CN105038298A - Wheat bran purple pigment extracting method - Google Patents
Wheat bran purple pigment extracting method Download PDFInfo
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- CN105038298A CN105038298A CN201510396227.7A CN201510396227A CN105038298A CN 105038298 A CN105038298 A CN 105038298A CN 201510396227 A CN201510396227 A CN 201510396227A CN 105038298 A CN105038298 A CN 105038298A
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- 235000015099 wheat brans Nutrition 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000001057 purple pigment Substances 0.000 title abstract 6
- 239000000049 pigment Substances 0.000 claims abstract description 25
- 239000000706 filtrate Substances 0.000 claims abstract description 23
- 241000209140 Triticum Species 0.000 claims abstract description 20
- 239000011347 resin Substances 0.000 claims abstract description 20
- 229920005989 resin Polymers 0.000 claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 235000021307 Triticum Nutrition 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 6
- 238000005119 centrifugation Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 235000013312 flour Nutrition 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical class Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000007667 floating Methods 0.000 claims abstract description 4
- 238000000967 suction filtration Methods 0.000 claims abstract description 4
- BBNQQADTFFCFGB-UHFFFAOYSA-N purpurin Chemical compound C1=CC=C2C(=O)C3=C(O)C(O)=CC(O)=C3C(=O)C2=C1 BBNQQADTFFCFGB-UHFFFAOYSA-N 0.000 claims description 66
- 239000003463 adsorbent Substances 0.000 claims description 10
- 239000000287 crude extract Substances 0.000 claims description 8
- 239000012141 concentrate Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000002336 sorption--desorption measurement Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000002386 leaching Methods 0.000 abstract 3
- 239000002244 precipitate Substances 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000005485 electric heating Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 241000196324 Embryophyta Species 0.000 description 6
- 239000000284 extract Substances 0.000 description 6
- 238000000605 extraction Methods 0.000 description 6
- 235000013305 food Nutrition 0.000 description 5
- 235000013339 cereals Nutrition 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002516 radical scavenger Substances 0.000 description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 230000007850 degeneration Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- HWYHZTIRURJOHG-UHFFFAOYSA-N luminol Chemical compound O=C1NNC(=O)C2=C1C(N)=CC=C2 HWYHZTIRURJOHG-UHFFFAOYSA-N 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 235000006008 Brassica napus var napus Nutrition 0.000 description 1
- 235000001169 Brassica oleracea var oleracea Nutrition 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 241001674939 Caulanthus Species 0.000 description 1
- 208000001953 Hypotension Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 235000004976 Solanum vernei Nutrition 0.000 description 1
- 241000352057 Solanum vernei Species 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229930014669 anthocyanidin Natural products 0.000 description 1
- 150000001453 anthocyanidins Chemical class 0.000 description 1
- 235000008758 anthocyanidins Nutrition 0.000 description 1
- 235000010208 anthocyanin Nutrition 0.000 description 1
- 229930002877 anthocyanin Natural products 0.000 description 1
- 239000004410 anthocyanin Substances 0.000 description 1
- 150000004636 anthocyanins Chemical class 0.000 description 1
- 230000002019 anti-mutation Effects 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000002864 food coloring agent Nutrition 0.000 description 1
- 239000000989 food dye Substances 0.000 description 1
- 235000012055 fruits and vegetables Nutrition 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 208000021822 hypotensive Diseases 0.000 description 1
- 230000001077 hypotensive effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000001932 seasonal effect Effects 0.000 description 1
- POECFFCNUXZPJT-UHFFFAOYSA-M sodium;carbonic acid;hydrogen carbonate Chemical compound [Na+].OC(O)=O.OC([O-])=O POECFFCNUXZPJT-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/899—Poaceae or Gramineae (Grass family), e.g. bamboo, corn or sugar cane
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Pharmacology & Pharmacy (AREA)
- Botany (AREA)
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- Medicinal Chemistry (AREA)
- Alternative & Traditional Medicine (AREA)
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- Biotechnology (AREA)
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- General Health & Medical Sciences (AREA)
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- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a wheat bran purple pigment extracting method which aims to realize high efficiency, good pigment color formation and high purity. The wheat bran purple pigment extracting method comprises the steps of crushing wheat bran, which is generated in the process of grinding purple wheat into flour, to 300 meshes; mixing the crushed wheat bran with a NaOH solution in a mass-volume ratio of 1 to 4 to obtain a mixture, leaching the mixture for 1 hour at the room temperature, and carrying out filtering; leaching and filtering filter residues twice according to the last step, and mixing filtrates which are obtained by the three times of leaching and filtering separately; cooling the mixed filtrates to 10-12 DEG C, adding saturated hydrochloric acid to regulate the pH value of the mixed filtrates to 4, carrying out 10000g lower-temperature centrifugation on the mixed filtrates for 10 minutes and then discarding precipitates, and removing a film-like floating object in liquid supernatant to obtain a crude purple pigment extracting solution; under an acidic environment with a pH value of 4, adsorbing pigment by macroporous adsorption resin, desorbing the pigment adsorbed in the resin by an ethanol solution to obtain eluant; starting a vacuum pump to carry out suction filtration and concentration; performing re-concentration by a rotary evaporator; carrying out 10000g centrifugation for 10 minutes by a high-speed centrifugal machine, and then removing precipitates to obtain a purple pigment extracting solution; and setting an air inlet temperature of a dryer to 140 DEG C, setting an air outlet temperature of the dryer to 60 DEG C, and adopting electric heating compensation to assist drying, thereby obtaining purple pigment powder.
