CN104876986A - Method for extracting anthocyanin in purple sweet potato - Google Patents
Method for extracting anthocyanin in purple sweet potato Download PDFInfo
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- CN104876986A CN104876986A CN201510339783.0A CN201510339783A CN104876986A CN 104876986 A CN104876986 A CN 104876986A CN 201510339783 A CN201510339783 A CN 201510339783A CN 104876986 A CN104876986 A CN 104876986A
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- 238000000034 method Methods 0.000 title claims abstract description 50
- 235000010208 anthocyanin Nutrition 0.000 title abstract description 20
- 239000004410 anthocyanin Substances 0.000 title abstract description 20
- 229930002877 anthocyanin Natural products 0.000 title abstract description 20
- 150000004636 anthocyanins Chemical class 0.000 title abstract description 20
- 244000017020 Ipomoea batatas Species 0.000 title abstract description 10
- 235000002678 Ipomoea batatas Nutrition 0.000 title abstract description 10
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 34
- 238000001728 nano-filtration Methods 0.000 claims abstract description 31
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 7
- 238000000605 extraction Methods 0.000 claims description 31
- 239000003480 eluent Substances 0.000 claims description 21
- 239000012528 membrane Substances 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 13
- 238000004587 chromatography analysis Methods 0.000 claims description 9
- 239000000284 extract Substances 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 235000004976 Solanum vernei Nutrition 0.000 description 2
- 241000352057 Solanum vernei Species 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000000825 ultraviolet detection Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 235000002634 Solanum Nutrition 0.000 description 1
- 241000207763 Solanum Species 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004438 eyesight Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- -1 starch) Chemical class 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
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- Coloring Foods And Improving Nutritive Qualities (AREA)
- Preparation Of Fruits And Vegetables (AREA)
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Abstract
The invention provides a method for extracting anthocyanin in purple sweet potato. The method comprises the steps of (1) crushing and squeezing, namely, cleaning the purple sweet potato, crushing, physically squeezing at normal temperature, and respectively collecting the squeezed juice and the leaves; (2) extracting by an eluting manner, namely, feeding the leaves of the purple sweet potato into a pressure resistant chromatographic column, compressing, sealing, pressurizing, eluting the leaves of the purple sweet potato through a hydrophilic solvent, collecting the eluting liquid, and combining the eluting liquid and the squeezing juice to obtain the mixed liquid; (3) centrifuging and performing ultrafiltration, namely, centrifuging the mixed liquid, and then performing ultrafiltration to obtain the ultrafiltration liquid; (4) performing nanofiltration and vacuum concentration, namely, performing nanofiltration for the ultrafiltration liquid, and concentrating the ultrafiltration liquid in vacuum to obtain the concentrated liquid; (5) drying in vacuum through microwave, namely, drying the concentrated liquid in vacuum through the microwave to obtain the anthocyanin product. The method has the characteristics of being simple in process and small in energy consumption; the yield of the extracted anthocyanin is high and not less than 75%; the product purity is not less than 40wt%; little impurities are caused; the storage is easy.
Description
Technical field
The present invention relates to a kind of method extracting anthocyanogen in Rhizoma Dioscoreae esculentae, be specifically related to a kind of method that wash-out formula method extracts anthocyanogen in Rhizoma Dioscoreae esculentae.
Background technology
Rhizoma Dioscoreae esculentae, formal name used at school Solanum tuberdsm, English name purple sweet potato, calls purple potato, black potato.All cultivation is had in China various places.
Purple potato has various active composition; nutritive value is higher, and it is rich in abundant anthocyanin class material, and purple sweet potato anthocyanin is a kind of natural pigment class material; there is the various health care functions such as anti-oxidant, anticancer and vision protection, be widely used in the fields such as food, drink and makeup.Because of the wide material sources of Rhizoma Dioscoreae esculentae, and anthocyanin content is higher, and price is low, can be used as the good raw material of one extracting anthocyanogen.
In recent years, China researchist is more to the research of extracting anthocyanogen from Rhizoma Dioscoreae esculentae.
