CN101311225A - Process for abstracting kohlrabi pigment - Google Patents
Process for abstracting kohlrabi pigment Download PDFInfo
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- CN101311225A CN101311225A CNA2007101094010A CN200710109401A CN101311225A CN 101311225 A CN101311225 A CN 101311225A CN A2007101094010 A CNA2007101094010 A CN A2007101094010A CN 200710109401 A CN200710109401 A CN 200710109401A CN 101311225 A CN101311225 A CN 101311225A
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Abstract
The invention discloses an extraction method for baga pigment, which takes fresh baga roots as the raw material and comprises the steps of ethanol immersion, liquid smash, solid-liquid separation, and one step completion of reduced pressure distillation, concentration and drying; wherein, the pressure of the reduced pressure distillation is reduced to less than or equal to 1000Pa and the temperature is controlled less than or equal to 50 DEG C. Ethanol is recycled in the process of reduced pressure distillation and the influence of heating is avoided in the whole process of water evaporation to dryness, thus achieving the purposes of keeping the extracted baga haematochrome beautiful in color and reserving the biological activity of the natural product.
Description
Technical field
The present invention relates to natural pigment extraction process, particularly process for abstracting kohlrabi pigment.
Technical background
The climing mountain valley with clumps of trees and bamboo (Brassica campetris L.ssp.ropiera. English name: Turnip) belong to the climing mountain valley with clumps of trees and bamboo subspecies of Cruciferae rape kind, it is excellent to be that dietotherapy is held concurrently, has long greengrocery plant among the people, it in NW YUNNAN area, the Yunnan Province of China traditional dish of all of a sudden making, climing mountain valley with clumps of trees and bamboo root is very large, be rose, color is gorgeous, is the high-quality natural food colour.
Food dye is very important raw materials for food industry, and early stage pigment source early in the twentieth century still using in food, but the manufacturer has been eliminated them under the ordering about of economic interests gradually in plant, animal and mineral raw material.The production technique of chemosynthesis pigment is simple, and is cheap, and dyeing behavior is very desirable, and consumption is little, can not produce bad flavor to food.But growth along with the synthetic colour usage quantity.Safety problem causes people's attention gradually.Many rules have been put into effect in countries in the world as a result, and the synthetic colour of ratifying as the U.S. falls sharply to 7 kinds from 700 kinds.Yet food is adulterated and has still been continued many years.And they are in recent years to food color and healthy singular news media, have promoted the concern of human consumer to pigment additive in the food jointly.Present food color market scale is not also had reliable statistical figure, but estimate that substantially there is 9.4 hundred million dollars the volume of trade every year in the whole world.The each several part portion is: 400,000,000 dollars of synthetic colours, 2.5 hundred million dollars of natural pigments, 1.89 hundred million dollars of natural origin pigments, 100,000,000 dollars of caramel colorants.The development that the transition of human consumer's pressure, society and development of technology have greatly promoted food-processing industry has driven food color market simultaneously comprehensively.Along with the human consumer increases day by day to the interest of pure natural food, the share of natural pigment on market increases sharply.It is predicted.Several years natural pigments in future will increase with 5～10% speed every year.The safe edible synthetic colour also can be stablized increase, but annual growth is between 3～5%.The food color that China approved allows to use has 65 kinds, wherein 48 kinds of plant milk extracts [Liu Lianfang. the new variety of Food Additives Used in China, new development [J] foodstuffs industry science and technology .1999, (3)].
