CN1834163A - Method of producing purpureal sweet potato haematochrome - Google Patents
Method of producing purpureal sweet potato haematochrome Download PDFInfo
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- CN1834163A CN1834163A CN 200610078643 CN200610078643A CN1834163A CN 1834163 A CN1834163 A CN 1834163A CN 200610078643 CN200610078643 CN 200610078643 CN 200610078643 A CN200610078643 A CN 200610078643A CN 1834163 A CN1834163 A CN 1834163A
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Abstract
This invention discloses a safe and highly efficient method for extracting purple sweet potato color with a high purity, which comprises the steps of: beating fresh purple sweet potatos, extracting with citric acid aqueous solution, cooling the extraxted solution, centrifuging, inactivating enzymes, performing a first time separation and purification with a microfiltration membrane, concentrating with a nanofiltration membrane, coupling the concentrated solution with resin, performing a second time separation and purification, and concentrating in vacuum to obtain the final product. The use of nanofiltration membrane and the coupling of the membrane with the resin can elongate the service life of the resin as well as raise the adsorption efficiency of the resin. The use of nanofiltration membrane for concentrating the color solution can effectively reduce the manufacturing cost and prevent degradation of the color solution at a high temperature, thus can protect the physiological functions of the color from being damaged.
Description
Technical field
The present invention relates to a kind of production method for preparing purple sweet potato haematochrome, belong to medicine, food, protective foods, makeup processed and applied technical field.
Background technology
Along with people's living standard improves, more and more higher to the requirement of food color.Therefore, synthetic food color just extensively is added in the food, to increase the assortment of food, improves the appetite of people sense.Yet, because synthetic food color more and more is subjected to people's attention to the harm that human body causes, uses that be under an embargo in succession of many synthetic food colors, even stop production.Therefore, from plant, extract natural pigment and cause people's interest again, its development and utilization becomes a big research focus, major cause is that natural pigment is directed to animals and plants and microorganism, be not only tinting materials such as food, medicine, makeup, and self also contain multiple nutritional components, have to the effective in cure effect of some disease, human body is had nourishing function.
Rhizoma Dioscoreae esculentae is the special kinds of sweet potato, because of its potato meat is rich in pigment, causes many scholars' concern as a kind of important natural pigment source.Purple sweet potato haematochrome is a kind of natural pigment that lixiviate is come out from the piece root of Rhizoma Dioscoreae esculentae and cauline leaf, and the vivid nature of color and luster is nontoxic, and no special odor has multiple nutrients, pharmacology and nourishing function, is a kind of ideal natural food colour resource.At present, the greatest problem that natural colorant exists is exactly most unstable in product, has therefore influenced its application in industry to a certain extent.But document announcement is arranged, and the pigment molecular of acylations can make the stability of pigment improve.Because the Rhizoma Dioscoreae esculentae pigment molecular is the pigment molecular of acylations, so its stability is stronger, application prospect is extensive.
Purple sweet potato haematochrome presents bright-coloured redness under acidic conditions, now be widely used in ice-creams, dairy beverage, cheese, fishery products, nectar, jelly, cereal.Simultaneously, because purple sweet potato haematochrome has anti-mutation, antioxygenation, physiological function such as antitumor, medicine and cosmetic industry have been widely used in.
At present acidifying ethanol or acidifying methyl alcohol are adopted in the extraction of purple sweet potato haematochrome more, cause dissolvent residual to a certain extent, and extraction yield all not very high.Adopt resin to the pigment separation and purification, because the existence of impurity such as protein, carbohydrate in the pigment makes that the work-ing life of resin is shorter, product purity is lower.Single employing vacuum concentration or spray thing drying concentrate product or are dry, make pigment easily degrade under hot conditions, owing to the mass consumption of the energy, have strengthened the cost of subsequent technique.
Summary of the invention
The objective of the invention is to provide a kind of production method of purple sweet potato haematochrome, this method make pigment extraction yield height, do not have dissolvent residual, the work-ing life and the adsorptive power that has strengthened resin of resin have been prolonged simultaneously, avoid pigment under hot conditions, to degrade, advantageously prevent the oxidation of purple sweet potato haematochrome, simultaneously purification efficiency and product purity are improved greatly.
In order to reach the technical scheme that purpose of the present invention takes be:
Light violet sweet potato making beating back is extracted with aqueous citric acid solution, the enzyme that goes out after the extracting solution cooling is centrifugal, after microfiltration membrane flash trapping stage purifying, nanofiltration membrane concentrated, concentrated solution and resin coupling were used and are carried out the secondary separation and purification, and last vacuum concentration obtains product.