CN104371351A discloses a kind of preparation method of Ipomoea batatas(L.)Lam, the method is by after Rhizoma Dioscoreae esculentae fragmentation, sour water is used to extract, then be separated through macroporous resin adsorption, concentrated, dry etc. obtains finished product, and product yield can reach 3%, anthocyanogen purity about 25%, the method technique is simple, meet suitability for industrialized production, but process power consumption is comparatively large, cost is relatively high.
CN101735646B discloses a kind of separating and extracting method of anthocyanins pigment from purple sweet potato, the method is by after fresh Rhizoma Dioscoreae esculentae making beating fragmentation, adopt ultrasound assisted extraction, through reclaiming, macroporous resin adsorption is separated, the obtained product such as concentrated and dry, and product anthocyanin content is about 30%, look valency 146, the method is applicable to factory's operation, but the cycle is relatively long, anthocyanogen Partial digestion sex change in process, product cost is high.
CN101735644B discloses a kind of extracting method of anthocyanins pigment from purple sweet potato, and the method is after using microwave thermal ripe Rhizoma Dioscoreae esculentae, then uses sour water homogenate extraction, through high speed centrifugation, concentrated, dry, obtain product, yield is 34.96%, and in product, anthocyanin content is about 10%.The method technique is simple, and product yield is higher, but the product impurity obtained is many, purity is low, should not preserve.
Summary of the invention
Technical problem to be solved by this invention is, overcome the above-mentioned defect that prior art exists, provide that a kind of operation is simple, the rate of recovery is high, energy consumption is low, product purity is high, impurity is few, the method for anthocyanogen in the extraction Rhizoma Dioscoreae esculentae easily preserved.
The technical solution adopted for the present invention to solve the technical problems is as follows: a kind of method extracting anthocyanogen in Rhizoma Dioscoreae esculentae, comprises the following steps:
(1) broken, squeezing: Rhizoma Dioscoreae esculentae is cleaned, broken, carry out normal temperature physical squeezing, collect squeezing juice and press residue respectively, for subsequent use;
(2) wash-out formula extraction: step (1) gained Rhizoma Dioscoreae esculentae press residue is loaded in withstand voltage chromatography column, compacting, sealing, pressurization, carries out wash-out as eluent to Rhizoma Dioscoreae esculentae press residue with hydrophilic solvent, collects elutriant, elutriant and step (1) gained squeezing juice are merged, obtains mixed solution;
(3) centrifugal, ultrafiltration: step (2) gained mixed solution is carried out centrifugal, then carries out ultrafiltration, obtain ultrafiltrated;
(4) nanofiltration, vacuum concentration: step (3) gained ultrafiltrated is carried out nanofiltration, nanofiltration trapped fluid is carried out vacuum concentration, obtains concentrated solution;
(5) microwave vacuum drying: step (4) gained concentrated solution is carried out microwave vacuum drying, obtains anthocyanogen product.
Further, in step (2), the pressure of described pressurization is 2.0 ~ 4.0Mpa.
Further, in step (2), described hydrophilic solvent is the ethanolic soln of volume fraction 50 ~ 70%.
Further, in step (2), the flow velocity of described eluent is 3 ~ 5BV/h, and the volume of the eluent of use is 25 ~ 30BV.
In step (2), described wash-out formula extraction, after raw material crushing is pulverized by one, loads in withstand voltage chromatography column, and after compacting, then under high pressure use the raw material in solvent coupled columns to carry out the extraction mode of wash-out, the beneficial effect of the relative traditional method of the method has:
1) extraction of wash-out formula is that after raw material squeezing being pulverized, dress post replaces traditional extraction pot type device, and it, while guarantee treatment capacity, greatly saves and extract space, and the process space of wash-out formula extraction is only extractor extracts space 1/8 ~ 1/10;
2) extraction of wash-out formula adopts high pressure mode to carry out wash-out, and in process, the flow velocity of eluent is relatively stable, its parameter control data, becomes more meticulous, and compare traditional method for extracting, level of automation is high, and efficiency is high;
3) wash-out formula extraction of the present invention selects 50 ~ 70% ethanolic solns as eluent, major cause has 2 points, one is guarantee that eluent has good perviousness to raw material, two is guarantee that target component anthocyanogen can be good at stripping, reduce the stripping of the macromole water-soluble substanceses such as polysaccharide (mainly starch), protein, tannin again, the purity of the anthocyanogen in wash-out formula extraction solution is 10 ~ 12 times of traditional refluxing extraction simultaneously;
4) wash-out formula of the present invention extraction be can carry out temperature controlled, in the methods of the invention, employing be normal temperature extraction, the time of whole wash-out formula extraction is only 40 ~ 60% of traditional extraction process, well protects anthocyanogen, decreases the probability of its degraded.