Market requirement increase along with food dye, the natural pigment technology continues to bring out, but still there is certain defective in existing technology, as, patent gazette discloses 200410065617.8 " dragon fruit pulps, extract the method for water-soluble red colouring matter in the pericarp " this method thaws by make the cell walls room temperature that rises broken afterwards-18 ℃～-23 ℃ sharp freezings, crushing, centrifugation gets parting liquid, slag is leached extracting solution with ethanol again, merge parting liquid and extracting solution, adopt distillation to be concentrated into the spissated glue pigment concentrate that contains then, further add ethanol again and come unstuck, moisture is removed in reverse osmosis, the dry product that gets.The defective of this technology is, given removal moisture operation adopts reverse osmosis, and reverse osmosis step can not be removed moisture, and the minimum needs of the working fluid of reverse osmosis system moisture 70% just might be in the thrust current downflow of fluid pump.This method of Gazette of Patent for Invention disclosed 02117769.4 " extracting method of Alkannia " uses carbonic acid gas to be solvent, extract by supercritical, high pressure extraction kettle system, though this method can obtain the higher alkannin of purity, but its defective is, the carbonic acid gas solvent only is suitable for the extraction of fat-soluble component, can't extract for water soluble component, secondly be, keeping the safety in production in the high top pressure operation of 15～20Mpa has certain threat.This method of patent gazette disclosed 98112151.9 " a kind of red heart square-bottomed bamboo basket that utilizes is foretold the method that the edible square-bottomed bamboo basket of extraction is foretold haematochrome " adopts hydrochloric acid soln lixiviate, and by the employing resin absorption, by concentrating under reduced pressure, spraying drying obtains product more then.The defective of this method is to adopt the waste water of hydrochloric acid soln lixiviate to environmental influence, secondly the inevitable resin wear of resin absorption process is to the pollution of food dye, studies show that, the problem of big empty resin in application mainly shows, macroporous resin is a vinylbenzene matrix type resin, pore-creating agent is an alkanes, harmful material [Ceng Changrong such as its residue and split product benzene, toluene, vinylbenzene, toluylene, alkanes, macroporous resin residue limit examine research in the Chinese medical extract, CHINA JOURNAL OF CHINESE MATERIA MEDICA, 2004,29 (6)].Spray-dired process is oxygen enrichment and high-temperature technology, pigment is produced urge oxidation affects.Disclosed 00105615.8 " from Asian puccoon, extracting the method for natural red colouring matter " this method employing hexane of patent gazette or acetone, sherwood oil, the lixiviate of ethyl acetate organic solvent, the defective of this method be the solvent that adopts residual inevitable in product, next is that these low boiling point solvents reclaim very difficulty in production technique, and environment is impacted.It is the solvent lixiviate that this method of disclosed 97115187.3 " preparation methods of natural alkannin " of patent gazette adopts hexane, then the extracting solution concentrating under reduced pressure is reclaimed a part of solvent, in order to obtain drying solid, it is that vehicle furnishing solution re-uses spraying drying that this method also needs to add emulsifier tween 80 (Tween80) corn dextrin.The defective of this method is, there are certain toxic side effect in residual extraction solvent and emulsifying agent in pigment product, and spray-dired oxygen enrichment operation exists oxidation to reduce the look valency and adds corn dextrin pigment and causes problems such as pigment content reduction.This process using of patent gazette disclosed 92104644.8 " extracting method of capsanthin " Na
2S
2O
5And Na
2The acetone soln of Cl extracts, and the major defect of this technology is the residual of noxious solvent acetone.This method of patent gazette disclosed 90101859.7 " a kind of natural edible red pigment and production technique thereof " is raw material with the poplar flower, use ethanol for extracting solvent, extracting solution is adopted concentrating under reduced pressure, and then employing spraying drying, problem of oxidation for fear of the spraying drying oxygen-enriched environment, this method gives, vacuum tightness is 600mmHg～700mmHg, dry in the loft drier that temperature is 30 ℃～50 ℃, according to the evaporating pressure of moisture and the character of vaporization temperature, the saturation vapour pressure of water under the environment of 30 ℃～50 ℃ of temperature is 31.82mmHg and the vast chief editor of 92.51mmHg[Jin nation, drying plant, chemical industry press, Beijing, 2002], the condition that provides of this method is to reach the exsiccant purpose.This method adopts and pull an oar, squeezes the juice patent gazette disclosed 96100493.2 " extracting the methods of purpurin from the red flesh square-bottomed bamboo basket is foretold ", press filtration, decoction, filtration, lyophilize, and purifying process adopts chloroform and primary isoamyl alcohol mixed solution to extract.The defective of this technology is, do not taking the processing step under the oxygen quarantine measures condition to make pigment composition oxidation under aerobic environment lose natural colored, and it is excellent in outstanding especially to decoct working-procedure problem.Secondly, this technology has also been used noxious solvent, and noxious solvent residual is to food applications security presence hidden danger.This method of the disclosed 02133563.x of patent gazette " a kind of preparation method of refined edible natural carthamin yellow " adopts Trisodium Citrate and acetic acid to adjust the pH of solvent, make solvent be acid, for avoiding the influence of leaching process pyritous, this method has provided relatively low extraction temperature (under 60 ℃ of constant temperature), but the final drying of this method has still been used the drying process with atomizing that needs high temperature evaporation, spraying drying need be in the inlet temperature more than 150 ℃, and the problem of oxidation of urging under high temperature and atmospheric condition all has certain influence to the oxidative deformation of carthamin with losing activity.