In the production method of above-mentioned purple sweet potato haematochrome, adopt aqueous citric acid solution to extract, 10～70 ℃ of extraction temperature, the extraction time is 0.5h～10h, and liquid-solid ratio is 1: 1～1: 5, and aqueous citric acid solution concentration is 0.1%～0.5%.
In the production method of above-mentioned purple sweet potato haematochrome, enzyme that Rhizoma Dioscoreae esculentae extracting solution cooling is gone out after centrifugal, 80～150 ℃ of temperature, time: 1～10min.
In the production method of above-mentioned purple sweet potato haematochrome, centrifugal back pigment solution carries out the flash trapping stage purifying through microfiltration membrane.One-level purifies and separates condition is: the microfiltration membrane material is pottery or polyethers sulfoxide, and membrane pore size is 10～1500nm, working pressure 0.5MP～5MP, and temperature is 20～60 ℃, flux is 15～100ml/min.
In the production method of above-mentioned purple sweet potato haematochrome, carry out the pigment solution that the flash trapping stage purifying obtains through microfiltration membrane and adopt nanofiltration membrane to carry out concentration technology.The nanofiltration membrane material is a ceramic membrane, molecular weight cut-off 50～200 dalton, and working pressure 0.5MP～5MP, temperature is 30～50 ℃, flux is 25～100ml/min.
In the production method of above-mentioned purple sweet potato haematochrome, will concentrate the coupling of back pigment solution and resin and use, carry out the secondary separation and purification.Secondary purifies and separates condition is: resin model AB-8 or 3520, adsorption temp is 20～60 ℃, the optimal pH 1～3 of resin absorption solution, the optimum ratio of resin quality and strength of solution: 1 (g): 35 (mg/1000g)～1 (g): 150 (mg/1000g), flow velocity 10～30VB/h, elutriant concentration 45～80%, eluent flow rate 2～10VB/h, 25～40 ℃ of eluting temperatures.
In the production method of above-mentioned purple sweet potato haematochrome,, obtain paste and be purple sweet potato haematochrome, 40 ℃～60 ℃ of temperature through vacuum concentration.
The present invention adopts membrane sepn and concentration technique first in the production of purple sweet potato haematochrome, handle the clear liquid that obtains through film, what contain nearly all is water colo(u)r, carbohydrate, protein and a large amount of water, different according to the molecular weight of these compositions and physical and chemical performance, membrane filtration is a kind of the most effective the simplest separation method that can not introduce any tramp material again.Micro-filtrate membrane filtration efficient is relevant with the material of film.The microfiltration membrane of using when the present invention filters is ceramic membrane or polyethers sulfoxide.Utilize method of the present invention, can from the 1000ml stock liquid, obtain qualified liquid purple sweet potato haematochrome product 500～700ml.
The production method of purple sweet potato haematochrome of the present invention compared with prior art has following advantage:
1, the pigment solution that extracts through microfiltration membrane carry out the flash trapping stage purifying concentrate after and the resin coupling use, carry out the secondary separation purifying.Not only prolong the work-ing life of resin, also improved the purity of the adsorption efficiency and the product of resin simultaneously greatly.
2, pigment solution carries out nanofiltration and concentrates behind the flash trapping stage purifying, and not only the subsequent technique cost reduces, and effectively prevents the pigment degraded simultaneously, and physiological function such as anti-oxidant obtains effectively protection.
3, adopt aqueous citric acid solution to extract, the enzyme that goes out after the extracting solution cooling is centrifugal, extraction yield height not only, and do not have problem of solvent residue.
Embodiment
Embodiment 1:
1, extracts 10 ℃ of extraction temperature, time 0.5h, liquid-solid ratio 1: 1, extraction progression 2 times with 0.1% aqueous citric acid solution;
2, extracting solution is cooled off the enzyme that goes out after centrifugal, 80 ℃ of enzyme-removal temperatures, time 1min, the rate of carrying reaches 95%;
3, extracting solution is carried out separation and purification through microfiltration membrane, mould material is a ceramic membrane, and membrane pore size is 10nm, and working pressure is 0.5MP, and service temperature is 20 ℃, and flux is 15ml/min;
4, with the pigment solution process nanofiltration membrane of flash trapping stage purifying, mould material is a ceramic membrane, molecular weight cut-off 50 dalton, and working pressure 5MP, service temperature is 30 ℃, and flux is 100ml/min, and cycles of concentration can reach 7 times, and the look valency is 25;
5, the pigment solution with the flash trapping stage purifying concentrates back and resin coupling use carrying out secondary separation and purification, resin model AB-8,40 ℃ of adsorption temps, pH1, the optimum proportion of resin quality and pigment concentration is 1 (g): 35 (mg/1000g), flow velocity 10VB/h, elutriant concentration 55%, eluent flow rate 3VB/h, 25 ℃ of eluting temperatures.Adsorption rate reaches 96%, and the look valency is 45;
6, secondary separation and purification liquid obtains the finished product through vacuum concentration.The vacuum concentration temperature: 40 ℃, product look valency is 60.