Further, in step (3), described centrifugal be that tubular type is centrifugal, centrifugal speed is 10000 ~ 14000r/min.Carrying out centrifugal main purpose is remove the sedimentable matter in mixed solution, and particulate matter, reduces the pressure of follow-up membrane filtration.
Further, in step (3), described ultrafiltration is second ultrafiltration, first time adopts molecular weight cut-off to be 20000 ~ 40000 daltonian ultra-filtration membranes, and mainly in order to remove the macromolecular substance such as carbohydrate, albumen, second time adopts molecular weight cut-off to be 4000 ~ 6000 daltonian ultra-filtration membranes, mainly in order to remove the material of the medium molecule sizes such as some polymers, for subsequent nano-filtration reduces pressure, improve the efficiency of membrane filtration, extend the service efficiency of film.
Further, in step (4), described nanofiltration adopts molecular weight cut-off to be 100 ~ 200 daltonian nanofiltration membrane.The main purpose of carrying out nanofiltration retains target anthocyanin class material, removes small molecules, salt and most of solvent.
Further, in step (4), the temperature of described vacuum concentration is 50 ~ 60 DEG C, and vacuum tightness is-0.08 ~-0.04Mpa, and being concentrated into hundred sharp degree is 25 ~ 30.
Further, in step (5), the vacuum tightness of described microwave vacuum drying is-0.08 ~-0.06Mpa, and the power of microwave is 8 ~ 12kw, is dried to moisture content≤5%.
The inventive method has the following advantages:
(1) the inventive method technical process is simple, convenient operation, adapts to modern factoriesization and produces;
(2) in the inventive method, the creative ethanol elution formula extraction mode that uses replaces traditional extraction mode, and this extraction mode is carried out at normal temperature, ensure that the stability of anthocyanogen, in addition, extract fully simultaneously guarantee anthocyanogen, the stripping of other impurity reduces, direct purification extraction liquid;
(3) the inventive method uses the centrifugal filter type be combined with second ultrafiltration, well eliminates most impurity, improves the efficiency of filtration;
(4) the inventive method uses nanofiltration, eliminates most solvent, decreases the pressure of follow-up vacuum concentration, and energy consumption reduces more than 30%;
(5) the whole technological process temperature of the inventive method is normal temperature, do not need in process to use traditional suction type to carry out purifying, and the treatment time is short, loss is few, the anthocyanogen yield of product is high, anthocyanogen yield >=75%, product purity >=40wt%, its purity is about the purity of 30wt% far away higher than general resin purification technique gained anthocyanogen;
(6), under the inventive method gained anthocyanogen product being placed in dry dark conditions, the quality guaranteed period reaches 2 years.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
The juice extractor that the embodiment of the present invention uses is industrial spiral juice extractor, model LZ-2.5, manufacturer: the special prestige mechanical equipment factory in Jingjiang City; Chromatography column specification is Ф 300 × 1200mm, and chromatography column material is stainless steel, withstand voltage≤10.0Mpa; Micro-wave vacuum equipment, model GW-WZ-20, manufacturer: Nanjing national strength and prestige electric heating apparatus company limited; The wavelength that HPLC UV-detector detects is 540 nm; The chemical reagent used, if no special instructions, is all obtained by routine business approach.
