CN103160139A - Extraction method for natural pigment - Google Patents
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Abstract
The invention discloses an extraction method for a natural pigment. The extraction method for a natural pigment comprises the following steps of: (1) washing, drying and crushing raw materials, then passing through a 100-mesh sieve, performing homogeneous extraction in the mixed solution of ethanol aqueous solution in the percentage of 60-95% by volume and hydrochloric acid aqueous solution in the concentration of 0.1 mole per litre, and filtering after the extraction, so as to obtain a filtrate, wherein the pH value of the obtained mixed solution is 2.0-5.0; and the homogeneous extraction comprises a high-speed pre-treatment phase and a homogeneous extraction phase; (2) neutralizing, centrifuging and deslagging the filtrate obtained in the step (1), so as to obtain a supernatant; and (3) concentrating and drying the supernatant obtained in the step (2), so as to obtain the natural pigment, wherein the raw materials are chestnut shells, black soya bean skins, dragon fruit peels, lychee exocarps, grape seeds, hickory exocarps, acorn shells, orange peels, hazelnut shells, nectarine peels and purple sweet potato or purple-black broomcorn shells. The extraction method disclosed by the invention is simple in process, low in requirements on production equipment, not easy to break pigment substances, and high in extraction rate.
Description
Technical field
The present invention relates to a kind of extracting method of natural pigment, relate to particularly a kind of technique that chestnut shell pigment, Testa sojae atricolor pigment, pitaya peel pigment, Litchi exocarp pigment, Proanthocyanidins from Grape Seeds, hickory nut epicarp pigment, Brown Pigment From Acorn Shells, peel of Citrus reticulata Blanco yellow pigment, pigment of hazelnut shell, nectarine skin red pigment, Ipomoea batatas(L.)Lam and purple black sorghum husk pigment are produced that can be used for.
Background technology
natural plant pigment can be divided into four large classes by the chemical structure difference, pyrrole derivative class pigment, polyenoid class pigment (carotenoids class prime system), the phenols pigment, ketone and Quinone Pigments, it is not only nontoxic, and much contain the necessary nutritive substance of human body or itself be exactly VITAMIN or material with VITAMIN character, as riboflavin, lycopene, β-carotene etc., the natural pigment tone is more natural simultaneously, can imitate preferably the color of natural goods, painted tone waits many factors more naturally, therefore modern food industry more and more trends towards using natural pigment to the selection of pigment, the extraction of natural pigment is also to have waved increasingly vital role.
The extracting method of natural pigment has solvent extraction method, microwave extraction method, supercritical fluid extraction, ultrasonic extraction etc. at present.Wherein solvent extraction method is as using the earliest, and simple to operate, becomes the most frequently used natural pigment extracting method at present, and its principle is to be isolated according to the different solubility of target component in different solvents (particularly ethanol).
Contain Flavonoid substances in chestnut shell, it is that a kind of good water solubility, tinting strength are strong, stable in properties, have the natural brown pigment of eliminating free radical, blocking-up and removing oxidative damage, health care and deferring senility and value, and wide development and application prospect are arranged.
The solvent-extraction process of chestnut shell pigment is due to the extracting method of commonly using the most at present that becomes easy and simple to handle, with low cost, as, Beijing Agricultural College. the extracting method of chestnut shell brown pigment [P]. China: CN 101407640A, 2009.4.15. the lixiviate of described diluted alkaline ethanolic soln secondary, pigment extraction yield be at 7-10%, look valency 18-20,0.1% mass body volume concentrations of pigment is red-brown, clear, free from extraneous odour, slightly Chinese chestnut fragrance; Li Yunyan, Song Guangsen. the extraction of chestnut shell pigment and main component qualitative analysis [J] thereof. Guangzhou Food Industry science and technology, 2003,19 (3): the optimization extraction conditions that 10-12. reports: the solid-liquid ratio of chestnut shell and 30% ethanol 1: 15 (mass ratio), extract 2 times each 3h under 80 ℃.But easily cause the destruction of Flavonoid substances and other antioxidant components in chestnut shell, and in extracting solution, foreign matter content is higher, is unfavorable for the isolation and purification of Flavonoid substances, extraction yield is not high yet.
Testa sojae atricolor is rich in haematochrome, and this pigment is soluble in water, flavor is fragrant and sweet, bright in colour, and nutritive value and pharmacological action are obvious, are a kind of natural pigments that application value is arranged very much.
China begin one's study from the nineties in 20th century extraction and the stability thereof of Property of pnaseolus Red Pigment, report more, mainly concentrate on traditional organic solvent lixiviate, as: Mei Jiansheng, Li Li, Hu Jiantao, Deng. the research of Testa sojae atricolor method for extracting pigment [J]. Northwest University's journal (natural science edition), 2004, 6, 34 (3): Testa sojae atricolor anthocyanin class pigment that 320-324. reports extracts optimal conditions: 50% ethanolic soln was solid-liquid ratio 1: 100, pH value 1.0 times, 70 ℃, 90min extracts 3 times, obtain cherry pigment medicinal extract, be red-purple pigment dry powder after dry, extraction yield can reach 98% left and right, Gao Xueqin, Wang Ruolan, Jianping YANG. the Property of pnaseolus Red Pigment microwave-assisted extracts the technique comparative studies [J] with alcohol steep. food and pharmaceutical, the ethanolic soln that 2006,8 (05A): 39-41. report extracts 4h, extraction yield 93% 1: 40 time at solid-liquid ratio, when adopting microwave-assisted to extract, have and save time, extraction yield is high, but solvent consumption is equally at 1: 40.Extract length consuming time, solvent consumption is large, and pigment thermotolerance, photostabilization and the difference that affected by metal ion large.
The Hylocereus undatus pericarp contains abundant pigment, the experiment record account for the fruit in the pigment total amount 21%, edible and processing mesocarp is dropped, be undoubtedly a kind of huge waste, therefore extracting pericarp pigment not only can widen the variety source of pigment, satisfy people's demand growing to natural pigment, and can make natural resources obtain more rationally, more effectively develop, thereby improve its value-added content of product, and be new outlet of deep processing creation of these agricultural-food, further improve the producer, manager's economic benefit
The aspects such as extractive technique, technique and the pigment stability report of China's Hylocereus undatus pericarp pigment is few, and systematic study history is not long.As Yang Changpeng, Tang Zhiyuan, Lu Yi, Deng. the extraction Separation Research [J] of Hylocereus undatus pericarp haematochrome. the Agriculture of Anhui science, 2010,38 (1): 347-349. has studied and has extracted 5-10min with glycollic acid solution for 1: 60 time at solid-liquid ratio, extraction effect is better, but overall pigment extraction efficiency is not high, and the solvent for use amount is large, easily causes waste.
Contain a large amount of excellent propertys in Litchi exocarp, brightly painted natural pigment is a kind of the natural of exploitation, raw material that can be used as foodstuff additive and healthcare products that purity is higher of being worth very much.China is maximum in the world lichee producing country, account for world's lichee total cultivated area 90% and ultimate production 80%.As the traditional Chinese medical science or other dietetic uses, use is litchi pulp usually due to lichee, and a large amount of litchi rinds abandon as waste, not only cause the wasting of resources and contaminate environment.