Description
Technical field
The present invention relates to food dye preparation field, be specifically related to a kind of method extracting purpurin from common purple Testa Tritici.
Background technology
The industries such as current food and drink mostly use synthetic colour, very easily HUMAN HEALTH is exerted an adverse impact, along with the raising of people's living standard, constantly pursue the quality of life of health, nature and high-quality, the development and application of natural pigment is more and more come into one's own.The purpurin safety non-toxic extracted from plant; there is anti-mutation, anti-oxidant, hypotensive; protection liver; preventing cancer, the effect increasing food nutrient composition and extend the shelf life, is mainly used in the red-purple tinting material of food; as (Pascual-Teresa1SD such as beverage, pickled prod, jelly, milky-drinks, happy sugar prod and healthcare products; Sanchez-BallestaMT.Anthocyanins:fromplanttohealth.Phytoc hemistryReviews, 2008,7:281 ~ 299; KirakosyanA, SeymourEM, UrcuyoLlanesDE, KaufmanPB, BollingSF.Chemicalprofileandantioxidantcapacitiesoftartc herryproducts.FoodChemistry, 2009,115 (1): 20 ~ 25).In recent years, along with the range of application of plant purpurin constantly expands, demand is huge, and especially Japan and Korea S offer high prices for plant purpurin for medicine and field of food to surpass.Current plant purpurin is separation and Extraction from purple potato, wild cabbage and purple corn mostly, but these method many employings fresh plants are material, by seasonal effect comparatively large (Chinese patent application CN101735647, CN101319095,102627870).Therefore, find and develop new plant purpurin and to originate attention always.
Wheat with purple grain principal feature is that trace element and protein, aminoacids content are high, and nutritive value is outstanding, and have Development volue, cultivated area constantly expands.Wheat with purple grain presents purple because its seed coat is rich in natural pigment, contained natural purpurin is nontoxic to human security, have stronger tint permanence and stability to food-drink, in promotion human body health and prevention cardiovascular and cerebrovascular diseases, have remarkable effect, be comparatively unique germ plasm resource.The research of current plant purpurin concentrates on fruits and vegetables mostly, composition and the determination study thereof of purple Wheat Species skin pigment are little, be only limitted to laboratory level (Zhao Shancang, Liu Bin, Zhao Lingjun etc., blue, wheat with purple grain seed anthocyanogen compositional analysis, Scientia Agricultura Sinica, 2010,43 (19): 4072 ~ 4080); The method that acidic ethanol method extracts purple wheat wheat bran pigment also has report, but this method is extracted under the strong acidic condition of pH=1, cause a large amount of pigmental degeneration, active bio afunction (Tang Xiaozhen, Liu Bin, Jiang Yuan, Sun Lanzhen, Yin Yan chessboard, acidic ethanol method extracts the Study of operational conditions of purple wheat wheat bran pigment, China's grain and oil journal, 2008,23 (5): 24 ~ 27).The document not having wheat purpurin to extract in a large number and patent report.Therefore, to the extraction of purple Wheat Species skin pigment, application and exploitation, there is important investigation and application to be worth.