Natural pigment is the kind of biologically active particularly, great majority are aldehydes matters, with the Rose pigment is example, the Rose haematochrome mixes the blue precipitation of generation with neutral acetate, show that this pigment contains the phenolic group material, become tawny after the vibration of iron(ic) chloride colour developing experiment colour developing cellulose solution color, show and contain phenolic hydroxyl group in the pigment.Hydrochloric acid-magnesium powder reaction; Add the small amount of magnesium powder at roseleaf haematochrome extracting solution, after the vibration, add several hydrochloric acid again, pigment solution produces bubble, darkens.If do not add the magnesium powder, only adding hydrochloric acid does not then have the bubble generation, shows that this pigment belongs to flavonoid compound, can be by H under hydrochloric acid-magnesium powder effect
2Reduction [Cao Shaoqian, the roseleaf haematochrome extracts and be qualitative, Food science, 2007,28 (3)].By UV spectrum and high performance liquid chromatograph analysis, contain flavones and anthocyanogen two big class pigments in the Rose, its component is flavonols and Minor centaury pattern aglycon-3-glucoside [Feng Zuoshan, the purifying of rose pigment and composition preliminary evaluation, food science and technology, 2006,10].
Studies show that, contain aldehydes matter and be subjected to the thermogenesis objectionable impurities at leaching process, tea-polyphenol in the tealeaves, ginkgo, pick up with the fingers on the mountain, the root of large-flowered skullcap, Radix Glycyrrhizae, Flavonoid substances such as sea-buckthorn, all be that the further oxidation of semiquinone formula free radical promptly generates quinone, quinones substance can produce intense stimulus to people's skin eyes, can cause cornea dermal respiration road inflammation, quinones substance produces detrimentally affect to kidney, experiment shows that Quercetin is very fast in the decay of 82 ℃ of (ginkgo is extracted thickening temperature) oxidation initial stage Quercetins, oxidized away 70% in 8 hours, Egb (Semen Ginkgo extrac) is from be dosed into out product needed more than 200 hour [Ni Lijun, the oxidation of Quercetin and to Egb (Semen Ginkgo extrac) preparation process and quality influence, Chinese patent medicine, 2000,22 (12)].