For the extraction of Litchi exocarp pigment, the aspects such as pigment stability report is few, and systematic study is also just at the early-stage.What is defeated, Li Guirong, Liu Chuanxiang. the extraction of Litchi exocarp haematochrome and stability observing [J]. and University Of Nanhua's journal medicine, 2002,9,30 (3): 269-271. soaked 1 day with 3 times of extraction agents or stirs and extract 4h, obtained red clarification extracting solution.Present Litchi exocarp pigment extracts the research with the pigment stability aspect, shows that overall pigment extraction efficiency is not high, and the less stable of pigment is unfavorable for preserving and use.
Contain multiple Polyphenols natural antioxidants in Semen Vitis viniferae.Along with going deep into of research, find grape wine particularly a lot of natural antioxidantss in red wine be directly to come from Semen Vitis viniferae, some oligomer only is present in Semen Vitis viniferae.Semen Vitis viniferae is brew tankage vinous, domesticly also it is not carried out sufficient processing and utilization, generally only processes as feed or fertilizer simply, even is taken as useless rubbish.If can rationally utilize these Semen Vitis viniferaes, extract useful matter wherein, not only can solve the trouble and worry of winery, but also can create economic worth.Therefore, to the natural plant resource deep exploitation, to protection of the environment, development protective foods, makeup and biological-pharmacy all have positive effect from extracting proanthocyanidin from grape seeds.
Aspect Study on extraction, mainly adopt at present the solvent soaking extraction method both at home and abroad, increase extraction efficiency with means such as heating, stir, wave concussion.As, Zhao Wenen, Han Guihua, Jiao Fengyun. Proanthocyanidins from Grape Seeds Study on extraction [J]. Food science, 2002,23 (8): 108-110. has used ethanol, acetone, ethyl acetate extraction, with 70% ethanol when extracting solvent, solid-liquid ratio room temperature under extracts 8-10h at 1: 4, and the proanthocyanidin yield can reach 14.4-36.1%, and purity is more than 32%; Qu Jingnian, Ceng Wenliang, Chen Hui, Deng. the extraction of Proanthocyanidins from Grape Seeds, modification and anti-oxidant study on the modification [J]. Hengyang Normal University's journal, 2010,6,31 (3): 48-51. is with 40% ethanolic soln 313K (40 ℃), solid-liquid ratio extracts 80min 1: 11 time, and effect is better, but overall pigment extraction efficiency is not high.
When Semen Caryae Cathayensis Chinese olive skin is the Semen Caryae Cathayensis prematurity, the green thick pericarp of one deck of outside, be Exocarpium Juglandis Immaturum in proved recipe of traditional Chinese medicine, and certain toxicity is arranged, and becomes Vandyke brown after maturation.In the Semen Caryae Cathayensis producing region, its exocarp is waste, now environment is caused huge pollution, if extract its pigment and be applied to the industries such as food, will become Fei Weibao, has both increased peasant's income, has protected again environment, and is significant.
Present food dye mostly is synthetic colour, though bright in colour, with low cost, modern medicine proves, most of chemosynthesis pigments have toxic side effect in various degree, therefore its use is restricted, are just progressively replaced by natural pigment.Extraction for pigment from walnut epicarp, Han Haixia, Bao Xiaowei, Fu Li, Deng. the extraction purifying of walnut husk brown pigments and stability study [J] thereof. Chinese agronomy circular, 2009,25 (22): 83-87. is respectively with hydrochloric acid and extraction using alcohol pigment the time, and extraction yield is close with 5.3%, two kind of pigments 6.2%.The present invention is directed to the traditional extraction process extraction yield not high, improved traditional pure extraction, make and improve hickory nut epicarp pigment extraction yield when not increasing extraction cost, for the industry using value that enlarges the hickory nut epicarp pigment lays the first stone.
The acorn nut output of China is abundant especially, and particularly, as the province that is national acorn nut output maximum, there is a lot of acorn nuts every year in Shaanxi Province for utilizing.But at present Shaanxi to the exploitation of acorn nut resource seldom, particularly to acorn cup, does not utilize basically, has caused the serious waste of this resource.
The comprehensive utilization of acorn cup, it is mainly the wherein utilization of pigment.China starts from 1994 to the utilization of Brown Pigment From Acorn Shells research, utilizes 50% the ethanol extracting pigment that refluxes as Chen Zhiyong etc., extracts length loaded down with trivial details, consuming time, and extraction yield is lower, and its composition be it be unclear that.
China is that world's citrus originates in one of center, and citrus production is about 1,500 ten thousand tons, is only second to Brazil and the U.S..Orange peel account for whole fruit heavy 20%, Chinese annual output orange peel approximately reaches 3,000,000 tons, at present except a small amount of as Chinese medicine and producing essence oil, major part not yet develops.
The peel of Citrus reticulata Blanco yellow pigment is again Yellow Pigment from Tangerine Peel, naringin, and main component is the mixture of limonene and carotenoid, also rich in vitamin E and rare elements selenium (Se).The peel of Citrus reticulata Blanco yellow pigment is not only simple tinting material, but also is the nutrition-fortifying agent of food, is the perfect additive that improves food nutrition and health-care effect.
The carotenoid that extracts from peel of Citrus reticulata Blanco (genus naringin) is a kind of natural pigment, main component is the mixture of carotenoids and limonene, also contain VE and rare elements Se, these materials are for preventing that growth of cancer cells, delaying cell aging, enhancing body immunity from having good effect.
The aspects such as extractive technique, technique and pigment stability of China's peel of Citrus reticulata Blanco yellow pigment report is few, and traditional orange peel pigment extracts and separates with dehydrated alcohol, sherwood oil water-bath lixiviate, and the time is long, and operation steps is many, and some solvent can not recycle and reuse, and energy consumption is large.Not high for the traditional extraction process extraction yield; if and the microwave and ultrasound technology is extracted misoperation; can cause the inactivation of yellow pigment; the present invention has improved traditional pure extraction; adopt the collaborative alcohol steep of homogeneous; having the advantages such as selectivity is strong, control convenience, conserve energy, reduce the requirement that process cost conforms with environment protection simultaneously, is the novel process with good development prospect.
Along with developing rapidly of fibert and going deep into of fibert processing technology in recent years, hazelnut shell quantity increases day by day, owing to not fully utilized, causes the wasting of resources and environmental pollution.
The research report, can extract brown pigments from hazelnut shell, as Xu Haiqing etc. the extraction of hazelnut shell brown pigment and stability study [J]. Agricultural University Of Shenyang's journal, 2009-02,40 (1): 58-61., this pigment good water solubility, character is more stable, can be used as natural pigment and be applied to the food service industrys such as beverage, cake, soy sauce, but the pigment extraction yield is lower.Northeast Forestry University forestry institute and for example. a kind of preparation method of hazelnut shell brown pigment [P]. China: CN 101798468 A, 2010.1.29., adopt salt and alkali effect to extract pigment, although the pigment yield that extracts is higher, but the effect of alkali can bring destruction and the pollution of environment, and the pigment that extracts is because its structure of effect of alkali can be destroyed to some extent.