embodiment 1
(1) broken, squeezing: fresh for 200kg Rhizoma Dioscoreae esculentae (anthocyanin content is 1.20%) is cleaned, broken, use juice extractor to carry out normal temperature physical squeezing, collect squeezing juice and press residue respectively, for subsequent use;
(2) wash-out formula extraction: step (1) gained Rhizoma Dioscoreae esculentae press residue is loaded in withstand voltage chromatography column, compacting, sealing, pressurization 2MPa, carries out wash-out as eluent to Rhizoma Dioscoreae esculentae slag press residue with the ethanolic soln of volume fraction 70%, and the flow velocity controlling eluent ethanolic soln is 3.25BV/h, the volume of the eluent ethanolic soln used is 25BV, collect elutriant, elutriant and step (1) gained squeezing juice are merged, obtains mixed solution;
(3) centrifugal, ultrafiltration: it is centrifugal step (2) gained mixed solution to be carried out under 14000r/min centrifugation rate tubular type, then second ultrafiltration is carried out, first time adopts molecular weight cut-off to be 20000 daltonian ultra-filtration membranes, second time adopts molecular weight cut-off to be 5000 daltonian ultra-filtration membranes, obtains ultrafiltrated;
(4) nanofiltration, vacuum concentration: adopt molecular weight cut-off to be that 150 daltonian nanofiltration membrane carry out nanofiltration step (3) gained ultrafiltrated, then by nanofiltration trapped fluid at 50 DEG C, vacuum tightness is under-0.08 ~-0.04Mpa, and the sharp degree of vacuum concentration to hundred is 25, obtains concentrated solution;
(5) microwave vacuum drying: be-0.08 ~-0.06Mpa in vacuum tightness by step (4) gained concentrated solution, under microwave power 10 kw, microwave vacuum drying is 4.32% to moisture, obtains 4.35kg anthocyanogen product.
Gained anthocyanogen product detects through UV try and error method, and anthocyanin content is 42.73wt%, and anthocyanogen yield is 77.45%; Under gained anthocyanogen product is placed in dry dark conditions, the quality guaranteed period reaches 2 years.
embodiment 2
(1) broken, squeezing: fresh for 200kg Rhizoma Dioscoreae esculentae (anthocyanin content is 1.20%) is cleaned, broken, use juice extractor to carry out normal temperature physical squeezing, collect squeezing juice and press residue respectively, for subsequent use;
(2) wash-out formula extraction: step (1) gained Rhizoma Dioscoreae esculentae press residue is loaded in withstand voltage chromatography column, compacting, sealing, pressurization 4MPa, carries out wash-out as eluent to Rhizoma Dioscoreae esculentae slag press residue with the ethanolic soln of volume fraction 50%, and the flow velocity controlling eluent ethanolic soln is 4.97BV/h, the volume of the eluent ethanolic soln used is 30BV, collect elutriant, elutriant and step (1) gained squeezing juice are merged, obtains mixed solution;
(3) centrifugal, ultrafiltration: it is centrifugal step (2) gained mixed solution to be carried out under 12000r/min centrifugation rate tubular type, then second ultrafiltration is carried out, first time adopts molecular weight cut-off to be 20000 daltonian ultra-filtration membranes, second time adopts molecular weight cut-off to be 4000 daltonian ultra-filtration membranes, obtains ultrafiltrated;
(4) nanofiltration, vacuum concentration: adopt molecular weight cut-off to be that 150 daltonian nanofiltration membrane carry out nanofiltration step (3) gained ultrafiltrated, then by nanofiltration trapped fluid at 60 DEG C, vacuum tightness is under-0.08 ~-0.04Mpa, and the sharp degree of vacuum concentration to hundred is 30, obtains concentrated solution;
(5) microwave vacuum drying: be-0.08 ~-0.06Mpa in vacuum tightness by step (4) gained concentrated solution, microwave power is under 10kw, and microwave vacuum drying is 4.73% to moisture, obtains 4.53kg anthocyanogen product.
