squeezing:Purple sweetpotato is cleaned, crushed, normal temperature physical squeezing is carried out, squeezing juice and press residue are collected respectively, it is standby With;
(2)Elution formula is extracted:By step(1)Gained purple sweetpotato press residue is fitted into pressure-resistant chromatographic column, is compacted, and sealing is forced into 2.0~4.0MPa, with the ethanol solution of volume fraction 50~70% as eluant, eluent, in the case where the flow velocity of eluant, eluent is 3~5BV/h, With the eluant, eluent that volume is 25~30BV, purple sweetpotato press residue is eluted, eluent is collected, by eluent and step(1) Gained squeezing juice merges, and obtains mixed liquor;
(3)Centrifugation, ultrafiltration:By step(2)Gained mixed liquor is centrifuged, and is then carried out ultrafiltration, is obtained ultrafiltrate;
(4)Nanofiltration, vacuum concentration:By step(3)Gained ultrafiltrate carries out nanofiltration, and nanofiltration retentate fluid is concentrated in vacuo, obtained Concentrate;
(5)Micro-wave vacuum:By step(4)Gained concentrate carries out micro-wave vacuum, obtains pattern glycoside product.
2. the method for anthocyanin in purple sweetpotato is extracted according to claim 1, it is characterised in that:Step(3)In, the centrifugation Centrifuged for tubular type, the speed of centrifugation is 10000~14000r/min.
3. the method according to claim 1 or claim 2 for extracting anthocyanin in purple sweetpotato, it is characterised in that:Step(3)In, it is described Ultrafiltration is second ultrafiltration, and molecular cut off is used for the first time for the milipore filter of 20000~40000 dalton, uses cut for the second time Stay the milipore filter that molecular weight is 4000~6000 dalton.
4. the method according to claim 1 or claim 2 for extracting anthocyanin in purple sweetpotato, it is characterised in that:Step(4)In, it is described Nanofiltration uses molecular cut off for the NF membrane of 100~200 dalton.
5. the method for anthocyanin in purple sweetpotato is extracted according to claim 3, it is characterised in that:Step(4)In, the nanofiltration Molecular cut off is used for the NF membrane of 100~200 dalton.
6. the method according to claim 1 or claim 2 for extracting anthocyanin in purple sweetpotato, it is characterised in that:Step(4)In, it is described The temperature of vacuum concentration is 50~60 DEG C, and vacuum is -0.08~-0.04Mpa, and it is 25~30 to be concentrated into hundred profit degree.
7. the method for anthocyanin in purple sweetpotato is extracted according to claim 3, it is characterised in that:Step(4)In, the vacuum The temperature of concentration is 50~60 DEG C, and vacuum is -0.08~-0.04Mpa, and it is 25~30 to be concentrated into hundred profit degree.
8. the method for anthocyanin in purple sweetpotato is extracted according to claim 4, it is characterised in that:Step(4)In, the vacuum The temperature of concentration is 50~60 DEG C, and vacuum is -0.08~-0.04Mpa, and it is 25~30 to be concentrated into hundred profit degree.
9. the method according to claim 1 or claim 2 for extracting anthocyanin in purple sweetpotato, it is characterised in that:Step(5)In, it is described The vacuum of micro-wave vacuum is -0.08~-0.06Mpa, and the power of microwave is 8~12kw, is dried to moisture≤5%.
10. the method for anthocyanin in purple sweetpotato is extracted according to claim 3, it is characterised in that:Step(5)In, it is described micro- The vacuum drying vacuum of ripple is -0.08~-0.06Mpa, and the power of microwave is 8~12kw, is dried to moisture≤5%.
11. the method for anthocyanin in purple sweetpotato is extracted according to claim 4, it is characterised in that:Step(5)In, it is described micro- The vacuum drying vacuum of ripple is -0.08~-0.06Mpa, and the power of microwave is 8~12kw, is dried to moisture≤5%.
12. the method for anthocyanin in purple sweetpotato is extracted according to claim 6, it is characterised in that:Step(5)In, it is described micro- The vacuum drying vacuum of ripple is -0.08~-0.06Mpa, and the power of microwave is 8~12kw, is dried to moisture≤5%.
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Address before: 410205 West, 2nd floor, main building, Jinma (Lugu) high tech park, 188 tongzipo West Road, high tech Zone, Changsha City, Hunan Province

Patentee before: HUNAN HUACHENG BIOTECH, Inc.