Absorbancy by pigment proves the sensitization test of temperature, the thermo-sensitivity of temperature and urge oxidation effect can make the pigmental degeneration of numerous species, the absorbancy of peony haematochrome is extracted temperature and is surpassed 75 ℃ maximum below 75 ℃, and raising with temperature reduces, [He Ling, the research of peony red pigment extraction process, Xibei Univ. of Agricultural ﹠ Forest Science ﹠ Technology's journal, natural science edition, 2006,34 (12)].The Rose haematochrome extracts 50 ℃ of absorbancy maximums of temperature, and when surpassing 50 ℃, absorbancy reduces [Liu Zhiguo, the optimization of rose pigment extraction conditions, Wuhan University of Technology's journal, 2005,24 (1)] gradually.The extraction yield Yin Wendu of Flower of Garden Balsam pigment raises and reduces, when being higher than 70 ℃ particularly evident [Su Huina, the research of Flower of Garden Balsam pigment optimum extraction process, food science and technology, 2007,24 (1)].Extracting solution is heated 20 ℃～60 ℃ scopes, and absorption peak does not have considerable change, and when temperature rose to 80 ℃, maximum absorption band promptly changed [Tian Junlian, the extraction Study on Stability of edible red heart square-bottomed bamboo basket fore-telling pigment, chemistry world, 1992,5 phases].Square-bottomed bamboo basket is foretold haematochrome resistance to oxidation reductibility inequality [Chen Cunshe, the extraction of edible natural pigment and stability study thereof, research and development of natural products, 2001,13 (6)].The wild rose pigment is when being higher than 50 ℃, with temperature rising absorbancy descend gradually [Shi Xiuhua, wild rose pigment Study on extraction, Food Additives Used in China, 2006,1].The cowberry haematochrome extracts 30～90 ℃ of temperature, obviously reduces [Zhang Hua, the research of cowberry red pigment extraction process, Liaoning agricultural science and technology, 1998,2] when being higher than 70 ℃ of pigment yields.Fructus Choerospondiatis skin pigment Study on extraction shows, experimental temperature has significant difference from 30 ℃～120 ℃ pigment yields, 30～80 ℃ of pigment yields of temperature increase trend gradually, after temperature arrives 85 ℃, no longer increase on the contrary and reduce, arrive 120 ℃ of pigments almost nil [Liu Xiaogeng, the extraction research of Fructus Choerospondiatis pericarp pigment, Jiangxi agricultural journals, 1994,6 (2)].The alkannin extraction process shows, 37 ℃～100 ℃ of temperature, it is dark more to extract the high more pigmentary colours of temperature, this experimental results show that alkannin easily produces brown stain, [Wu Jinxia, the extraction of alkannin and stability in 37 ℃～100 ℃ scopes when temperature raises, Hebei University of Technology's journal, natural science edition, 1997,17 (supplementary issues)].The red flesh radish is extracted the evidence of haematochrome, and in 50 ℃ to the 80 ℃ temperature ranges, temperature is high more, and the pigment extracted amount of red flesh radish is low more.Wherein 50 ℃ and 60 ℃ differences of drying extraction total recovery between the processing are not remarkable, but total recoverys that both extract all are significantly higher than 70 ℃ and 80 ℃.The oven dry processing contrasts the total recovery of extracting with Exposure to Sunlight and also significantly is lower than 50 ℃ and 60 ℃ of oven dry processing, but is significantly higher than 70 ℃ and 80 ℃ of oven dry processing.Consider from save energy simultaneously, should select for use 50 ℃ of temperature as red flesh radish dried temperature, radish red pigment solution absorbency value reduces with holding time prolonging, high more its pigment degraded of temperature is fast more, after 40 ℃, 60 ℃, 80 ℃ and 98 ℃ were handled 3 hours, the pigment storage rate was respectively 99.53%, 94.16%, 76.04% and 56.45%.As seen the high more pigment survival rate of temperature is low more, palliating degradation degree big more [model Gong Jian, the extraction process of radish red pigment and stability thereof, Jiangsu agricultural journal, 2002,22 (2)].Studies have shown that, the variation that haematochrome causes in the temperature rising, be because after anthocyanogen is heated, its structure changes to phenyl styryl ketone, cause coloured structure 2-benzopyralium salt and quinoid pseudobase to reduce [Dong's congruence, edible natural pigment---the fresh-keeping and processing of radish red progress [J], 2004,25 (6): 9～11].The pelargonidin structure that too high temperature is foretold in the haematochrome square-bottomed bamboo basket changes, balance is carried out to colourless phenyl styryl ketone direction, cause having reduction [DrybyM.Light and heat sensitivity of red cabbage extract insoft drink model systems[J] the .Food Chemistry of colour pattern compounds content, 2001,72:431～437].