Other extracting method of hazelnut shell brown pigment are as steam distillation, solvent extraction method, supercritical extraction method, microwave method and supersonic method.These methods extract that length consuming time, solvent consumption are large, pigment thermotolerance, photostabilization and differing greatly of being subjected to that metal ion affects, and often can not reach industrial requirement.
The bright-coloured redness in nectarine fruits surface covers all fruit faces, has abundant natural red colouring matter in skin, is good natural pigment resource.It is trend of the times that the natural food colour that application safety is nontoxic replaces synthetic food colors.
In recent years, many scholars have done a large amount of researchs such as nectarine cultivation technique, but less as the exploitation research of natural food colour to its skin at present.The relevant research that Wei Ya slowly waits the people that microwave extraction nectarine haematochrome is carried out, but overall pigment extraction efficiency is not high.
Ipomoea batatas(L.)Lam is the water-soluble red colouring matter that extracts from the piece root of Rhizoma Dioscoreae esculentae, belongs to anthocyanidin, is the flavonoid class compound.Anthocyanidin is the natural red colouring matter that allows use, in fields such as food, beverage, makeup, purposes is widely arranged, therefore be in great demand both at home and abroad, and be functional food additive and the healthy food material that has future.
Similar extracting method about Ipomoea batatas(L.)Lam is also arranged both at home and abroad, as NISHAMA K, MUROI T.Anthocyanin isolation from purple sweet potato; JP:823919[P] .1996-01-30. Shenyang Inst. of Applied Ecology, Chinese Academy of Sciences. a kind of extracting method of Brown Pigment in Chestnut Shells [P]. China: CN 1569970A, 2005.1.26. Shenyang Inst. of Applied Ecology, Chinese Academy of Sciences. a kind of extracting method of Brown Pigment in Chestnut Shells [P]. China: CN 1569970A, 2005.1.26.
The aspects such as the extractive technique of China's Ipomoea batatas(L.)Lam, technique and pigment stability have report successively, but systematic study history is not long, has the report of microwave and ultrasonic extracting method to rest on the optimization of method itself to purple potato pigment at present.In recent years, Gu Hongmei, Xu Zhenghong, Gao Yanxiang etc., Yang Hua rely blue and green grade in succession to carry out correlative study, have studied the extraction process of microwave and ultrasound technology aspect the extraction Ipomoea batatas(L.)Lam.But microwave or ultrasonic extraction be comparatively power consumption all, and need to buy more microwave or ultrasonic extraction equipment, increases cost.
China's higher kind of main popularizing planting output and cross-fertilize seed, its sorghum husk color mostly is red-purple and atropurpureus.Sorghum husk as one of by product in the sorghum production process, its contained red sorghum pigment is as a kind of natural pigment, this pigment is soluble in water, nontoxic, without special odor, tinctorial property is good, color and luster is soft, and certain nutritive value and pharmacological action are arranged, and is a kind of natural pigment that application value is arranged very much.
The aspects such as extractive technique, technique and pigment stability of the purple black sorghum husk pigment of China have report successively, but systematic study history is not long, since the nineties in 20th century, Li Cunxiong, Wang Guangyan and Cao Xiaofeng, Wei Jiancong, Diao Haipeng etc. and Zhang Hairong etc. carry out correlative study in succession, but overall pigment extraction efficiency is not high.
Summary of the invention
Technical problem to be solved by this invention is in order to overcome in existing extracting method to natural pigments such as chestnut shell pigment, Testa sojae atricolor pigment, Hylocereus undatus pericarp pigments, the defectives such as cost is higher, extraction yield is lower, and a kind of extracting method of natural pigment is provided.Extracting method technique of the present invention is simple, low to the production unit requirement, colors is survivable, extraction yield is higher.
The present invention relates to a kind of extracting method of natural pigment, it comprises the following step:
(1) with raw material washing, dry, rear 100 mesh sieves of crossing of pulverizing, in the mixed solution of the aqueous hydrochloric acid of the aqueous ethanolic solution of percent by volume 60-95% (preferred 75%-95%) and 0.1 mole every liter, carrying out homogeneous extracts, the pH of described mixed solution is 2.0-5.0 (preferred 3.0), filter after extracting, get filtrate; Described homogeneous extracts and comprises that high speed pretreatment stage and homogeneous extract the stage;
(2) with the neutralization of step (1) gained filtrate, centrifugal slagging-off, get supernatant liquor;
(3) supernatant liquor of step (2) gained is concentrated and dry, get final product;
Wherein, described raw material is chestnut shell, Testa sojae atricolor, Hylocereus undatus pericarp, Litchi exocarp, Semen Vitis viniferae, hickory nut epicarp, acorn cup, peel of Citrus reticulata Blanco, hazelnut shell, nectarine skin, Rhizoma Dioscoreae esculentae or purple black sorghum husk.
In step (1), after the raw material after described pulverizing and sieving and mixed solution mixed, that solid-to-liquid ratio is better was mass volume ratio (w/v) 1g: 5ml-1g: 10ml.
In step (1), described homogeneous extracts equipment used and can be commercially available high-shear homogenizing machine.What described high speed pretreatment stage condition was better is that under 5000-10000 (preferred 9000-10000) rpm, effect is no less than 5 minutes (preferred 5-20min); What temperature was better is room temperature (20～35 ℃).It is to process under 1000-4000 (preferred 3000-4000) rpm to be no less than 30 minutes (preferred 30-60min) that described homogeneous extracts the stage condition.
The temperature that described homogeneous extracts the stage can be room temperature (20～35 ℃).The time that described homogeneous extracts the stage can be 5～8 hours.What the number of times in described homogeneous extraction stage was better is 1～3 time (preferred 2 times).Namely after the 1st homogeneous extracts, step (1) gained filter residue can be repeated 1～2 homogeneous and extract.
In step (2), the method for described neutralization can be conventional neutralization method, as adds alkali aqueous solution (for example 0.1 mole of every liter of aqueous sodium hydroxide solution), adjusts pH to 6～8 (in general, getting final product to neutral).Described centrifugal condition can be the normal condition of this area centrifugally operated, and better is processed 5-30 minute under 200-2000 (preferred 1000) rpm, and better is under 1000 rpms centrifugal 5-15 minute.
In step (3), described drying can be conventional drying means, as lyophilize.
Extracting method of the present invention, better step is as follows:
(1) get fresh feed through washing removal of impurities, drying, pulverizing, crossing 100 mesh sieves;
(2) add ethanol, hydrochloric acid, transfer pH to acid, homogeneous extracts and filters;
(3) filter residue is processed once by abovementioned steps (2) again, filtered;
(4) merge twice filtrate in front and back, with sodium hydroxide solution neutralization, centrifugal slagging-off;
(5) collect centrifuged supernatant,, lyophilize concentrated through reduced vacuum gets this product.
Except specified otherwise, the raw material that the present invention relates to is commercially available getting all.
Positive progressive effect of the present invention is:
(1) the present invention adopts the lixiviate of ethanol acid adding, has improved the pigment efficiency of pcr product that utilizes merely organic solvent and utilize merely acid extraction.