Gained anthocyanogen product detects through UV try and error method, and anthocyanin content is 40.12wt%, and anthocyanogen yield is 75.73%; Under gained anthocyanogen product is placed in dry dark conditions, the quality guaranteed period reaches 2 years.
embodiment 3
(1) broken, squeezing: fresh for 200kg Rhizoma Dioscoreae esculentae (anthocyanin content is 1.20%) is cleaned, broken, use juice extractor to carry out normal temperature physical squeezing, collect squeezing juice and press residue respectively, for subsequent use;
(2) wash-out formula extraction: step (1) gained Rhizoma Dioscoreae esculentae press residue is loaded in withstand voltage chromatography column, compacting, sealing, pressurization 3MPa, carries out wash-out as eluent to Rhizoma Dioscoreae esculentae slag press residue with the ethanolic soln of volume fraction 60%, and the flow velocity controlling eluent ethanolic soln is 3.93BV/h, the volume of the eluent ethanolic soln used is 28BV, collect elutriant, elutriant and step (1) gained squeezing juice are merged, obtains mixed solution;
(3) centrifugal, ultrafiltration: it is centrifugal step (2) gained mixed solution to be carried out under 13000r/min centrifugation rate tubular type, then second ultrafiltration is carried out, first time adopts molecular weight cut-off to be 40000 daltonian ultra-filtration membranes, second time adopts molecular weight cut-off to be 6000 daltonian ultra-filtration membranes, obtains ultrafiltrated;
(4) nanofiltration, vacuum concentration: adopt molecular weight cut-off to be that 200 daltonian nanofiltration membrane carry out nanofiltration step (3) gained ultrafiltrated, then by nanofiltration trapped fluid at 55 DEG C, vacuum tightness is under-0.08 ~-0.04Mpa, and the sharp degree of vacuum concentration to hundred is 27, obtains concentrated solution;
(5) microwave vacuum drying: be-0.08 ~-0.06Mpa in vacuum tightness by step (4) gained concentrated solution, microwave power is under 10kw, and microwave vacuum drying is 3.94% to moisture, obtains 4.39kg anthocyanogen product.
Gained anthocyanogen product is through HPLC ultraviolet detection, and anthocyanin content is 41.56wt%, and anthocyanogen yield is 76.02%; Under gained anthocyanogen product is placed in dry dark conditions, the quality guaranteed period reaches 2 years.
embodiment 4
(1) broken, squeezing: fresh for 200kg Rhizoma Dioscoreae esculentae (anthocyanin content is 1.20%) is cleaned, broken, use juice extractor to carry out normal temperature physical squeezing, collect squeezing juice and press residue respectively, for subsequent use;
(2) wash-out formula extraction: step (1) gained Rhizoma Dioscoreae esculentae press residue is loaded in withstand voltage chromatography column, compacting, sealing, pressurization 2.5MPa, carries out wash-out as eluent to Rhizoma Dioscoreae esculentae slag press residue with the ethanolic soln of volume fraction 65%, and the flow velocity controlling eluent ethanolic soln is 3.63BV/h, the volume of the eluent ethanolic soln used is 26BV, collect elutriant, elutriant and step (1) gained squeezing juice are merged, obtains mixed solution;
(3) centrifugal, ultrafiltration: it is centrifugal step (2) gained mixed solution to be carried out under 10000r/min centrifugation rate tubular type, then second ultrafiltration is carried out, first time adopts molecular weight cut-off to be 40000 daltonian ultra-filtration membranes, second time adopts molecular weight cut-off to be 5000 daltonian ultra-filtration membranes, obtains ultrafiltrated;
(4) nanofiltration, vacuum concentration: adopt molecular weight cut-off to be that 150 daltonian nanofiltration membrane carry out nanofiltration step (3) gained ultrafiltrated, then by nanofiltration trapped fluid at 57 DEG C, vacuum tightness is under-0.08 ~-0.04Mpa, and the sharp degree of vacuum concentration to hundred is 26, obtains concentrated solution;
(5) microwave vacuum drying: be-0.08 ~-0.06Mpa in vacuum tightness by step (4) gained concentrated solution, microwave power is under 10kw, and microwave vacuum drying is 4.11% to moisture, obtains 4.48kg anthocyanogen product.
Gained anthocyanogen product is through HPLC ultraviolet detection, and anthocyanin content is 40.95wt%, and anthocyanogen yield is 76.44%; Under gained anthocyanogen product is placed in dry dark conditions, the quality guaranteed period reaches 2 years.
