CN105524482A - Hylocereus polyrhizus flesh and pericarp red pigment and extraction method thereof - Google Patents
Hylocereus polyrhizus flesh and pericarp red pigment and extraction method thereof Download PDFInfo
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- CN105524482A CN105524482A CN201510985861.4A CN201510985861A CN105524482A CN 105524482 A CN105524482 A CN 105524482A CN 201510985861 A CN201510985861 A CN 201510985861A CN 105524482 A CN105524482 A CN 105524482A
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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
- C09B23/00—Methine or polymethine dyes, e.g. cyanine dyes
- C09B23/10—The polymethine chain containing an even number of >CH- groups
- C09B23/105—The polymethine chain containing an even number of >CH- groups two >CH- groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/02—Heterocyclic radicals containing only nitrogen as ring hetero atoms
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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
Abstract
The invention relates to an extraction method of a Hylocereus polyrhizus flesh and pericarp red pigment. The method comprises the steps of flesh and pericarp pretreatment, fruit paste extraction and filtration, degumming treatment, macro-porous adsorption resin pretreatment, adsorption resin separation and enrichment, eluate dialysis, and concentration spray drying. The extraction method adopting an enzyme technology and an ultrasonic wave technology to extract natural edible red pigments from red heart Hylocereus undatus Britt in order to obtain a powder and an extract, the powder and the extract are dark purple, the maximum wavelength is 538nm, and the pigment extraction rate reaches up to 3.96%. The Hylocereus polyrhizus pigment belongs to betanin pigments, is a water-soluble pigment, and can be extremely easily dissolved in water, the solubility reduces with the reduction of the polarity of a solvent, and the Hylocereus undatus Britt pigment is soluble in methanol and ethanol, and is insoluble in acetic acid, ethyl ester, acetone, ether and other low polarity solvents. The Hylocereus undatus Britt pigment is stable when the pH value is 3-6, and is instable under alkaline conditions.
Description
Technical field
The present invention relates to a kind of extraction process of natural pigment, be specifically related to a kind of Hylocereus undatus pulp, pericarp red pigments and extracting method thereof.
Background technology
Hylocereus undatus (Latin literary fame: HylocereusundulatusBritt), also known as Herba Passiflorae Foetidae, celestial mamoncillo, Yu Longguo.Cactaceae, triangular prism belong to or seleniereus meja-lantous plant.The ground such as Costa Rica, Guatemala, Panama, Ecuador, Cuba, Colombia in Central America, country of origin.After import Taiwan Province of the country in Southeast Asia such as Vietnam, Thailand and China, the provinces and regions such as Hainan, Guangxi, Guangdong, Fujian, Yunnan of China's Mainland into.Hylocereus undatus not only taste is fragrant and sweet, also has very high nutritive value, and it combines in fruit, bud, vegetables, medical advantage.Not only nutritious, function is unique, seldom has disease and pest, uses any agricultural chemicals can normal growth hardly.Therefore, Hylocereus undatus be a kind of green, environmental protection fruit and have must the health care nutrient food of curative effect.In each hectogram Hylocereus undatus pulp, moisture content 83.75 grams, ash content 0.34 gram, crude fat 0.17 gram, crude protein 0.62 gram, robust fibre 1.21 grams, 13.91 grams, carbohydrate, heat 59.65 kilocalories, food fibre 1.62 grams, vitamins C 5.22 milligrams, 2.83 grams, fructose, glucose 7.83 grams, calcium 6.3-8.8 milligram, phosphorus 30.2-36.1 milligram, iron 0.55 ~ 0.65 milligram and lot of anthocyanin (red meat fruit kind is the richest), aqueous soluble dietary albumen, phyto albumin etc.
Hylocereus undatus is sweet flat, and main nutrient composition has protein, food fibre, Lin Suanna Vitamin B2 Sodium Phosphate, vitamin B3, vitamins C, iron, phosphorus, calcium, magnesium, potassium etc.Be rich in a large amount of pulp, there is abundant carotene, Vitamin B1 hcl, B2, B3, B12, C etc., (seed of black sesame) is more containing the abundant mineral substance such as calcium, phosphorus, iron and various enzyme, albumin, cellulosic and high density natural pigment anthocyanidin (especially be with red meat) in fruit stone, and colored, stem and tender shoots are more just like various effects of its close relative (aloe).