(2) extraction of pigment is to carry out in two stages under high-shear homogenizing machine auxiliary, the high speed homogenization of pretreatment stage with the powder particle of shell become less, make its easier being distributed in uniformly in solution, reach extraction effect more even, extraction comparison is thorough; And extract the stage than the homogeneous under low rate, also more standing extraction or other extracting method have higher pigment extraction yield.
(3) this extraction process is simple, and low to the production unit requirement, extraction efficiency is high, and colors is survivable, obviously is better than the traditional water bath extraction method.
(4) the pigment good water solubility of this processing method extraction, product appearance is bright in colour, and proterties is stable, is suitable for as foodstuff additive and healthy food material.
Description of drawings
Fig. 1 is the absorption spectrum of chestnut shell pigment in the different pH value aqueous solution that embodiment 3 makes.(annotate: the absorption spectrum of its absorption spectrum and other flavonoids such as cacao color, kaoliang colour etc. is very close, can look into pertinent literature, all at visible region without obvious absorption peak, and along with the increase of pH value, the color burn look of pigment, absorbancy increases)
Fig. 2 is the UV-Vis spectrogram of the Testa sojae atricolor pigment that makes of embodiment 6.(annotate: pigment has maximum absorption at 285nm and 525nm place, meets one of anthocyanogen maximum absorption wavelength near 500-540nm, and another can judge this pigment anthocyanogen near ultraviolet 275nm)
Fig. 2 a is the HPLC figure of Testa sojae atricolor pigment under 520nm that embodiment 6 obtains.
Fig. 2 b is the HPLC figure of Testa sojae atricolor pigment under 280nm that embodiment 6 obtains.
Fig. 3 is the UV-Vis spectrogram of the Hylocereus undatus pericarp pigment after supernatant liquor that step in embodiment 9 (3) obtains is further purified.(annotate: maximum absorption wavelength belongs to beet glycoside pigment at the 538nm place)
Fig. 4 is the HPLC figure of the Hylocereus undatus pericarp pigment after supernatant liquor that step in embodiment 9 (3) obtains is further purified.
Fig. 5 is the HPLC spectrogram of the Semen Vitis viniferae pigment that makes of embodiment 15.Wherein the HPLC condition is: chromatographic column: Sephadex C18 post; Moving phase: methanol-water (0-1) gradient elution; Detector: UV-detector; Detect wavelength: 280nm.
Fig. 6 a, 6b are respectively the visible and UV spectrogram of the hickory nut epicarp pigment that embodiment 18 makes, (Fig. 6 a is the visible light spectrogram, 6b is infrared spectrogram) (annotate: in Fig. 6 a, pigment solution is in the wavelength region of 320-470nm, the absorbancy curve reduces rapidly with the increase of wavelength, and in the 470-650nm wavelength region, the absorbancy curve slows down with the trend that the increase of wavelength reduces, and this pigment without maximum absorption wave, infers that it is mixture at visible region; 2. in Fig. 6 b, sample has a lot of absorption peaks, therefore should be mixture, maximum absorption peak is respectively 284.5nm and 286nm, should be maximum at this wavelength place substances content.)
Fig. 7 is the UV-Vis collection of illustrative plates of the peel of Citrus reticulata Blanco pigment that makes of embodiment 25.(pigment product is the mixture of fat-soluble pigment and water colo(u)r)
Embodiment
The below further illustrates the present invention with embodiment, but the present invention is not limited.
Embodiment 1:
1) get fresh chestnut shell and wash, dry, pulverize, cross 100 mesh sieves, standby.
2) take 100 gram chestnut shell powder, adding volume fraction is 95% ethanol, and 0.1 mole every liter hydrochloric acid adjust pH is 2.0, and solid-liquid ratio quality volume fraction is 1: 5.
3) under room temperature, 10000 rpms of high speed pre-treatment 10min, then filter after 3000 rpms of lower homogeneous extract 30min.
4) with above-mentioned steps 3) in filter residue under 3000 rpms again homogeneous extracted 5 hours, filter.
5) merge twice filtrate, neutralize with the sodium hydroxide solution of 0.1 mole every liter, under 1000 rpms centrifugal 10 minutes, go precipitation, collect concentrate after supernatant, lyophilize is powdered, obtains chestnut shell pigment 6.32 grams (color is brown), pigment extraction yield 96.5%.
Embodiment 2:
1) get fresh chestnut shell and wash, dry, pulverize, cross 100 mesh sieves, standby.
2) take 100 gram chestnut shell powder, adding volume fraction is 95% ethanol, and 0.1 mole every liter hydrochloric acid adjust pH is 3.0, and solid-liquid ratio quality volume fraction is 1: 10.
3) under room temperature, 10000 rpms of high speed pre-treatment 20 minutes, then filter after 4000 rpms of lower homogeneous extract 60min.
4) with above-mentioned steps 3) in filter residue under 3000 rpms again homogeneous extracted 7 hours, filter.
5) merge twice filtrate, neutralize with the sodium hydroxide solution of 0.1 mole every liter, under 1000 rpms centrifugal 15 minutes, go precipitation, collect concentrate after supernatant, lyophilize is powdered, obtains chestnut shell pigment 6.67 grams, color is brown, pigment extraction yield 97.4%.
Embodiment 3:
1) get fresh chestnut shell and wash, dry, pulverize, cross 100 mesh sieves, standby.
2) take 100 gram chestnut shell powder, adding volume fraction is 95% ethanol, and 0.1 mole every liter hydrochloric acid adjust pH is 4.0, and solid-liquid ratio quality volume fraction is 1: 7.
3) under room temperature, 9000 rpms of high speed pre-treatment 5min, then filter after 4000 rpms of lower homogeneous extract 45min.
4) with above-mentioned steps 3) in filter residue under 3000 rpms again homogeneous extracted 8 hours, filter.
5) merge twice filtrate, with the sodium hydroxide neutralization of 0.1 mole every liter, centrifugal 5min under 1000 rpms, go precipitation, collect concentrate after supernatant, lyophilize is powdered, obtains chestnut shell pigment 6.15 grams (color is brown), pigment extraction yield 96.1%.
Embodiment 4:
(1) get fresh Testa sojae atricolor drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram Testa sojae atricolor powder, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 2.0, solid-liquid ratio is 1: 5 (quality volume fraction), 9000 rpms of processing 5min of high speed under room temperature, filter after 3000 rpms of lower homogeneous of low speed extract 30min again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, with 0.1 mole of every liter of sodium hydroxide solution neutralization, the lower 1000 rpms of centrifugal 5min of normal temperature collect supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the Testa sojae atricolor pigment, pigment extraction yield 96.4%, color: red-purple.
Embodiment 5:
(1) get fresh Testa sojae atricolor drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram Testa sojae atricolor powder, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 3.0, solid-liquid ratio is 1: 7 (quality volume fraction), changing at a high speed 9000 rpms under room temperature processed 10 minutes, filter after 4000 rpms of lower homogeneous of low speed extract 45 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 10 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the Testa sojae atricolor pigment, pigment extraction yield 97.1%, color: red-purple.