Embodiment 2:
1, extracts 30 ℃ of extraction temperature, time 5h, liquid-solid ratio 1: 2.5, extraction progression 2 times with 0.2% aqueous citric acid solution;
2, extracting solution is cooled off the enzyme that goes out after centrifugal, 120 ℃ of enzyme-removal temperatures, time 5min, extraction rate reached to 98%;
3, extracting solution is carried out separation and purification through microfiltration membrane, mould material is a polymeric amide, and membrane pore size is 100nm, and working pressure is 2.5MP, and service temperature is 40 ℃, and flux is 50ml/min;
4, with the pigment solution process nanofiltration membrane of flash trapping stage purifying, mould material is a ceramic membrane, molecular weight cut-off 80 dalton, and working pressure 4MP, service temperature is 45 ℃, and flux is 100ml/min, and cycles of concentration can reach 6 times, and the look valency is 30;
5, the pigment solution with the flash trapping stage purifying concentrates and resin coupling use carrying out secondary separation and purification, resin model 3520,40 ℃ of adsorption temps, pH1, the optimum proportion of resin quality and pigment concentration are 1 (g): 70 (mg/1000g), flow velocity 5VB/h, elutriant concentration 70%, eluent flow rate 2VB/h, 30 ℃ of eluting temperatures, adsorption rate arrives 94%, look valency 40;
6, secondary separation and purification liquid obtains the finished product through vacuum concentration.The vacuum concentration temperature: 40 ℃, product look valency is 50.
Embodiment 3:
1, extracts 70 ℃ of extraction temperature, time 10h, liquid-solid ratio 1: 5, extraction progression 2 times with 0.3% aqueous citric acid solution;
2, extracting solution is cooled off the enzyme that goes out after centrifugal, 150 ℃ of enzyme-removal temperatures, time 10min, extraction yield 96%;
3, extracting solution is carried out separation and purification through microfiltration membrane, mould material is a polymeric amide, and membrane pore size is 1200nm, and working pressure is 5MP, and service temperature is 40 ℃, and flux is 80ml/min;
4, with the pigment solution process nanofiltration membrane of flash trapping stage purifying, mould material is a ceramic membrane, molecular weight cut-off 100 dalton, and working pressure 4MP, service temperature is 45 ℃, and flux is 100ml/min, and cycles of concentration can reach 6 times, and the look valency is 25;
5, the pigment solution with the flash trapping stage purifying concentrates back and resin coupling use carrying out secondary separation and purification, resin model AB-8,30 ℃ of adsorption temps, pH2, the optimum proportion of resin quality and pigment concentration are 1 (g): 105 (mg/1000g), flow velocity 7VB/h, elutriant concentration 80%, eluent flow rate 4VB/h, 25 ℃ of eluting temperatures, adsorption rate reaches 92%, and the look valency is 35;
6, secondary separation and purification liquid obtains the finished product through vacuum concentration.The vacuum concentration temperature: 40 ℃, product look valency is 45.
Embodiment 4:
1, extracts 50 ℃ of extraction temperature, time 5h, liquid-solid ratio 1: 4, extraction progression 2 times with 0.4% aqueous citric acid solution;
2, extracting solution is cooled off the enzyme that goes out after centrifugal, 110 ℃ of enzyme-removal temperatures, time 8min, extraction yield 94%;
3, extracting solution is carried out separation and purification through microfiltration membrane, mould material is a polymeric amide, and membrane pore size is 1200nm, and working pressure is 3MP, and service temperature is 30 ℃, and flux is 80ml/min;
4, with the pigment solution process nanofiltration membrane of flash trapping stage purifying, mould material is a ceramic membrane, molecular weight cut-off 150 dalton, and working pressure 4MP, service temperature is 45 ℃, and flux is 100ml/min, and cycles of concentration can reach 4 times, and the look valency is 20;
5, the pigment solution with the flash trapping stage purifying concentrates back and resin coupling use carrying out secondary separation and purification, resin model XAD-1600,30 ℃ of adsorption temps, pH3, the optimum proportion of resin quality and pigment concentration are 1 (g): 125 (mg/1000g), flow velocity 7VB/h, elutriant concentration 80%, eluent flow rate 4VB/h, 25 ℃ of eluting temperatures, adsorption rate reaches 92%, and the look valency is 30;
6, secondary separation and purification liquid obtains the finished product through vacuum concentration.The vacuum concentration temperature: 40 ℃, product look valency is 40.
