Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of purification process of Ipomoea batatas(L.)Lam, the Ipomoea batatas(L.)Lam free from extraneous odour obtaining after the method purifying, and purity is higher.
In order to solve above technical problem, the invention provides a kind of purification process of Ipomoea batatas(L.)Lam, comprise the following steps:
By Ipomoea batatas(L.)Lam extracting solution wash-out after absorption with macroporous adsorbent resin, after recovery solvent, obtain feed liquid;
Take ion exchange chromatography resin as ion-exchanger, described feed liquid is carried out to ion exchange chromatography, obtain the chromatographic solution that contains Ipomoea batatas(L.)Lam.
Preferably, described ion exchange chromatography resin is one or more in polymeric amide, polyacrylic acid and polystyrene.
Preferably, the moving phase of described ion exchange chromatography is for containing the water-soluble solvent of 0.05~0.5% hydrochloric acid or containing 0.05~0.5% or the water-soluble solvent of citric acid.
Preferably, the flow rate of mobile phase of described ion exchange chromatography is 0.1~2BV/h.
Preferably, feed liquid is carried out also comprising before ion exchange chromatography:
The filtering with microporous membrane that is 1.0~0.1um by described feed liquid via hole diameter.
Preferably, described Ipomoea batatas(L.)Lam extracting solution is prepared as follows:
Utilize level Four Continuous Countercurrent Extraction method to carry out pigment extracting to Rhizoma Dioscoreae esculentae, after filtration, obtain Ipomoea batatas(L.)Lam extracting solution.
Preferably, described extraction temperature is 20~40 ℃, and extraction time is 2~8h.
Preferably, also comprise:
By the described chromatographic solution that contains Ipomoea batatas(L.)Lam through nanofiltration membrane purifying.
Preferably, also comprise:
In described chromatographic solution after nanofiltration membrane purifying, add maltodextrin, after spraying is dry, obtain Ipomoea batatas(L.)Lam powder.
Preferably, the DE value of described maltodextrin is 10~24.
The purification process that the invention provides a kind of Ipomoea batatas(L.)Lam, comprises the following steps: by Ipomoea batatas(L.)Lam extracting solution wash-out after absorption with macroporous adsorbent resin, reclaim solvent and obtain feed liquid; Take ion exchange chromatography resin as chromatography stationary phase, described feed liquid, by ion exchange chromatography bed, is obtained to the chromatographic solution that contains Ipomoea batatas(L.)Lam.Compared with prior art, the present invention be take ion exchange chromatography resin as chromatography agent, by feed liquid is carried out to ion exchange chromatography, by small molecules degradation product residual in feed liquid, polysaccharide and the Impurity removal approaching with Ipomoea batatas(L.)Lam adsorption effect, Ipomoea batatas(L.)Lam purity is improved, and the peculiar smell such as odorless, " rotten Ipomoea batatas " taste and bitter taste.
Embodiment
Below the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
The purification process that the invention discloses a kind of Ipomoea batatas(L.)Lam, comprises the following steps:
By Ipomoea batatas(L.)Lam extracting solution wash-out after absorption with macroporous adsorbent resin, reclaim solvent and obtain feed liquid;
Take ion exchange chromatography resin as ion-exchanger, described feed liquid is carried out to ion exchange chromatography, obtain the chromatographic solution that contains Ipomoea batatas(L.)Lam.