Embodiment 6:
(1) get fresh Testa sojae atricolor drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram Testa sojae atricolor powder, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 5.0, solid-liquid ratio is 1: 10 (quality volume fraction), changing at a high speed 10000 rpms under room temperature processed 20 minutes, filter after 4000 rpms of lower homogeneous of low speed extract 60 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 15 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the Testa sojae atricolor pigment, pigment extraction yield 97.9%, color: red-purple.
Pigment extract in Testa sojae atricolor (supernatant liquor that step (3) obtains) is scanned in the 200-650nm scope, if as shown in Figure 2, as can be seen from Figure 2, pigment has maximum absorption band at 285nm and 525nm place.
In view of above result, pigment to be carried out HPLC analyze, condition is as follows:
With each 10 direct injection liquid analysis of hplc of μ L of pigment diluent, chromatographic condition is Nucleodur100-50DS C18 post (5 μ m 250*406mm), and moving phase is methyl alcohol: water; Detector: the RF-10AXL fluorimetric detector, detect wavelength: 520nm, 280nm; 520nm surveys anthocyanidin, and 280nm surveys Polyphenols.40 ℃ of column temperatures, flow velocity are 1mL/min, and transferring pH with hydrochloric acid is 3.0.The results are shown in Figure 2a and Fig. 2 b, Fig. 2 a is the HPLC figure of Testa sojae atricolor pigment under 520nm, and Fig. 2 b is the HPLC figure of Testa sojae atricolor pigment under 280nm.
Embodiment 7:
(1) fresh Hylocereus undatus pericarp is washed removal of impurities, drying, pulverizing, crossed 100 mesh sieves, and is standby.
(2) take 100 gram Hylocereus undatus fruit peel powders, adding volume fraction is 95% ethanol, 0.1 mole every liter of hydrochloric acid adjust pH is 3.0, the mass body integration numerical control of solid-liquid ratio was built in 1: 5, under room temperature, 10000 rpms of processing of high speed are 20 minutes, filter after 3000 rpms of lower homogeneous of low speed extract 60min again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, with 0.1 mole of every liter of sodium hydroxide neutralization, centrifugal 10 minutes of lower 1000 rpms of normal temperature removes to precipitate the collection supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains Hylocereus undatus pericarp pigment (extraction yield 93.21%, color: redness).
Embodiment 8:
(1) fresh Hylocereus undatus pericarp is washed removal of impurities, drying, pulverizing, crossed 100 mesh sieves, and is standby.
(2) take 100 gram Hylocereus undatus fruit peel powders, adding volume fraction is 95% ethanol, 0.1 mole every liter of hydrochloric acid adjust pH is 2.0, the mass body integration numerical control of solid-liquid ratio was built in 1: 7,9000 rpms of processing 5min of high speed under room temperature, filter after 3000 rpms of lower homogeneous of low speed extract 30min again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, with 0.1 mole of every liter of sodium hydroxide neutralization, the lower 1000 rpms of centrifugal 5min of normal temperature go precipitation, collect supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains Hylocereus undatus pericarp pigment (extraction yield 95.34%, color: redness).
Embodiment 9:
(1) fresh Hylocereus undatus pericarp is washed removal of impurities, drying, pulverizing, crossed 100 mesh sieves, and is standby.
(2) take 100 gram Hylocereus undatus fruit peel powders, adding volume fraction is 95% ethanol, 0.1 mole every liter of hydrochloric acid adjust pH is 4.0, the mass body integration numerical control of solid-liquid ratio was built in 1: 10,10000 rpms of processing 10min of high speed under room temperature, filter after 4000 rpms of lower homogeneous of low speed extract 45min again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, with 0.1 mole of every liter of sodium hydroxide neutralization, the lower 1000 rpms of centrifugal 15min of normal temperature go precipitation, collect supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains Hylocereus undatus pericarp pigment (extraction yield 96.98%, color: redness).
the supernatant liquor (pigment extract) that step (3) is obtained activates through methyl alcohol in advance, the ODS C-18 solid phase extraction column that the HCl solution equilibria of 0.01% (volume fraction) is crossed carries out separation and purification, add a certain amount of pigment extract, pigment is adsorbed on post, then use the 0.01%HCl solution of 5 times of volumes with sugar, the water-soluble substanceses such as acid wash, ethyl acetate with 5 times of volumes washes Polyphenols again, Flavonoid substances, at last with the methanol solution that contains 0.01%HCl with the pigment wash-out, collect elutriant, 35 ℃ of lower vacuum concentration, eliminate methyl alcohol, concentrated solution is with 0.01% HCl solution dilution constant volume, get Hylocereus undatus pigment refined solution, carrying out the UV-Vis collection of illustrative plates detects, and HPLC detects, result is seen respectively Fig. 3 and Fig. 4.
Embodiment 10:
(1) get fresh lichee shell drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram Litchi exocarp powder, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 2.0, solid-liquid ratio is 1: 5 (quality volume fraction), 9000 rpms of processing 5min of high speed under room temperature, filter after 3000 rpms of lower homogeneous of low speed extract 30min again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, with 0.1 mole of every liter of sodium hydroxide solution neutralization, the lower 1000 rpms of centrifugal 5min of normal temperature collect supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the Litchi exocarp pigment, pigment extraction yield 96.15%, and color: chestnut is brown.
Embodiment 11:
(1) get fresh lichee shell drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram Litchi exocarp powder, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 3.0, solid-liquid ratio is 1: 7 (quality volume fraction), changing at a high speed 9000 rpms under room temperature processed 10 minutes, filter after 4000 rpms of lower homogeneous of low speed extract 45 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 10 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the Litchi exocarp pigment, pigment extraction yield 96.32%, and color: chestnut is brown.
Embodiment 12:
(1) get fresh lichee shell drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram Litchi exocarp powder, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 5.0, solid-liquid ratio is 1: 10 (quality volume fraction), changing at a high speed 10000 rpms under room temperature processed 20 minutes, filter after 4000 rpms of lower homogeneous of low speed extract 60 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 15 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the Litchi exocarp pigment, pigment extraction yield 96.67%, and color: chestnut is brown.
Embodiment 13:
(1) get fresh Semen Vitis viniferae drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram Semen Vitis viniferae powder, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 2.0, solid-liquid ratio is 1: 5 (quality volume fraction), 9000 rpms of processing 5min of high speed under room temperature, filter after 3000 rpms of lower homogeneous of low speed extract 30min again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, with 0.1 mole of every liter of sodium hydroxide solution neutralization, the lower 1000 rpms of centrifugal 5min of normal temperature collect supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the Semen Vitis viniferae pigment, pigment extraction yield 95.63%.
Embodiment 14:
(1) get fresh Semen Vitis viniferae drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram Semen Vitis viniferae powder, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 3.0, solid-liquid ratio is 1: 7 (quality volume fraction), changing at a high speed 9000 rpms under room temperature processed 10 minutes, filter after 4000 rpms of lower homogeneous of low speed extract 45 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 10 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the Semen Vitis viniferae pigment, pigment extraction yield 95.76%.
Embodiment 15:
(1) get fresh Semen Vitis viniferae drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram Semen Vitis viniferae powder, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 5.0, solid-liquid ratio is 1: 10 (quality volume fraction), changing at a high speed 10000 rpms under room temperature processed 20 minutes, filter after 4000 rpms of lower homogeneous of low speed extract 60 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 15 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the Semen Vitis viniferae pigment, pigment extraction yield 95.96%.