Embodiment 5:
1, extracts 70 ℃ of extraction temperature, time 10h, liquid-solid ratio 1: 5, extraction progression 2 times with 0.5% aqueous citric acid solution;
2, extracting solution is cooled off the enzyme that goes out after centrifugal, 150 ℃ of enzyme-removal temperatures, time 10min, extraction yield 97%;
3, extracting solution is carried out separation and purification through microfiltration membrane, mould material is a polymeric amide, and membrane pore size is 1200nm, and working pressure is 5MP, and service temperature is 40 ℃, and flux is 80ml/min;
4, with the pigment solution process nanofiltration membrane of flash trapping stage purifying, mould material is a ceramic membrane, molecular weight cut-off 200 dalton, and working pressure 4MP, service temperature is 45 ℃, and flux is 100ml/min, and cycles of concentration can reach 5 times, and the look valency is 15;
5, the pigment solution with the flash trapping stage purifying concentrates back and resin coupling use carrying out secondary separation and purification, resin model 3520,30 ℃ of adsorption temps, pH1, the optimum proportion of resin quality and pigment concentration are 1 (g): 150 (mg/1000g), flow velocity 8VB/h, elutriant concentration 65%, eluent flow rate 4VB/h, 25 ℃ of eluting temperatures, adsorption rate reaches 92%, and the look valency is 25;
6, secondary separation and purification liquid obtains the finished product through vacuum concentration.The vacuum concentration temperature: 40 ℃, product look valency is 35.
Claims (7)
1. the production method of a purple sweet potato haematochrome, it is characterized in that: light violet sweet potato making beating back is extracted with aqueous citric acid solution, enzyme goes out after the extracting solution cooling is centrifugal, after microfiltration membrane flash trapping stage purifying, nanofiltration membrane concentrate, concentrated solution and resin coupling are used and are carried out the secondary separation and purification, and last vacuum concentration obtains product.
2. according to the described purple sweet potato haematochrome production method of claim 1, it is characterized in that: in the purple sweet potato haematochrome production method, 10～70 ℃ of extraction temperature, time 0.5h～10h, liquid-solid ratio 1: 1～1: 5, citric acid concentration 0.1%～0.5%.
3. according to the described purple sweet potato haematochrome production method of claim 1, it is characterized in that: with Rhizoma Dioscoreae esculentae extracting solution cooling centrifugal after, 80～150 ℃ of temperature, enzyme goes out under time 1～10min condition.
4. according to the described purple sweet potato haematochrome production method of claim 1, it is characterized in that: in the purple sweet potato haematochrome production method, one-level purifies and separates condition is: the microfiltration membrane material is pottery or polyethers sulfoxide, membrane pore size is 10～1500nm, working pressure is 0.5～5MP, 20～60 ℃ of service temperatures, flux are 15～100ml/min.
5. according to the described purple sweet potato haematochrome production method of claim 1, it is characterized in that: the condition of carrying out concentration technology by nanofiltration membrane is: mould material is a ceramic membrane, molecular weight cut-off 50～200 dalton, working pressure is 0.5MP～5MP, 30～50 ℃ of service temperatures, flux are 25～100ml/min.
6. according to the described purple sweet potato haematochrome production method of claim 1, it is characterized in that: secondary purifies and separates condition is: resin model AB-8 or 3520, adsorption temp is 20～60 ℃, the optimal pH 1～3 of resin absorption solution, the optimum ratio of resin quality and strength of solution: 1 (g): 35 (mg/1000g)～1 (g): 150 (mg/1000g), flow velocity 10～30VB/h; Macroporous adsorbent resin to the dynamic desorption condition of purple sweet potato haematochrome is: elutriant concentration 45～80%, eluent flow rate 2～10VB/h, 25～40 ℃ of eluting temperatures.