According to the present invention, described Ipomoea batatas(L.)Lam extracting solution is preferably prepared as follows: utilize level Four Continuous Countercurrent Extraction method to carry out pigment extracting to Rhizoma Dioscoreae esculentae, obtain Ipomoea batatas(L.)Lam extracting solution after filtration.Wherein, the present invention preferably carries out chopping processing to the Rhizoma Dioscoreae esculentae for level Four Continuous Countercurrent Extraction, be specially: Rhizoma Dioscoreae esculentae is cleaned to the surperficial foreign material such as silt with clear water, put in chopping equipment, the spacing of adjustable blade, makes the Rhizoma Dioscoreae esculentae silk specification cutting be: thickness≤3.5mm, length≤3cm.Utilizing level Four Continuous Countercurrent Extraction method to carry out in pigment extractive process Rhizoma Dioscoreae esculentae, described extraction temperature is preferably 20~40 ℃, more preferably 20~35 ℃, most preferably is 25~30 ℃; The described extracting time is preferably 2~8h, and more preferably 2~6h, most preferably is 2~5h; Solid-to-liquid ratio is preferably 1: (5~20), more preferably 1: (5~10), most preferably are 1: 7.The solvent that described level Four Continuous Countercurrent Extraction method adopts is preferably the hydrochloric acid that contains 0.1~0.5% or the aqueous ethanolic solution that contains 0.1~0.5% hydrochloric acid; Can also be for containing 0.1~0.5% lemon aqueous acid or aqueous ethanolic solution, the volumetric concentration of described aqueous ethanolic solution is preferably 1~80%.The described filtration step that obtains Ipomoea batatas(L.)Lam extracting solution preferably adopts 1~400 object strainer filtering, and filter screen matter material is preferably stainless steel or micropore sand.
When preparing Ipomoea batatas(L.)Lam extracting solution, pass through to adopt level Four Continuous Countercurrent Extraction method, make Ipomoea batatas(L.)Lam extract production process serialization, the intermittent type extraction process adopting with respect to other patents, the production efficiency of the method obviously improves, and is conducive to reduce production costs and the expansion of products production scale.
The present invention, for method the particular requirement of described absorption with macroporous adsorbent resin, can adopt method well known to those skilled in the art to adsorb.Preferably, process is specially: Ipomoea batatas(L.)Lam extracting solution is adsorbed through macroporous adsorptive resins, and described macroporous adsorptive resins is preferably nonpolar or low-pole macroporous adsorptive resins.Wherein, in preparing Ipomoea batatas(L.)Lam extracting solution process, when solvent adopts the aqueous ethanolic solution that contains 0.1~0.5% hydrochloric acid, before carrying out absorption with macroporous adsorbent resin, preferably by Ipomoea batatas(L.)Lam extracting solution heating under vacuum, reclaim ethanol, then add water or aqueous ethanolic solution containing 0.1 hydrochloric acid to dilute 5~20 times; Or add the water of the citric acid that contains 0.1~0.5% or aqueous ethanolic solution to dilute 5~20 times.
The step of described wash-out is specially: 0.1~0.5% hydrochloric acid or 0.1~0.5% aqueous citric acid solution drip washing resin column that utilize 5~20BV resin volume, with the pigment of the aqueous ethanolic solution desorption macroporous adsorbent resin institute enrichment of the citric acid containing 0.1~0.5% hydrochloric acid or 0.1~0.5%, in described aqueous ethanolic solution, the volumetric concentration of ethanol is preferably 30~80% afterwards.In addition, the present invention also preferably includes vacuum and reclaims the ethanol in described feed liquid, and vacuum tightness is preferably 0~-0.09MPa, temperature is preferably 40 ℃~100 ℃.After ethanol in reclaiming feed liquid, preferably in described feed liquid, add 2~10 times of deionized water dilutions.
In addition, the present invention is carrying out feed liquid also to preferably include before ion exchange chromatography: the filtering with microporous membrane that is 1.0~0.1 μ m by described filtration via hole diameter, described millipore filtration preferably include polypropylene (PP) film, ceramic membrane or sand stick etc. one or more, for filtering out the graininess impurity of feed liquid.Described ion exchange chromatography resin is one or more in polymeric amide, polyacrylic acid and polystyrene.The moving phase of described ion exchange chromatography is for containing the water-soluble solvent of 0.05~0.5% hydrochloric acid or containing 0.05~0.5% or the water-soluble solvent of citric acid, preferably, for containing the water-soluble solvent of 0.05~0.15% hydrochloric acid or containing 0.05~0.15% or the water-soluble solvent of citric acid, for example, the aqueous solution of one or more in the water-soluble solvent such as the ethanol of hydrochloric acid or citric acid, methyl alcohol, acetone.The flow rate of mobile phase of described ion exchange chromatography is preferably 0.1~2BV/h, and more preferably 0.2~1.8BV/h, most preferably is 0.5~1.5BV/h.