Embodiment 16:
(1) get fresh hickory nut epicarp drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 Keshan walnut husk powder, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 2.0, solid-liquid ratio is 1: 5 (quality volume fraction), 9000 rpms of processing 5min of high speed under room temperature, filter after 3000 rpms of lower homogeneous of low speed extract 30min again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, with 0.1 mole of every liter of sodium hydroxide solution neutralization, the lower 1000 rpms of centrifugal 5min of normal temperature collect supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the hickory nut epicarp pigment, pigment extraction yield 95.63%.
Embodiment 17:
(1) get fresh hickory nut epicarp drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 Keshan walnut husk powder, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 3.0, solid-liquid ratio is 1: 7 (quality volume fraction), changing at a high speed 9000 rpms under room temperature processed 10 minutes, filter after 4000 rpms of lower homogeneous of low speed extract 45 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 10 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the hickory nut epicarp pigment, pigment extraction yield 95.76%.
Embodiment 18:
(1) get fresh hickory nut epicarp drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 Keshan walnut husk powder, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 5.0, solid-liquid ratio is 1: 10 (quality volume fraction), changing at a high speed 10000 rpms under room temperature processed 20 minutes, filter after 4000 rpms of lower homogeneous of low speed extract 60 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 15 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the hickory nut epicarp pigment, pigment extraction yield 95.96%.
Embodiment 19:
(1) get fresh acorn cup drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram acorn-case powders, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 2.0, solid-liquid ratio is 1: 5 (quality volume fraction), 9000 rpms of processing 5min of high speed under room temperature, filter after 3000 rpms of lower homogeneous of low speed extract 30min again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, with 0.1 mole of every liter of sodium hydroxide solution neutralization, the lower 1000 rpms of centrifugal 5min of normal temperature collect supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains Brown Pigment From Acorn Shells, pigment extraction yield 96.85%.
Embodiment 20:
(1) get fresh acorn cup drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram acorn-case powders, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 3.0, solid-liquid ratio is 1: 7 (quality volume fraction), changing at a high speed 9000 rpms under room temperature processed 10 minutes, filter after 4000 rpms of lower homogeneous of low speed extract 45 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 10 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains Brown Pigment From Acorn Shells, pigment extraction yield 97.22%.
Embodiment 21:
(1) get fresh acorn cup drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram acorn-case powders, adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 5.0, solid-liquid ratio is 1: 10 (quality volume fraction), changing at a high speed 10000 rpms under room temperature processed 20 minutes, filter after 4000 rpms of lower homogeneous of low speed extract 60 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 15 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains Brown Pigment From Acorn Shells, pigment extraction yield 98.03%.
Embodiment 22:
(1) get fresh peel of Citrus reticulata Blanco drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram citrus peel meals, adding volume fraction is 60% ethanol, and solid-liquid ratio is 1: 5 (quality volume fraction), under room temperature at a high speed 10000 rpms process 10min, filter after 3000 rpms of lower homogeneous of low speed extract 60 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, centrifugal 10 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the peel of Citrus reticulata Blanco pigment, pigment extraction efficiency 90.8%, color: yellowish brown.
Embodiment 23:
(1) get fresh peel of Citrus reticulata Blanco drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram citrus peel meals, adding volume fraction is 70% ethanol, and solid-liquid ratio is 1: 20 (quality volume fraction), under room temperature at a high speed 9000 rpms processed 20 minutes, filter after 3000 rpms of lower homogeneous of low speed extract 60 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, centrifugal 10 minutes of lower 1200 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the peel of Citrus reticulata Blanco pigment, pigment extraction efficiency 91.4%, color: yellowish brown.
Embodiment 24:
(1) get fresh peel of Citrus reticulata Blanco drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram citrus peel meals, adding volume fraction is 80% ethanol, solid-liquid ratio is 1: 5) (quality volume fraction), under room temperature, 10000 rpms of processing of high speed are 5 minutes, filter after 3000 rpms of lower homogeneous of low speed extract 30 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, centrifugal 10 minutes of lower 1500 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the peel of Citrus reticulata Blanco pigment, pigment extraction efficiency 91.9%, color: yellowish brown.
Embodiment 25:
(1) get fresh peel of Citrus reticulata Blanco drying, pulverizing, mistake 100 mesh sieves, standby.
(2) take 100 gram citrus peel meals, adding volume fraction is 90% ethanol, solid-liquid ratio is 1: 10 (quality volume fraction), under room temperature, 10000 rpms of processing of high speed are 20 minutes, filter after the lower homogeneous of 4000 rpms of low speed extract 120 (changing 60 into) minute again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, centrifugal 10 minutes of lower 2000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains the peel of Citrus reticulata Blanco pigment, pigment extraction efficiency 94.7%, color: yellowish brown.
In this embodiment, the extraction yield of peel of Citrus reticulata Blanco pigment is 90-95%, stable high, the quality better of gained pigment, to light, heat, and the part chemical substance stable, good with Partial Food additive property mixed with the common food raw material.
Embodiment 26:
(1) get fresh hazelnut shell drying, pulverizing, mistake 40 mesh sieves, take 5 grams standby.
(2) adding volume fraction is 50% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 3.0, solid-liquid ratio is 1: 10 (quality volume fraction), under room temperature, 10000 rpms of processing of high speed are 20 minutes, filter after 1000 rpms of lower homogeneous of low speed extract 120 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 10 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains hazelnut shell brown pigment 0.34 gram, pigment yield 6.8%.
Embodiment 27:
(1) get fresh hazelnut shell drying, pulverizing, mistake 50 mesh sieves, take 5 grams standby.
(2) adding volume fraction is 60% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 3.0, solid-liquid ratio is 1: 20 (quality volume fraction), under room temperature, 10000 rpms of processing of high speed are 20 minutes, filter after 2000 rpms of lower homogeneous of low speed extract 3 hours again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 10 minutes of lower 1200 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains hazelnut shell brown pigment 0.35 gram, pigment yield 7.0%.
Embodiment 28:
(1) get fresh hazelnut shell drying, pulverizing, mistake 50 mesh sieves, take 5 grams standby.
(2) adding volume fraction is 60% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 3.0, solid-liquid ratio is 1: 25 (quality volume fraction), under room temperature, 10000 rpms of processing of high speed are 20 minutes, filter after 2000 rpms of lower homogeneous of low speed extract 3 hours again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 10 minutes of lower 1200 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains hazelnut shell brown pigment 0.36 gram, pigment yield 7.2%.
Embodiment 29:
(1) get fresh hazelnut shell drying, pulverizing, mistake 60 mesh sieves, take 5 grams standby.
(2) adding volume fraction is 70% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 3.0, solid-liquid ratio is 1: 30 (quality volume fraction), under room temperature, 10000 rpms of processing of high speed are 20 minutes, filter after 3000 rpms of lower homogeneous of low speed extract 3.5 hours again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 10 minutes of lower 1500 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains hazelnut shell brown pigment 0.38 gram, pigment yield 7.6%.