In the colourful daily life of food service industry, daily chemical industry, medicine industry and people, be unable to do without a kind ofly to be widely used, indispensable raw material-pigment.Pigment is divided into two large classes: chemosynthesis pigment and natural food colour.Chemosynthesis pigment mainly makes raw material, by forming of manually closing with the phenyl ring dyestuff separated in coal tar.And phenyl ring thing has extremely strong toxic side effect, even may make that people is carcinogenic, teratogenesis.Along with the continuous progress of science and technology and the progressively raising of standard of living, people more and more pay attention to health, also recognize the harm of chemosynthesis pigment to human body more and more clear-headedly.For the worry to health and safety problem, various countries are to the in addition strict restriction of the use of most synthetic colour, and some countries total ban use chemosynthesis pigment in food, medicine.Natural food colour mainly extracts from plant He in animal, as red pepper, tomato, Radix Dauci Sativae, pumpkin, herbal medicine etc.The haematochrome composition of tomato, capsicum extracts yield and is only 0.2%, and the peculiar smell in this kind of plant is not easily removed, also there is certain toxic side effect and the not strong feature of tinting strength in what have, so the quality and quantity of product is all difficult to the demand meeting market, therefore the source of goods is in short supply in market always, expensive.Foreign market natural pigment price in 2013 reached 210-240 dollar/kilogram, price per ton about 1,500,000 yuans.It is reported, the whole world is to the annual demand of natural food colour product 25000 tons, but throughput is limited, and market product is under-supply, and product breach is huge.At present, China still retains famille rose, Yuan Caihong, beautiful indigo plant, light blue, Sunset yellow, the large class chemosynthesis food dye of lemon yellow six, and in the application of each field yet based on chemosynthesis pigment additive.But European countries' Two decades years has been made laws and has been prohibitted the use.Visible, to the worry of food safety and eliminate this worry, require that we are in the more safe and reliable substitute of the market development.From 2009 to 2014 years, Nanning China-annual exhibition of Association of South-east Asian Nations's expo there are the various places businessmans such as Shanghai chemical industry additive product supply and marketing business, Xinjiang lycopene Product processing manufacturer, Wuhan, Qingdao, Changsha, Guangzhou all in the production and marketing trend exploring market natural edible additive product innovation; The products such as yellow pigment from Cucurbita pepo as Japanese, American-European in producer of Qingdao City pin, red mast of Huang of Hunan producer, yellow ginger are plain, look valency is bought higher, has also bought 650,000-80 ten thousand yuan for one ton.Both production and marketing thrive for natural edible additive, and supply falls short of demand.Therefore, edible natural food dye additive product, the just common voice that goes back to nature of the mankind.
Retrieve and extract the method for pigment about from dragon fruit pulp, pericarp or from pericarp, extract the method for pigment or extract the document of method of pigment from dragon fruit pulp below:
Application number: 200610089610.9; Applicant: BJ University of Aeronautics & Astronautics; Denomination of invention: a kind of method extracting water-soluble natural haematochrome from red heart Hylocereus undatus; Summary: the invention discloses a kind of method extracting water-soluble natural haematochrome from red heart Hylocereus undatus, extract natural red colouring matter by freezing broken wall method, distilled water extraction and biological enzyme in red heart Hylocereus undatus.Hylocereus undatus squeezes to obtain parting liquid after peeling, fragmentation, freeze thawing treatment, and remaining pomace obtains extracting solution with centrifugal after distilled water lixiviate, and merging parting liquid and extracting solution obtain pigment solution.Add polygalacturonase in pigment solution to destroy pectin wherein, underpressure distillation obtains dragon fruit pulp pigment.The inventive method simple and efficient, and remain the natural nutrient component in Hylocereus undatus to greatest extent, gained dragon fruit pulp pigment can be widely used in the many-sides such as heath food, beverage, makeup, pharmaceuticals.
Application number: 200410065617.8; Applicant: Feng Chang; Denomination of invention: the method extracting water-soluble red colouring matter from dragon fruit pulp, pericarp; Summary: a kind of method extracting water-soluble red colouring matter from dragon fruit pulp, pericarp, red skin red meat type dragon fruit pulp freeze thawing broken wall, crushing, centrifugation is it is characterized in that to obtain parting liquid, slag the ethanol soaks out and extracts is obtained extracting solution, and merging parting liquid and extracting solution obtain pigment solution; Pigment solution reclaims ethanol through underpressure distillation must contain glue pigment solution, then it is refining to come unstuck with ethanol, and moisture is removed in reverse osmosis, dry must product.Pericarp is dry in microwave oven, drying is obtained peel crushing, adds ethanol, pigment solution is extracted to obtain in leaching, the underpressure distillation on water-bath of gained pigment solution, reclaims ethanol, resistates add pH value be 5 buffer solution, filtration, dewater with reverse osmosis membrane concentrated, through microwave drying and get final product.Present method simple and efficient, remains the natural bioactive pigment composition in Hylocereus undatus extract to greatest extent.