The present invention utilizes chromatographic theory, relies on the difference of the dissolving partition ratio of different substances in chromatography media and moving phase, makes the Ipomoea batatas(L.)Lam in Ipomoea batatas(L.)Lam extracting solution occur completely separated with impurity in chromatography column.The present invention be take ion exchange chromatography resin as ion-exchanger, by feed liquid is carried out to ion exchange chromatography, by small molecules degradation product residual in feed liquid, polysaccharide and the Impurity removal approaching with Ipomoea batatas(L.)Lam adsorption effect, thereby Ipomoea batatas(L.)Lam purity is improved, the peculiar smell such as odorless, " rotten Ipomoea batatas " taste and bitter taste.
Described feed liquid is being carried out after ion exchange chromatography, and the present invention also preferably includes the described chromatographic solution that contains Ipomoea batatas(L.)Lam through nanofiltration membrane (NF film) purifying.This nanofiltration membrane is preferred for the daltonian molecule of molecular weight cut-off 100~500, and the look valency that obtains concentrated solution after nanofiltration membrane purifying is preferably 10~100.After nanofiltration membrane purifying, also preferably include: in described chromatographic solution after nanofiltration membrane purifying, add maltodextrin, after spraying is dry, obtain Ipomoea batatas(L.)Lam powder.The DE value of described maltodextrin is preferably 10~24, and more preferably 15~20.The present invention concentrates by adopting nanofiltration membrane to carry out purifying to the chromatographic solution that contains Ipomoea batatas(L.)Lam, the generation of the phenomenons such as the degraded easily producing in the time of can avoiding adopting heating means to process, polymerization.The good water solubility of the potato pigment obtaining after above-mentioned processing, aqueous solution clarity is high.In addition, the look valency of the sweet potato haematochrome powder that the present invention is prepared can reach E1% >=200, high more a lot of than the E1%≤60 sweet potato haematochrome purity of preparing in prior art.The photostabilization of gained Ipomoea batatas(L.)Lam of the present invention, thermotolerance can improve more than 20%~30%.In addition, the present invention extracts and can carry out serialization production the pigment in Rhizoma Dioscoreae esculentae, and production efficiency is high, pigment extraction yield can reach more than 90%, the solvent adopting, moving phase, resin, fixing equal all recyclable the reusing of chromatography, be suitable for industrialized production and amplify, and Environmental Safety.
In order to further illustrate technical scheme of the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these are described is for further illustrating the features and advantages of the present invention, rather than limiting to the claimed invention.
The chemical reagent adopting in the embodiment of the present invention is commercial.
Embodiment 1
500Kg Rhizoma Dioscoreae esculentae silk by cleaning up, after chopping is put in an extractor in " level Four Continuous Countercurrent Extraction " system, utilize the extraction solvent of upper level containing the deionized water of 0.1%~0.5% hydrochloric acid, to carry out first step lixiviate, 30 ℃ of temperature, time 3.5h, solid-to-liquid ratio is 1: 7, emit extracting solution, by 400 mesh filter screens, filter, obtain filtrate;
Described filtrate is passed through to HZ816 polymeric adsorbent, after resin absorption is saturated, stop material loading, continue 0.1~0.5% the aqueous hydrochloric acid drip washing resin column with 8BV resin volume, use afterwards the pigment of the aqueous ethanolic solution desorption macroporous adsorbent resin institute enrichment of the hydrochloric acid that contains 0.1~0.5%, the volumetric concentration of described aqueous ethanolic solution is 80%; Then the pigment solution after desorption is reclaimed to ethanol under-0.08MPa, 75 ℃ of conditions, to recycle, then, to the hydrochloric acid dilution that adds 10 times 0.1~0.5% in the pigment solution obtaining, diluent, by 0.8um ceramic membrane, obtains feed liquid; By described feed liquid, by chromatographic resin bed, 15% aqueous ethanolic solution containing 0.1~0.5% hydrochloric acid of take is moving phase, with the flow velocity of 0.35BV/h, carries out chromatography, obtains chromatographic solution; Afterwards chromatographic solution is concentrated into 60 look valencys by nanofiltration membrane; To add in described chromatographic solution after concentrated with concentrated after the DE value that equates of the chromatographic solution quality maltodextrin that is 18, stirring and dissolving is complete, the spray-dried purple sweet potato haematochrome powder of making under 180 ℃~190 ℃ conditions.