Claims (9)
1. extract a method for anthocyanogen in Rhizoma Dioscoreae esculentae, it is characterized in that: comprise the following steps:
(1) broken, squeezing: Rhizoma Dioscoreae esculentae is cleaned, broken, carry out normal temperature physical squeezing, collect squeezing juice and press residue respectively, for subsequent use;
(2) wash-out formula extraction: step (1) gained Rhizoma Dioscoreae esculentae press residue is loaded in withstand voltage chromatography column, compacting, sealing, pressurization, carries out wash-out as eluent to Rhizoma Dioscoreae esculentae press residue with hydrophilic solvent, collects elutriant, elutriant and step (1) gained squeezing juice are merged, obtains mixed solution;
(3) centrifugal, ultrafiltration: step (2) gained mixed solution is carried out centrifugal, then carries out ultrafiltration, obtain ultrafiltrated;
(4) nanofiltration, vacuum concentration: step (3) gained ultrafiltrated is carried out nanofiltration, nanofiltration trapped fluid is carried out vacuum concentration, obtains concentrated solution;
(5) microwave vacuum drying: step (4) gained concentrated solution is carried out microwave vacuum drying, obtains anthocyanogen product.
2. extract the method for anthocyanogen in Rhizoma Dioscoreae esculentae according to claim 1, it is characterized in that: in step (2), the pressure of described pressurization is 2.0 ~ 4.0Mpa.
3. according to claim 1 or 2, extract the method for anthocyanogen in Rhizoma Dioscoreae esculentae, it is characterized in that: in step (2), described hydrophilic solvent is the ethanolic soln of volume fraction 50 ~ 70%.
4. according to the method for anthocyanogen in the described extraction Rhizoma Dioscoreae esculentae of one of claims 1 to 3, it is characterized in that: in step (2), the flow velocity of described eluent is 3 ~ 5BV/h, and the volume of the eluent of use is 25 ~ 30BV.
5., according to the method for anthocyanogen in the described extraction Rhizoma Dioscoreae esculentae of one of Claims 1 to 4, it is characterized in that: in step (3), described centrifugal be that tubular type is centrifugal, centrifugal speed is 10000 ~ 14000r/min.
6. according to the method for anthocyanogen in the described extraction Rhizoma Dioscoreae esculentae of one of Claims 1 to 5, it is characterized in that: in step (3), described ultrafiltration is second ultrafiltration, first time adopts molecular weight cut-off to be 20000 ~ 40000 daltonian ultra-filtration membranes, and second time adopts molecular weight cut-off to be 4000 ~ 6000 daltonian ultra-filtration membranes.
7. according to the method for anthocyanogen in the described extraction Rhizoma Dioscoreae esculentae of one of claim 1 ~ 6, it is characterized in that: in step (4), described nanofiltration adopts molecular weight cut-off to be 100 ~ 200 daltonian nanofiltration membrane.
8. according to the method for anthocyanogen in the described extraction Rhizoma Dioscoreae esculentae of one of claim 1 ~ 7, it is characterized in that: in step (4), the temperature of described vacuum concentration is 50 ~ 60 DEG C, and vacuum tightness is-0.08 ~-0.04Mpa, and being concentrated into hundred sharp degree is 25 ~ 30.
9. according to the method for anthocyanogen in the described extraction Rhizoma Dioscoreae esculentae of one of claim 1 ~ 8, it is characterized in that: in step (5), the vacuum tightness of described microwave vacuum drying is-0.08 ~-0.06Mpa, and the power of microwave is 8 ~ 12kw, is dried to moisture content≤5%.
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| CN106819936A (en) * | 2017-02-15 | 2017-06-13 | 扬州大学 | A kind of purple vegetable juice sausage and preparation method thereof |
| IT201700057655A1 (en) * | 2017-05-26 | 2018-11-26 | Rosario Timpone | PROCEDURE FOR SEPARATION AND PURIFICATION OF RED ORANGE POLYPHENOLS |
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| IT201700057655A1 (en) * | 2017-05-26 | 2018-11-26 | Rosario Timpone | PROCEDURE FOR SEPARATION AND PURIFICATION OF RED ORANGE POLYPHENOLS |
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