Application number: 201510448098.1; Applicant: Zeng Fanzhang; Denomination of invention: a kind of method extracting natural pigment from Hylocereus undatus; Summary: a kind of method extracting natural pigment from Hylocereus undatus, is characterized in that, comprise the following steps: be broken into homogenate after 1) being cleaned by Hylocereus undatus; 2) after homogenate being mixed with water 1:1,100kHz ultrasonication 20min; 3) pressure filtration, obtains filtrate 1; 4) filter residue adds ethanol and to be mixed acquisition mixed solution, and the add-on of described ethanol and filter residue mass ratio are 8:1, by mixed solution 100kHz ultrasonication 20min; 5) filter, obtain filtrate 2; 6) after filtrate 1 and filtrate 2 being mixed, dry, obtained pigment dry product.The method extracting natural pigment from Hylocereus undatus of the present invention, method is simple, and production efficiency is high, and production cost is low, has good market outlook.
Application number: 201310561712.6, applicant: Wang Yuqing, denomination of invention: a kind of extracting method of Hylocereus undatus red pigments, summary: the extracting method that the present invention relates to a kind of Hylocereus undatus red pigments, belong to food processing technology field, its extracting method comprises the following steps the pre-treatment of a. Hylocereus undatus: Hylocereus undatus cleans, get pulp stripping and slicing, pulp and water are mixed with the mass ratio of 1:10, making beating, b. the extraction of pigment: regulate pH4.0 ~ 5.0, 40 ~ 50 DEG C of shaking bath 3 ~ 5h, cross leaching filter residue to extract than for 1:3 ~ 1:5 mixing water-bath with filter residue and quality, repeat to bleach look to pulp, collect each filtrate, c. lyophilize: dry certain hour at-10 ~-5 DEG C, d. dry: at 60 ~ 70 DEG C of constant temperature drying 6 ~ 8h, e. pulverize: low temperature liquid nitrogen is pulverized, obtain red pigments powder, the method technique is simple, effectively improves pigment yield, and protection pigment is not destroyed, and is adapted at industrial production.
Application number: 201310437588.2; Applicant: Zhong Renzhi industry bio tech ltd, Qingdao; Denomination of invention: a kind of Hylocereus undatus pericarp pigment extraction process; Summary: a kind of Hylocereus undatus pericarp pigment extraction process, is characterized in that Extraction solvent is ethanol, and the concentration of ethanol is 60% ~ 80%, and solid-liquid ratio is 1: 2 ~ 1: 5, and extraction time is 45min ~ 80min, and Extracting temperature is 25 DEG C ~ 50 DEG C.The method is easy and simple to handle, successful, can extract the natural bioactive pigment in Hylocereus undatus pericarp to greatest extent.
Application number: 201310299065.6; Applicant: South China Science & Engineering University; Denomination of invention: a kind of natural pigment of extracting from Hylocereus undatus and methods and applications; Summary: the invention discloses a kind of natural pigment of extracting from Hylocereus undatus and methods and applications, comprise the following steps: (1) prepares Hylocereus undatus dry powder and/or pigment crude extract; (2) Hylocereus undatus dry powder and/or pigment crude extract are loaded in semi-permeable membranes bag, it is 30 ~ 40 DEG C by distilled water nature dialysis dialysis temperature, penetration time be 12h ~ 24h at-50 DEG C ~-20 DEG C, lyophilize 24h under the condition of 30 ~ 50mbar, namely obtains Hylocereus undatus pigment.The red heart Hylocereus undatus pigment production method that present method is produced green, simple, convenient and because of semi-permeable membranes used reusable and economical.The Hylocereus undatus pigment solution that the present invention permeates gained can directly apply in the production of cool beverage, ice river in Henan Province icepro and milk tea etc.