Summary of the invention
The object of the invention is to the deficiency overcoming above-mentioned prior art, the Testa Tritici purpurin extracting method that a kind of pigment extraction efficiency is high, pigment is of good quality, purity is high is provided.
Step of the present invention is as follows:
(1) Feedstock treating: the wheat bran that purple wheat flour milling produces is broken to 300 orders with wheat bran pulverizer;
(2) buck lixiviate: by pulverize after wheat bran and concentration be the NaOH solution of 1.5% by quality: volume be 1:4 mixing, fully stir, every 20 minutes stir 1 time, lixiviate 1 hour under room temperature, gained extracting solution 100 order metre filter obtain filtrate; Wherein the volume unit of the quality of wheat bran raw material and NaOH solution is than for gram than milliliter or kilogram than rising;
(3) filtrate is mixed: by the filter residue after lixiviate by above-mentioned steps lixiviate again, filtration secondary, then the filtrate of three times is mixed;
(4) centrifugal acquisition crude extract: when filtrate temperature to be mixed is down to 10 DEG C ~ 12 DEG C, adds the pH=4 that saturated hydrochloric acid makes filtrate, then filtrate is abandoned precipitation after 10000g low-temperature centrifugation 10min, obtains purpurin crude extract after removing the membranaceous floating matter in supernatant liquor;
(5) adsorption-desorption: after above-mentioned purpurin crude extract is used absorption with macroporous adsorbent resin pigment under the sour environment of pH=4, adopt concentration to be the pigment adsorbed in the ethanolic soln desorb resin of 60 ~ 65% (v/v), obtain elutriant;
(6) sodium filter membrane concentrates: poured into by elutriant in container and start vacuum pump suction filtration, use organic sodium filter membrane of resistance to ethanol to concentrate elutriant, obtain the concentrated solution that concentration is 10%;
(7) evaporation concentration: above-mentioned concentrated solution rotatory evaporator is carried out reconcentration, arranging vacuum tightness is 0.9MPa, makes concentrated solution volume reach 40% of stoste volume;
(8) separation and purification: remove throw out after above-mentioned concentrated solution is used the centrifugal 10min of supercentrifuge 10000g, obtain purpurin extracting solution;
(9) spraying dry: setting moisture eliminator inlet temperature is 140 DEG C, and air outlet temperature is 60 DEG C, adopts electrical heating combination drying aid, obtains purpurin powder.
Described purple wheat adopts peaceful spring No. 46 or agricultural university 3753.Described wheat bran mill type number is WFJ-15.Described macroporous adsorbent resin adopts AB-8 macroporous adsorbent resin, also can adopt other common resins.Described rotatory evaporator adopts the sub-flourish rotatory evaporator RE-52A in Shanghai.
Purpurin crude extract uses absorption with macroporous adsorbent resin pigment under the sour environment of pH=4, whip attachment filtered out filtrate after 2 hours, it is the pigment adsorbed in the ethanolic soln desorb resin of 60% ~ 65% (v/v) the resin concentration being adsorbed with pigment, desorb, after about 30 minutes, is filtered resin and is obtained elutriant; Resin water is reusable after rinsing;
Macroporous adsorbent resin adsorpting pigment under sour environment in above-mentioned steps (5), pH=4 is optimal envrionment conditions, extracts under the strong acidic condition of pH<3, can make a large amount of pigmental degeneration, active bio afunction.
In above-mentioned steps (9), drying means also can adopt lyophilize.
The present invention adopts the byproduct wheat bran of flour milling to be that raw material carries out pigment extraction, is applicable to producing in enormous quantities, and have economize on resources, feature that production cost is low; Wheat bran degree of crushing is good, and pigment extraction efficiency is high; The purpurin extracted is natural food colour, and safety is guaranteed; The extraction time of extract by solvents obviously shortens, comparatively efficiently.Pigment is of good quality, stability is high, quality better, directly can be used as the additives such as food, medicine, healthcare products.
Accompanying drawing explanation
Fig. 1 is purple Wheat Species skin pigment uv-spectrogram scanning curve.