7. according to the described purple sweet potato haematochrome production method of claim 1, it is characterized in that: the vacuum concentration temperature is 40 ℃～60 ℃.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2096146A1 (en) * | 2008-02-29 | 2009-09-02 | San-Ei Gen F.F.I., Inc. | Deodorized plant pigment derived from Ipomoea Batatas |
| CN101525499A (en) * | 2008-02-29 | 2009-09-09 | 三荣源有限公司 | Deodorized plant colorant derived from Ipomoea Batatas |
| CN101768370A (en) * | 2008-12-30 | 2010-07-07 | 天津市食品工业生产力促进中心 | Method for extracting and purifying natural high-purity red pigment from purple sweet potatoes |
| CN101186757B (en) * | 2007-12-24 | 2010-10-06 | 钱生球 | Method for producing purple sweet potato haematochrome |
| CN101962486A (en) * | 2010-08-26 | 2011-02-02 | 永康市毕尔锐思生物技术有限公司 | Industrial production method for extracting natural purple sweet potato coloring matter for food from edible purple sweet potato |
| CN102206426A (en) * | 2011-03-23 | 2011-10-05 | 武汉普赛特膜技术循环利用有限公司 | Comprehensive utilization of pigment of purple sweet potato in purple sweet potato and method for comprehensively utilizing component thereof |
| CN101305797B (en) * | 2008-07-17 | 2011-11-16 | 江西国亿生物科技有限公司 | Carotin preparation method and its carotin products |
| CN102391669A (en) * | 2011-11-08 | 2012-03-28 | 北京工业大学 | Natural haematochrome extracted from sweet potato skin and preparation method thereof |
| CN102516807A (en) * | 2011-12-29 | 2012-06-27 | 江苏久吾高科技股份有限公司 | Method for extracting purple sweet photo anthocyanidin from ceramic membrane |
| CN107467122A (en) * | 2017-08-31 | 2017-12-15 | 兰溪市捷喜食品加工技术有限公司 | A kind of beauty treatment bread and preparation method thereof |
| CN109618980A (en) * | 2018-12-14 | 2019-04-16 | 宣城九只鸭健康科技有限公司 | A kind of method that crack position of crack egg is determining, repairs and recycles |
| CN112442285A (en) * | 2019-08-27 | 2021-03-05 | 湖南省天香生物科技有限责任公司 | Preparation method of purple sweet potato pigment |
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- 2006-04-29 CN CN 200610078643 patent/CN1834163A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186757B (en) * | 2007-12-24 | 2010-10-06 | 钱生球 | Method for producing purple sweet potato haematochrome |
| CN101525499A (en) * | 2008-02-29 | 2009-09-09 | 三荣源有限公司 | Deodorized plant colorant derived from Ipomoea Batatas |
| EP2096146A1 (en) * | 2008-02-29 | 2009-09-02 | San-Ei Gen F.F.I., Inc. | Deodorized plant pigment derived from Ipomoea Batatas |
| CN101305797B (en) * | 2008-07-17 | 2011-11-16 | 江西国亿生物科技有限公司 | Carotin preparation method and its carotin products |
| CN101768370A (en) * | 2008-12-30 | 2010-07-07 | 天津市食品工业生产力促进中心 | Method for extracting and purifying natural high-purity red pigment from purple sweet potatoes |
| CN101962486A (en) * | 2010-08-26 | 2011-02-02 | 永康市毕尔锐思生物技术有限公司 | Industrial production method for extracting natural purple sweet potato coloring matter for food from edible purple sweet potato |
| CN101962486B (en) * | 2010-08-26 | 2013-06-26 | 浙江毕尔锐思生物技术有限公司 | Industrial production method for extracting natural purple sweet potato coloring matter for food from edible purple sweet potato |
| CN102206426A (en) * | 2011-03-23 | 2011-10-05 | 武汉普赛特膜技术循环利用有限公司 | Comprehensive utilization of pigment of purple sweet potato in purple sweet potato and method for comprehensively utilizing component thereof |
| CN102391669A (en) * | 2011-11-08 | 2012-03-28 | 北京工业大学 | Natural haematochrome extracted from sweet potato skin and preparation method thereof |
| CN102516807A (en) * | 2011-12-29 | 2012-06-27 | 江苏久吾高科技股份有限公司 | Method for extracting purple sweet photo anthocyanidin from ceramic membrane |
| CN102516807B (en) * | 2011-12-29 | 2014-03-19 | 江苏久吾高科技股份有限公司 | Method for extracting purple sweet photo anthocyanidin from ceramic membrane |
| CN107467122A (en) * | 2017-08-31 | 2017-12-15 | 兰溪市捷喜食品加工技术有限公司 | A kind of beauty treatment bread and preparation method thereof |
| CN109618980A (en) * | 2018-12-14 | 2019-04-16 | 宣城九只鸭健康科技有限公司 | A kind of method that crack position of crack egg is determining, repairs and recycles |
| CN112442285A (en) * | 2019-08-27 | 2021-03-05 | 湖南省天香生物科技有限责任公司 | Preparation method of purple sweet potato pigment |
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