Application number: 201310290535.2; Applicant: Foshan Vocationl Technical College; Denomination of invention: one utilizes supercritical CO
2the method of fluid extraction Hylocereus undatus pericarp pigment; Summary: the invention discloses one and utilize supercritical CO
2the method of fluid extraction Hylocereus undatus pericarp pigment, comprises the following steps: A. gets Hylocereus undatus pericarp, pulverizes and obtains Hylocereus undatus pericarp powder after drying; B. supercritical CO is carried out to Hylocereus undatus pericarp powder
2fluid extraction, adds polarity entrainment agent in extraction process, obtain Hylocereus undatus pericarp pigment solution and extract remainder, collects Hylocereus undatus pericarp pigment solution, for subsequent use; C. add the ethanol of 95% concentration to extract remainder, obtain extract remainder ethanolic soln, intensified by ultrasonic wave is carried out to extract remainder ethanolic soln, obtain Hylocereus undatus pericarp pigment solution; D. the Hylocereus undatus pericarp pigment solution mixing will obtained respectively in B and in C, then after carrying out underpressure distillation, rotary evaporation, obtain Hylocereus undatus pericarp pigment.Adopt the present invention can obtain highly purified Hylocereus undatus pericarp pigment, the present invention is simultaneously applicable to scale operation, is conducive to applying.
Application number: 201310180278.7; Applicant: Xuchang College; Denomination of invention: a kind of method extracting Hylocereus undatus pericarp pigment; Summary: a kind of method extracting Hylocereus undatus pericarp pigment, is characterized in that Extraction solvent is ethanol, and the concentration of ethanol is 55% ~ 75%, and solid-liquid ratio is 1: 2 ~ 1: 4, and extraction time is 50min ~ 70min, and Extracting temperature is 30 DEG C ~ 40 DEG C.The method is easy and simple to handle, successful, can extract the natural bioactive pigment in Hylocereus undatus pericarp to greatest extent.
Above technology all can extract the pigment in Hylocereus undatus, but is all single use alcohol extracting or water extraction or ultrasonicly carries, and extraction yield is not high, and it is little to extract the pigment formulation obtained, and is not enough to the needs meeting people.And Hylocereus undatus pigment product wide market.The present invention's application enzyme engineering and ultrasonic wave engineering extract natural edible red pigments (powder-type and medicinal extract type) from Hylocereus undatus, belong to the whole nation pioneering.Product with its unique pure natural, nontoxic, harmless, tasteless, look fresh, strong coloring force and content is high, cost is low feature, and the advantage of technology, leads over world standard.
The Hylocereus undatus that the present invention adopts is " match dragon No. 1 " (contriver calls oneself) that contriver researches and develops for many years, and external form resembles drapes over one's shoulders the red lantern of imperial squama, peculiar attractive in appearance, noble lucky.Pulp is rose-colored, bright-coloured tempting, sugar degree more than 10% (pol 18-20 degree) and be fructose entirely, not containing sucrose and maltose, very easily absorbs, fresh and sweet tasty and refreshing, is with refined perfume (or spice).Detect through Guangxi food quality inspection institute and Beijing Disease Prevention and Control Centre, in fruit except rich vitamin A, B1, B2, B3, C, unsaturated fatty acids, calcium, zinc, iron, selenium and 18 seed amino acid compositions, particularly containing sulfoprotein, phyto albumin, anthocyanidin, soluble dietary fibre and chitosan that other fruit are rare, and effect is peculiar, very remarkable to the health-care effect of human body.
The high-new technology farming product of the real Sustainable high yield (Wan Yuantian) of new variety Hylocereus undatus.In plant development process, few disease and pest, need not use agricultural chemicals, and thus whole manure use does not have the residual contamination of fertilizer and pesticide, is a kind of environment-friendly type natural green food, is described as model, the century sage fruit of green ecological by modern.
Hylocereus undatus pericarp contains abundant pigment, experiment records and accounts for 21% of pigment total amount in fruit, edible and processing mesocarp is dropped, a kind of huge waste beyond doubt, therefore the variety source that pericarp pigment not only can widen pigment is extracted, meet the demand that people are growing to natural pigment, and natural resources can be made to obtain more rationally, more effectively developing, thus improve its value-added content of product, and create a new outlet for the deep processing of these agricultural-food, improve the economic benefit of the producer, manager further.
In order to overcome above-mentioned defect, the object of this invention is to provide a kind of Hylocereus undatus pulp, pericarp red pigments and extracting method thereof, namely application enzyme engineering and ultrasonic wave engineering extract natural edible red pigments (powder-type and medicinal extract type) from red heart Hylocereus undatus, product with its unique pure natural, nontoxic, harmless, tasteless, look fresh, strong coloring force and content is high, cost is low feature, and the advantage of technology, lead over world standard.