Embodiment
Following embodiment is convenient to understand the present invention better, but does not limit the present invention.Experimental technique in following embodiment, if no special instructions, is ordinary method.Experiment material used in following embodiment, if no special instructions, all can buy in routine biochemistry reagent shop.Wheat breed is purple wheat peaceful spring No. 46 and agricultural university 3753.
Concrete steps are:
(1) be that the wheat bran pulverizer of WFJ-15 is broken to 300 orders the wheat bran that purple wheat flour milling produces by model;
(2) pulverize after wheat bran get 0.5Kg, add concentration be 1.5% NaOH solution 2.0L carry out lixiviate, every 20 minutes stir 1 time, fully stir, under room temperature extract within 1 hour, obtain filtrate; By filtrate with 100 order metre filter;
(3) filter residue after lixiviate pressed above-mentioned steps lixiviate again, filter secondary, then the filtrate of three times is mixed;
(4) above-mentioned filtrate temperature is down to 10 DEG C ~ 12 DEG C, adds the pH=4 that saturated hydrochloric acid makes filtrate, then filtrate is got supernatant after 10000g low-temperature centrifugation 10min, remove the membranaceous floating matter in precipitation and supernatant liquor, obtain purpurin crude extract;
(5) use macroporous adsorbent resin AB-8 adsorpting pigment, at sour environment (pH=4) upper prop, after the even colour band of the saturated formation of macroporous adsorbent resin, adopt concentration to be the pigment adsorbed in the ethanolic soln desorb resin of 60% ~ 65%;
(6) elutriant is poured in container start vacuum pump suction filtration, use organic sodium filter membrane of resistance to ethanol to concentrate stripping liquid, obtain the concentrated solution of concentration 10%;
(7) adopt rotatory evaporator to concentrate above-mentioned concentrated solution, vacuum tightness 0.9MPa is set, concentrated solution concentration is reached 40%;
(8) above-mentioned concentrated solution is removed precipitation with after the centrifugal 10min of supercentrifuge 10000g again, get supernatant;
(9) by dry for the liquid spray obtained after separation, setting moisture eliminator inlet temperature 140 DEG C, air outlet temperature 60 DEG C, obtains purple powder finished product 3.1g after drying, look valency is 91, and this powder is the present embodiment and prepares gained purpurin dry powder;
The purpurin dry powder that takes a morsel is dissolved in 30% ethanolic soln and carries out ultraviolet-visible spectrum scanning, and as can be seen from Figure 1 at 310 ~ 355nm and 520 ~ 540nm place, anthocyanidin and anthocyanogen have stronger absorption peak and occur.
Table 1. purple wheat seed coat purpurin extract nature examination
| Project | Standard | Measured value | Conclusion | Remarks |
| Look valency | ≥30 | 91 | Qualified | |
| Heavy metal | ≤40 μg/g | ＜24 μg/g | Qualified | In Pb |
| Plumbous | ≤8.0 μg/g | Do not detect | Qualified | |
| Arsenic | ≤4.0μg/g | Do not detect | Qualified | With AS 2O 3 |
| Weight loss on drying | ≤10% | 5.9% | Qualified | |
| Ash content | ≤6% | 2.1% | Qualified |
Remove H
2o
2ability detects: containing H
2o
2after adding the wheat purpurin of different concns in luminol,3-aminophthalic acid cyclic hydrazide luminescence system, the absorbance of system or luminous intensity reduce, and show that purpurin has the effect of Scavenger of ROS.The antioxidant concentration added is higher, higher to the clearance rate of active oxygen.Concrete steps are: in mensuration bottle, add 100 μ l concentration is successively the H of 5mmol/L
2o
2and the sodium carbonate-bicarbonate damping fluid 500 μ l of 0.2mol/L, pH=9.7, then adding the test sample of different concns, distilled water is as blank; CTMAB (cetyl trimethylammonium bromide) the equivalent mixed liquor 500 μ l of the luminol,3-aminophthalic acid cyclic hydrazide and 10mmol/L that add 5mmol/L after mixing starts reaction, sample is placed in liquid flashing determining instrument, time delay 10 seconds, measure the luminous intensity in 12 seconds, each sample arranges three and repeats to average.Relative clearance rate is: clearance rate=(blank value-sample value)/blank value × 100%.IC
50required scavenger concentration when luminous for inhibited oxidation 50%, maps to scavenger concentration to remove percentage, can be calculated IC by straight-line equation
50size be 1.436, show that wheat purpurin has stronger removing H
2o
2ability.