Measure in accordance with the following methods the performance index of Ipomoea batatas(L.)Lam prepared by the present embodiment.
The detection method of look valency: taking quality is the pigment sample of 0.2g (being accurate to 0.0001g), the citric acid-sodium citrate damping fluid that is 3.0 with pH value dissolves, is settled in 100ml volumetric flask, shake up this solution of rear extraction 1.0ml to another 100ml volumetric flask, with above-mentioned damping fluid dilution, constant volume, after shaking up, be test solution to be measured.Take above-mentioned damping fluid as reference liquid, the wide cuvette of 1cm, utilizing ultraviolet-visible spectrophotometer is 530nm place detection absorbance A at wavelength.
Look valency E1%=A/M*100
Smell: the sweet potato haematochrome liquid after going nanofiltration membrane concentrated, at room temperature after airtight placement 24h in standard sensory evaluation chamber, judge smell, more than judging personnel 3 people.
Flavour: purple sweet potato haematochrome pulvis is configured to 1% solution with distilled water, judges the flavour of this pigment solution.
Utilize said determination method to obtain, the absorbance of Ipomoea batatas(L.)Lam prepared by the present embodiment is 217.4, and look valency is 120, aqueous solution clear, without water-insoluble, pigment aqueous solution is without " rotten Ipomoea batatas " taste, without bitter taste, odorless, and 0.01% the aqueous solution is fast light.
Embodiment 2
500Kg Rhizoma Dioscoreae esculentae silk by cleaning up, after chopping is put in an extractor in " level Four Continuous Countercurrent Extraction " system, utilize the extraction solvent of upper level containing 50% ethanolic soln water of 0.1%~0.5% citric acid, to carry out first step lixiviate, 25 ℃ of temperature, time 2.5h, solid-to-liquid ratio is 1: 8, emit extracting solution, by 400 mesh filter screens, filter, obtain filtrate;
Described filtrate is led under-0.08MPa, 75 ℃ of conditions and reclaimed ethanol, ethanol recycles, then in resulting pigment solution, add 10 times of 0.1% citric acid water dilutions to pass through afterwards HZ816 polymeric adsorbent, after resin absorption is saturated, stop material loading, continue 0.1~0.5% the aqueous citric acid solution drip washing resin column with 8BV resin volume, use afterwards the pigment of the aqueous ethanolic solution desorption macroporous adsorbent resin institute enrichment of the citric acid that contains 0.1~0.5%, the volumetric concentration of described aqueous ethanolic solution is 70%; Pigment solution after desorption is reclaimed to ethanol under-0.08MPa, 75 ℃ of conditions, and to recycle, then, to the citric acid water dilution that adds 13 times 0.1~0.5% in the pigment solution obtaining, diluent, by 0.45um ceramic membrane, obtains feed liquid; By described feed liquid, by chromatographic resin bed, 15% aqueous ethanolic solution containing 0.1~0.5% citric acid of take is moving phase, with the flow velocity of 0.25BV/h, carries out chromatography, obtains chromatographic solution; Afterwards received feed liquid is passed through to NF membrane concentration to 65 look valency; To add in described chromatographic solution after concentrated with concentrated after the DE value that equates of the chromatographic solution quality maltodextrin that is 18, stirring and dissolving is complete, the spray-dried purple sweet potato haematochrome powder of making under 180 ℃~190 ℃ conditions.
Adopt measuring of Ipomoea batatas(L.)Lam that the measuring method identical with embodiment 1 prepared the present embodiment, result is: the look valency of Ipomoea batatas(L.)Lam prepared by the present embodiment is 140, aqueous solution clear, without water-insoluble, pigment aqueous solution is without " rotten Ipomoea batatas " taste, without bitter taste, odorless, and 0.01% the aqueous solution is fast light good.
Above-mentioned explanation to the disclosed embodiments, makes professional and technical personnel in the field can realize or use the present invention.To the multiple modification of these embodiment, will be apparent for those skilled in the art, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.