Summary of the invention
The object of this invention is to provide a kind of Hylocereus undatus pulp, pericarp red pigments and extracting method thereof, namely application zymotechnic and ultrasonic technology extract natural edible red pigments (powder-type and medicinal extract type) from red heart Hylocereus undatus.
Technical scheme of the present invention is achieved in that
Hylocereus undatus pulp, pericarp red pigments, pigmentary structures is as follows:
Hylocereus undatus pulp, pericarp red pigments extracting method, comprise the pre-treatment of pulp, pericarp, and pulp lixiviate is filtered, degumming process, macroporous adsorbent resin pre-treatment, polymeric adsorbent separation, enrichment, elutriant dialysis, the drying of elutriant concentrated spray, concrete steps are as follows:
(1) pre-treatment of pulp, pericarp: select medium well above, without rotting, without going mouldy, without disease and pest, fresh " imperial No. 1 of match " Hylocereus undatus, first with Hylocereus undatus fruit face under clean water, then water is outwelled, soak 10-15 minute with the sodium hexametaphosphate solution that mass percent is 0.01%-0.1% again, thoroughly wash away the metal ion of remained on surface; Finally clean with clear water, after draining away the water, remove the cyan base of leaf on pericarp, separating pericarp and pulp, be cut into small pieces pulp and pericarp, uses hollander pulping, obtain pulp, for subsequent use;
(2) pulp lixiviate is filtered: the pulp that step (1) obtains is delivered to pure water extractor in soak at room temperature 60-80min, and add the L-AA of pulp gross weight 0.5-1%, extend fading of haematochrome as antioxidant, after extraction terminates, obtain pulp liquid; Then pulp liquid is delivered to ultrasonic extraction tank and carry out ultrasonic extraction, extraction time is 90-120min, and Extracting temperature is 45-50 DEG C, extracts after terminating, and adopts separating centrifuge to carry out filtering separation to pulp liquid, gets upper strata extracting solution;
(3) degumming process: stir after adding polygalacturonase in the upper strata extracting solution that the volume proportion adding 1.5-3 milliliter polygalacturonase according to often liter of parting liquid obtains toward step (2) and come unstuck, upper strata extracting solution is made to become clear, upper strata extracting solution temperature when coming unstuck is 48-52 DEG C, usually time is 60-80min, come unstuck centrifugal after terminating, centrifugal rotational speed is 4000 revs/min, gets upper solution;
(4) macroporous adsorbent resin pre-treatment: X-5 macroporous adsorbent resin is placed in clean brown bottle, add the alcohol immersion 24 hours that volume fraction is 95%, outwell upper strata suspended substance, and activated resin, carry out degassed by vacuum outgas method to resin simultaneously, then adopting wet method dress post, is the ethanol-eluting resin column of 95% with triploid integration number, adds the not muddy and elutriant uv scan of isopyknic distilled water can't check absorption peak to washings in test tube; Be washed with distilled water to without ethanol taste again, effluent liquid is neutral, saves backup;
(5) polymeric adsorbent separation, enrichment: the upper solution that step (3) obtains is entered X-5 macroporous adsorptive resins with the adsorption flow rate of 2BV/h, when the absorbancy of effluent liquid is substantially equal with the absorbancy of pigment, be that eluent is to colourless with the aqueous solution of mass concentration to be 0.2%HCl-mass concentration be 40% ethanol, elution flow rate is 2BV/h, enrichment elutriant;
(6) elutriant dialysis: the elutriant that step (5) obtains is inserted the dialysis tubing that molecular weight cut-off is 3500, and extraneous solution is deionized water, changes once extraneous solution every 5 hours, and dialysis time is 13 hours, after dialysis terminates, obtains dialyzate A;
(7) dialyzate concentrated spray is dry: the NaCl adding the 1-1.5% of dialyzate A gross weight in the dialyzate A that step (6) obtains, and the KCl of dialyzate A gross weight 0.5-1%, obtains dialyzate B; By dialyzate B concentrating under reduced pressure, after rotary evaporation, carry out spraying dry 5-10min, obtain powder-type and medicinal extract type two kinds of pigment products, by pigment product cooling storage.