Embodiment 30:
(1) get fresh hazelnut shell drying, pulverizing, mistake 80 mesh sieves, take 5 grams standby.
(2) adding volume fraction is 80% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 3.0, solid-liquid ratio is 1: 40 (quality volume fraction), under room temperature, 10000 rpms of processing of high speed are 20 minutes, filter after 4000 rpms of lower homogeneous of low speed extract 4 hours again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 10 minutes of lower 2000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains hazelnut shell brown pigment 0.39 gram, pigment yield 7.8%.
In this embodiment, the extraction yield of hazelnut shell brown pigment is 90-95%, stable high, the quality better of gained hazelnut shell brown pigment, to light, heat, and the part chemical substance stable, good with Partial Food additive property mixed with the common food raw material.
Embodiment 31:
(1) get fresh nectarine skin drying, pulverizing, mistake 10 mesh sieves, take 5 grams standby.
(2) adding volume fraction is 50% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 1.0, solid-liquid ratio is 1: 30 (quality volume fraction), under room temperature, 10000 rpms of processing of high speed are 20 minutes, filter after 3000 rpms of lower homogeneous of low speed extract 30 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 10 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains nectarine skin red pigment 0.36 gram, pigment extraction yield 7.23%, color: redness.
Embodiment 32:
(1) get fresh nectarine skin drying, pulverizing, mistake 20 mesh sieves, take 5 grams standby.
(2) adding volume fraction is 50% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 1.0, solid-liquid ratio is 1: 40 (quality volume fraction), under room temperature, 10000 rpms of processing of high speed are 20 minutes, filter after 3000 rpms of lower homogeneous of low speed extract 40 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 10 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains nectarine skin red pigment 0.39 gram, pigment extraction yield 7.83%, color: redness.
Embodiment 33:
(1) get fresh nectarine skin drying, pulverizing, mistake 20 mesh sieves, take 5 grams standby.
(2) adding volume fraction is 50% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 1.0, solid-liquid ratio is 1: 50 (quality volume fraction), under room temperature, 10000 rpms of processing of high speed are 20 minutes, filter after 3000 rpms of lower homogeneous of low speed extract 50 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 10 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains nectarine skin red pigment 0.356 gram, pigment extraction yield 7.12%, color: redness.
Embodiment 34:
1) get fresh Rhizoma Dioscoreae esculentae through washing, removal of impurities, oven dry, pulverizing, mistake 60 mesh sieves, standby.
2) take 5 gram chestnut shell powder, adding volume fraction is 95% ethanol, and 0.1 mole every liter hydrochloric acid adjust pH is 3.0, and solid-liquid ratio quality volume fraction is 1: 20.
3) under room temperature, 10000 rpms of high speed pre-treatment 10 minutes, then filter after 3000 rpms of lower homogeneous extract 1 hour.
4) with above-mentioned steps 3) in filter residue extract again once by abovementioned steps, filter.
5) merge twice filtrate, with the sodium hydroxide neutralization of 0.1 mole every liter, under 1000 rpms centrifugal 10 minutes, go precipitation, carry out lyophilize after the collection supernatant powdered, obtain Ipomoea batatas(L.)Lam 0.26 gram, pigment yield 5.2%.
Embodiment 35:
(1) get new light violet black sorghum husk drying, pulverizing, mistake 80 mesh sieves, take 5 grams standby.
(2) adding volume fraction is 95% ethanol, 0.1 the hydrochloric acid adjust pH of mole every liter is 3.0, solid-liquid ratio is 1: 30 (quality volume fraction), under room temperature, 10000 rpms of processing of high speed are 20 minutes, filter after 3000 rpms of lower homogeneous of low speed extract 60 minutes again, collect respectively filter residue, filtrate.
(3) filter residue is processed once by above-mentioned steps (2) again, merged twice filtrate after filtering, neutralize with 0.1 mole of every liter of sodium hydroxide solution, centrifugal 10 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after the decompression rotary evaporation is concentrated, and lyophilize is powdered, namely obtains purple black sorghum husk 0.31 gram, pigment yield 6.2%.
Claims (10)
1. the extracting method of a natural pigment is characterized in that comprising the following step:
(1) with raw material washing, dry, rear 100 mesh sieves of crossing of pulverizing, in the mixed solution of the aqueous hydrochloric acid of the aqueous ethanolic solution of percent by volume 60-95% and 0.1 mole every liter, carry out homogeneous and extract, the pH of described mixed solution is 2.0-5.0, filter after extracting, get filtrate; Described homogeneous extracts and comprises that high speed pretreatment stage and homogeneous extract the stage;
(2) with the neutralization of step (1) gained filtrate, centrifugal slagging-off, get supernatant liquor;
(3) supernatant liquor of step (2) gained is concentrated and dry, get final product;
Wherein, described raw material is chestnut shell, Testa sojae atricolor, Hylocereus undatus pericarp, Litchi exocarp, Semen Vitis viniferae, hickory nut epicarp, acorn cup, peel of Citrus reticulata Blanco, hazelnut shell, nectarine skin, Rhizoma Dioscoreae esculentae or purple black sorghum husk.
2. extracting method as claimed in claim 1 is characterized in that: in step (1), after the raw material after described pulverizing and sieving and mixed solution mixed, solid-to-liquid ratio was mass volume ratio (w/v) 1g: 5ml-1g: 10ml.
3. extracting method as claimed in claim 1, it is characterized in that: in step (1), the percent by volume of described aqueous ethanolic solution is 75%-95%.
4. extracting method as claimed in claim 1 is characterized in that: in step (1), it is commercially available high-shear homogenizing machine that described homogeneous extracts equipment used.
5. extracting method as claimed in claim 1 is characterized in that: in step (1), described high speed pretreatment stage condition is effect 5-20 minute under 5000-10000 rpm.
6. extracting method as claimed in claim 1 is characterized in that: in step (1), the condition that described homogeneous extracts the stage is to process 30-60 minute under 1000-4000 rpm.
7. extracting method as claimed in claim 1 is characterized in that: in step (1), the temperature that described homogeneous extracts the stage is 20～35 ℃; The time that described homogeneous extracts the stage is 5～8 hours; The number of times that described homogeneous extracts the stage is 1～3 time.
8. extracting method as claimed in claim 1 is characterized in that: in step (2), the method for described neutralization is for adding 0.1 mole of every liter of aqueous sodium hydroxide solution to adjust pH to 6～8; Described centrifugal condition is to process 5-30 minute under 200-2000 rpm.
9. extracting method as claimed in claim 8 is characterized in that: in step (2), described centrifugal condition is under 1000 rpms centrifugal 5-15 minute.
10. extracting method as claimed in claim 1, it is characterized in that: in step (3), described drying is lyophilize.