Claims (5)
1. a Testa Tritici purpurin extracting method, is characterized in that:
(1) Feedstock treating: the wheat bran that purple wheat flour milling produces is broken to 300 orders with wheat bran pulverizer;
(2) buck lixiviate: by pulverize after wheat bran and concentration be the NaOH solution of 1.5% by quality: volume be 1:4 mixing, fully stir, every 20 minutes stir 1 time, lixiviate 1 hour under room temperature, gained extracting solution 100 order metre filter obtain filtrate; Wherein the volume unit of the quality of wheat bran raw material and NaOH solution is than for gram than milliliter or kilogram than rising;
(3) filtrate is mixed: by the filter residue after lixiviate by above-mentioned steps lixiviate again, filtration secondary, then the filtrate of three times is mixed;
(4) centrifugal acquisition crude extract: when filtrate temperature to be mixed is down to 10 DEG C ~ 12 DEG C, adds the pH=4 that saturated hydrochloric acid makes filtrate, then filtrate is abandoned precipitation after 10000g low-temperature centrifugation 10min, obtains purpurin crude extract after removing the membranaceous floating matter in supernatant liquor;
(5) adsorption-desorption: after above-mentioned purpurin crude extract is used absorption with macroporous adsorbent resin pigment under the sour environment of pH=4, adopt concentration to be the pigment adsorbed in the ethanolic soln desorb resin of 60 ~ 65% (v/v), obtain elutriant;
(6) sodium filter membrane concentrates: poured into by elutriant in container and start vacuum pump suction filtration, use organic sodium filter membrane of resistance to ethanol to concentrate elutriant, obtain the concentrated solution that concentration is 10%;
(7) evaporation concentration: above-mentioned concentrated solution rotatory evaporator is carried out reconcentration, arranging vacuum tightness is 0.9MPa, makes concentrated solution volume reach 40% of stoste volume;
(8) separation and purification: remove throw out after above-mentioned concentrated solution is used the centrifugal 10min of supercentrifuge 10000g, obtain purpurin extracting solution;
(9) spraying dry: setting moisture eliminator inlet temperature is 140 DEG C, and air outlet temperature is 60 DEG C, adopts electrical heating combination drying aid, obtains purpurin powder.
2. Testa Tritici purpurin extracting method according to claim 1, is characterized in that described purple wheat adopts peaceful spring No. 46 or agricultural university 3753.
3. Testa Tritici purpurin extracting method according to claim 1 and 2, is characterized in that described wheat bran mill type number is WFJ-15.
4. Testa Tritici purpurin extracting method according to claim 1 and 2, is characterized in that described macroporous adsorbent resin adopts AB-8 macroporous adsorbent resin.
5. Testa Tritici purpurin extracting method according to claim 1 and 2, is characterized in that described rotatory evaporator adopts the sub-flourish rotatory evaporator RE-52A in Shanghai.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510396227.7A CN105038298A (en) | 2015-07-08 | 2015-07-08 | Wheat bran purple pigment extracting method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510396227.7A CN105038298A (en) | 2015-07-08 | 2015-07-08 | Wheat bran purple pigment extracting method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883638A (en) * | 2017-02-28 | 2017-06-23 | 晨光生物科技集团股份有限公司 | A kind of continuous centrifugal improves the industrial method of capsicum red pigment quality |
| US20240124833A1 (en) * | 2022-02-24 | 2024-04-18 | Mushlabs Gmbh | Production of coloured fungal mycelium |
-
2015
- 2015-07-08 CN CN201510396227.7A patent/CN105038298A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 蒋彦婕等: "大孔树脂对紫小麦麸皮花色苷的纯化动力学", 《江苏农业学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883638A (en) * | 2017-02-28 | 2017-06-23 | 晨光生物科技集团股份有限公司 | A kind of continuous centrifugal improves the industrial method of capsicum red pigment quality |
| CN106883638B (en) * | 2017-02-28 | 2019-08-20 | 晨光生物科技集团股份有限公司 | A kind of continuous centrifugal improves the industrial method of capsicum red pigment quality |
| US20240124833A1 (en) * | 2022-02-24 | 2024-04-18 | Mushlabs Gmbh | Production of coloured fungal mycelium |
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