Summary of the invention
Task of the present invention is, defective at existing extraction natural pigment, provide a kind of natural pigment of avoiding in the leaching process temperature distortion with extract the climing mountain valley with clumps of trees and bamboo haematochrome extracting method that the course of processing is urged oxidation defect, the kohlrabi pigment of extraction also need satisfy the requirement of food safety.
The present invention is achieved in that after the clean processing of climing mountain valley with clumps of trees and bamboo root piece, be placed in the sealed vessel, in container, fill edible ethanol, make vessel space full fully, reach the air purpose in the displacement container, make and be in anaerobic state in the container, in container, press the dress high-speed shearing device, the climing mountain valley with clumps of trees and bamboo root piece that uses high-speed shearing device will be immersed in the ethanolic soln is sheared pulverizing, crushing process ethanol plays the effect of dissolving pigment in sealed vessel, the climing mountain valley with clumps of trees and bamboo that to pulverize by vacuum filter after pulverizing carries out solid-liquid separation, get filtrate, slag discards, filtered liquid is passed through microfiltration systems, further separate small solid and a part of macromolecular colloid material, get filtered liquid, adopt negative pressure less than the 1000pa decompression distillation system filtered liquid, ethanol and moisture in the distillating filtering liquid, when negative pressure reaches 1000pa, water saturation vapour pressure corresponding temperature is 7 ℃, therefore as long as the negative pressure of control decompression distillation system can be finished the purpose of moisture evaporate to dryness at normal temperatures less than 1000pa, adopt ultralow pressure normal-temperature distilled until steam to water content less than 2%, contained pigment solution reaches crystalline state in the climing mountain valley with clumps of trees and bamboo root piece, promptly reached the purpose of extracting kohlrabi pigment, leaching process has avoided high temperature also to avoid urging simultaneously the effect of oxidation, extraction process is not used any noxious solvent, has avoided the residual of harmful toxic matter, the climing mountain valley with clumps of trees and bamboo haematochrome that present method is extracted, beautiful in colour, the extract yield of the climing mountain valley with clumps of trees and bamboo root of bright product piece reaches 5%.Detect ethanol water mixed solution dissolving back maximum absorption band 532nm through Dalian Inst of Chemicophysics, Chinese Academy of Sciences physical and chemical testing center.Contained harmful heavy metal (sees Table 1) within the safe edible standard range
Table 1
| Project | Sample (kohlrabi pigment) |
| Plumbous (in pb) ppm,＜ | 1.0 |
| Arsenic (in As) ppm,＜ | 1.0 |
| Cadmium (in Cr) ppm,＜ | 0.5 |
| Mercury (in Hg) ppm,＜ | 0.5 |
| Kind in the qualitative test sample | Ca，K，Mg，p，Al，B，Ba，Cu，Fc，Mn |
Positive effect of the present invention is embodied in:
1, the present invention adopts the anaerobic extraction process, and the natural true qualities of natural pigment can not changed, and has kept the biological activity of natural product to greatest extent, has improved the pigment using value.
2, the present invention has avoided the employing noxious solvent, makes the food dye security more guaranteed.
3, the present invention adopts the distillation dehydration technology of ultralow negative pressure, has avoided the heated denaturalization of high temperature to natural compounds.
4, the present invention can play active effect for deep processing, the raising value of farm production of agricultural-food.
Specific embodiment
The first step: get the clean processing of the bright climing mountain valley with clumps of trees and bamboo.
Second step: the climing mountain valley with clumps of trees and bamboo root piece that cleaning is handled places in the sealed vessel, and the perfusion edible ethanol is filled with container, reaches the purpose of the air in the displacement container, twists cut then and pulverizes.
The 3rd step: the climing mountain valley with clumps of trees and bamboo is pulverized the mixed solution vacuum filtration, get filtrate, slag discards.
The 4th step: with climing mountain valley with clumps of trees and bamboo filtrate micro-filtrate membrane filtration, reject the small-particle solid, reject a part of macromolecular colloid material, get filtered liquid.