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| CN201110407459XA CN103160139A (en) | 2011-12-08 | 2011-12-08 | Extraction method for natural pigment |
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| CN103349921A (en) * | 2013-06-27 | 2013-10-16 | 北京市理化分析测试中心 | Multiwalled carbon nanotubes-polyether sulfone composite filter membrane as well as preparation method and application thereof |
| CN103360785A (en) * | 2013-07-16 | 2013-10-23 | 华南理工大学 | Natural pigment extracted from dragon fruit, as well as extract method and application thereof |
| CN103472056A (en) * | 2013-09-23 | 2013-12-25 | 集美大学 | Method for determining vitamin in fruits and vegetables by purple sweet potato anthocyanin and preparation method of purple sweet potato anthocyanin |
| CN103497534A (en) * | 2013-07-11 | 2014-01-08 | 佛山职业技术学院 | Method for extracting pitaya peel pigment by supercritical CO2 fluid |
| CN103571221A (en) * | 2013-10-31 | 2014-02-12 | 北京林业大学 | Extracting and purifying method of red-brown pigment of chestnut shells |
| CN103843852A (en) * | 2014-03-27 | 2014-06-11 | 东北林业大学 | Making method for sugar-free yeast fermentation cake |
| CN104178349A (en) * | 2014-08-18 | 2014-12-03 | 湖南博善思生物技术有限公司 | Method for preparing dragon fruit peel organic essential oil |
| CN104403358A (en) * | 2014-11-10 | 2015-03-11 | 云南瑞宝生物科技有限公司 | Preparation method of heatproof anthocyanin pigment |
| CN104497623A (en) * | 2014-12-04 | 2015-04-08 | 常州大学 | Method for extracting natural pigment from fruit shell |
| CN105421102A (en) * | 2015-12-22 | 2016-03-23 | 广州番禺职业技术学院 | Process of printing and dyeing leather with lemon peel juice |
| CN105670337A (en) * | 2016-03-15 | 2016-06-15 | 常州市阿曼特化工有限公司 | Technology method for extracting pigment from black soy bean peels |
| CN107163617A (en) * | 2017-06-09 | 2017-09-15 | 贵州省果树科学研究所 | A kind of dragon fruit pericarp pigment is extracted, purifying process |
| CN107266343A (en) * | 2017-06-20 | 2017-10-20 | 广州市桐晖药业有限公司 | A kind of extraction process of natural bata-carotene |
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| CN109079939A (en) * | 2018-08-09 | 2018-12-25 | 阜南县环宇柳木工艺制品有限公司 | A kind of wood staining method that performance is stable |
| CN109181356A (en) * | 2018-11-14 | 2019-01-11 | 罗莱生活科技股份有限公司 | A kind of technique extracted pigment from grape pip and prepare dyestuff |
| CN113100381A (en) * | 2021-05-14 | 2021-07-13 | 江南大学 | Pitaya peel powder for milk-containing beverage and preparation method and application thereof |
| CN114391662A (en) * | 2022-01-14 | 2022-04-26 | 浙江农林大学暨阳学院 | Device and method for extracting natural pigment in peel |
| CN115054547A (en) * | 2022-06-07 | 2022-09-16 | 青海民族大学 | Notopterygium root effervescent bath salt ball and preparation method thereof |
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| CN103349921A (en) * | 2013-06-27 | 2013-10-16 | 北京市理化分析测试中心 | Multiwalled carbon nanotubes-polyether sulfone composite filter membrane as well as preparation method and application thereof |
| CN103497534B (en) * | 2013-07-11 | 2015-05-20 | 佛山职业技术学院 | Method for extracting pitaya peel pigment by supercritical CO2 fluid |
| CN103497534A (en) * | 2013-07-11 | 2014-01-08 | 佛山职业技术学院 | Method for extracting pitaya peel pigment by supercritical CO2 fluid |
| CN103360785A (en) * | 2013-07-16 | 2013-10-23 | 华南理工大学 | Natural pigment extracted from dragon fruit, as well as extract method and application thereof |
| CN103472056A (en) * | 2013-09-23 | 2013-12-25 | 集美大学 | Method for determining vitamin in fruits and vegetables by purple sweet potato anthocyanin and preparation method of purple sweet potato anthocyanin |
| CN103472056B (en) * | 2013-09-23 | 2016-04-20 | 集美大学 | Purple sweet potato anthocyanin measures the method for fruits and vegetables vitamin and the preparation method of purple sweet potato anthocyanin |
| CN103571221A (en) * | 2013-10-31 | 2014-02-12 | 北京林业大学 | Extracting and purifying method of red-brown pigment of chestnut shells |
| CN103571221B (en) * | 2013-10-31 | 2015-04-01 | 北京林业大学 | Extracting and purifying method of red-brown pigment of chestnut shells |
| CN103843852A (en) * | 2014-03-27 | 2014-06-11 | 东北林业大学 | Making method for sugar-free yeast fermentation cake |
| CN104178349A (en) * | 2014-08-18 | 2014-12-03 | 湖南博善思生物技术有限公司 | Method for preparing dragon fruit peel organic essential oil |
| CN104403358B (en) * | 2014-11-10 | 2016-04-06 | 云南瑞宝生物科技股份有限公司 | A kind of preparation method of heat-resisting anthocyani pigment |
| CN104403358A (en) * | 2014-11-10 | 2015-03-11 | 云南瑞宝生物科技有限公司 | Preparation method of heatproof anthocyanin pigment |
| CN104497623A (en) * | 2014-12-04 | 2015-04-08 | 常州大学 | Method for extracting natural pigment from fruit shell |
| CN105421102A (en) * | 2015-12-22 | 2016-03-23 | 广州番禺职业技术学院 | Process of printing and dyeing leather with lemon peel juice |
| CN105670337A (en) * | 2016-03-15 | 2016-06-15 | 常州市阿曼特化工有限公司 | Technology method for extracting pigment from black soy bean peels |
| CN107163617A (en) * | 2017-06-09 | 2017-09-15 | 贵州省果树科学研究所 | A kind of dragon fruit pericarp pigment is extracted, purifying process |
| CN107266343B (en) * | 2017-06-20 | 2019-02-01 | 广州市桐晖药业有限公司 | A kind of extraction process of natural beta-carotin |
| CN107266343A (en) * | 2017-06-20 | 2017-10-20 | 广州市桐晖药业有限公司 | A kind of extraction process of natural bata-carotene |
| CN108635304A (en) * | 2018-08-06 | 2018-10-12 | 大连民族大学 | Edible Jasmine lipstick |
| CN108785230A (en) * | 2018-08-06 | 2018-11-13 | 大连民族大学 | More effect facial treatment liquid foundation of edible natural |
| CN109079939A (en) * | 2018-08-09 | 2018-12-25 | 阜南县环宇柳木工艺制品有限公司 | A kind of wood staining method that performance is stable |
| CN109181356A (en) * | 2018-11-14 | 2019-01-11 | 罗莱生活科技股份有限公司 | A kind of technique extracted pigment from grape pip and prepare dyestuff |
| CN113100381A (en) * | 2021-05-14 | 2021-07-13 | 江南大学 | Pitaya peel powder for milk-containing beverage and preparation method and application thereof |
| CN114391662A (en) * | 2022-01-14 | 2022-04-26 | 浙江农林大学暨阳学院 | Device and method for extracting natural pigment in peel |
| CN115054547A (en) * | 2022-06-07 | 2022-09-16 | 青海民族大学 | Notopterygium root effervescent bath salt ball and preparation method thereof |
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