The 5th step: will be filtering climing mountain valley with clumps of trees and bamboo filtrate decompression distillation (be decompressed to≤1000Pa, temperature control≤50 ℃), recovery ethanol; Steam to remove part moisture in the mixing solutions to solid.
The 6th step: rewinding (obtaining climing mountain valley with clumps of trees and bamboo haematochrome).
Claims (2)
1, a kind of process for abstracting kohlrabi pigment is characterized in that being operated by following steps:
The first step: get the clean processing of the bright climing mountain valley with clumps of trees and bamboo.
Second step: the climing mountain valley with clumps of trees and bamboo of aquatic foods is placed in the sealed vessel, perfusion edible ethanol in the container, the strand cut is pulverized.
The 3rd step: vacuum filtration, get filtrate, slag discards.
The 4th step: micro-filtrate membrane filtration, reject small-particle solid and a part of macromolecular colloid material, get filtered liquid.
The 5th step: with the filtered liquid underpressure distillation.Reclaim ethanol; Steam to remove part moisture in the mixing solutions to solid.
2, process for abstracting kohlrabi pigment according to claim 1 is characterized in that described step the five, with the filtered liquid underpressure distillation, is decompressed to≤1000Pa, temperature control≤50 ℃.
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| CNA2007101094010A CN101311225A (en) | 2007-05-26 | 2007-05-26 | Process for abstracting kohlrabi pigment |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103773063A (en) * | 2014-01-16 | 2014-05-07 | 河南科技大学 | Process for preparing natural plant dye from first case of red |
| CN105527239A (en) * | 2016-01-18 | 2016-04-27 | 中国农业科学院茶叶研究所 | Method for synchronously and quantitatively detecting tea resin soluble pigment monomer |
| CN106726868A (en) * | 2016-11-22 | 2017-05-31 | 厦门上新日用化学制品有限公司 | A kind of preparation method of the China rose anthocyanidin for having whitening capability |
| CN109443872A (en) * | 2018-11-13 | 2019-03-08 | 河南工业大学 | A kind of raw long-life noodles brown stain product purification methods |
| CN113750130A (en) * | 2021-09-30 | 2021-12-07 | 新疆华圣元医药科技有限公司 | Extraction method of turnip extract |
-
2007
- 2007-05-26 CN CNA2007101094010A patent/CN101311225A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103773063A (en) * | 2014-01-16 | 2014-05-07 | 河南科技大学 | Process for preparing natural plant dye from first case of red |
| CN103773063B (en) * | 2014-01-16 | 2015-08-05 | 河南科技大学 | A kind of technique utilizing SHOUANHONG tree peony to prepare natural plant dye |
| CN105527239A (en) * | 2016-01-18 | 2016-04-27 | 中国农业科学院茶叶研究所 | Method for synchronously and quantitatively detecting tea resin soluble pigment monomer |
| CN105527239B (en) * | 2016-01-18 | 2018-10-12 | 中国农业科学院茶叶研究所 | A method of synchronizing quantitative detection tea tree fat-soluble pigment monomer |
| CN106726868A (en) * | 2016-11-22 | 2017-05-31 | 厦门上新日用化学制品有限公司 | A kind of preparation method of the China rose anthocyanidin for having whitening capability |
| CN106726868B (en) * | 2016-11-22 | 2019-10-29 | 厦门上新日用化学制品有限公司 | A kind of preparation method for the China rose anthocyanidin having whitening capability |
| CN109443872A (en) * | 2018-11-13 | 2019-03-08 | 河南工业大学 | A kind of raw long-life noodles brown stain product purification methods |
| CN109443872B (en) * | 2018-11-13 | 2021-01-22 | 河南工业大学 | Method for purifying fresh wet-surface browning product |
| CN113750130A (en) * | 2021-09-30 | 2021-12-07 | 新疆华圣元医药科技有限公司 | Extraction method of turnip extract |
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