Sodium hexametaphosphate 99, molecular formula is Na
6o
18p
6, molecular weight is 611.7704, Yi Rongshui, is insoluble to organic solvent, colourless transparent glass sheet or white particulate crystallization.In the present invention, Sodium hexametaphosphate 99 can play the effect of the metal ion on chelating Hylocereus undatus pericarp surface, thus thoroughly removes the metal ion of Hylocereus undatus pericarp remained on surface, avoids its chromatophagous color and endangers the healthy of people.
L-AA (AscorbicAcid, 2,3,5,6-tetrahydroxy-2-hexenoic acid-4-lactone), also known as vitamins C, be a kind of acid polyol containing 6 carbon atoms, molecular formula is C
6h
8o
6, molecular weight is 176.12.L-AA is acid hexose derivative, is rare alcohol of formula saccharinic acid lactone, belongs to water soluble antioxidant.L-AA industry manufacturing process has two kinds, be one section of fermentation manufacturing method for porous of Reichstein invention, a kind of is that Yin Guanglin invents two sections of newer fermentation methods, can be used as foodstuff additive and uses, in the present invention as antioxidant, extend fading of Hylocereus undatus haematochrome.
X-5 macroporous adsorbent resin of the present invention is a kind of spherical, nonpolar polymer absorbant, this resin is a cross-linked polymer, it is different from early stage hydrophobic adsorption agent, hydrophilic radical is addition of in its skeleton structure, different from general ion exchange resin again, in its structure, only there is non-ionic function base.Based on the working method of uniqueness, make it have sizable specific surface area and suitable aperture, to Hylocereus undatus pulp, pericarp pigment, there is higher adsorptive power.In the present invention, macroporous adsorbent resin is adopted to carry out purifying to elutriant, primary attachment pigment.
Contriver, in experimentation, finds: before absorption, the maximum absorption band of Hylocereus undatus pulp pigment solution is at 538nm place, and this absorption peak is the charateristic avsorption band (510-540nm) of anthocyania pigment.After absorption reaches balance, the absorbancy at 538nm place declines, this illustrates that resin mainly adsorbs pigment, also the composition such as carbohydrate, organic acid may be contained in Hylocereus undatus pulp, pericarp pigment, and these materials seldom absorb or substantially do not absorb in the scope of visible ray, so the change absorbing the absorbancy of front and back represents the change of the concentration of pigment composition substantially.
With prior art a bit compared with, positively effect of the present invention is:
1, the object of this invention is to provide a kind of Hylocereus undatus pulp, pericarp red pigments extracting method, application zymotechnic and ultrasonic technology extract natural edible red pigments from red heart Hylocereus undatus, obtain powder-type and medicinal extract type two kinds of products, all in intense violet color, maximum wavelength is 538nm, and pigment extraction yield is up to 3.96%.Hylocereus undatus pigment belongs to betanin pigment, is water colo(u)r, very easily water-soluble, and the polarity with solvent reduces solvability and reduces, and dissolves in methyl alcohol and ethanol, is insoluble in the low value solvents such as acetic acid, second fat, acetone, ether.Stable under condition when pH=3-6, unstable in the basic conditions.
2, the red pigments that the inventive method obtains belongs to rose-red natural food colour, safe and reliable, natural in color, have nutrition and pharmacological action concurrently, the fields such as widespread use and food, medicine, makeup, enjoy domestic and international market to favor, domestic market demand is based on medicinal extract pigment, and world market then prefers the higher powder pigment of purity.
3, in the methods of the invention, Hylocereus undatus sorting, washing, remove metal ion, making beating, pure water extractor is sent to soak, add L-AA, fading of haematochrome is extended as oxygenant, ultrasonic extraction is carried out through ultrasonic extraction tank, filter, add polygalacturonase to come unstuck, extracting solution is made to become clear, recycling absorption with macroporous adsorbent resin, wash-out, elutriant is dialysed, remove mineral ion and glucide, add NaCl and KCl again, maintenance pigment solution is stablized, finally that solution concentrated spray is dry, powder-type and medicinal extract type two kinds of pigment products, by pigment product cooling storage.
4, in the inventive method, after red heart Hylocereus undatus adopts clear water flushing fruit face, Sodium hexametaphosphate 99 is also adopted to soak, play the effect of the metal ion on chelating Hylocereus undatus pericarp surface, thus thoroughly remove the metal ion of Hylocereus undatus pericarp remained on surface, avoid its chromatophagous color and endanger the healthy of people.
5, in the present invention, add polygalacturonase and intercellular pectin substance is degraded, cell is separated in tissue.Utilize polygalacturonase, a large amount of pectin in Hylocereus undatus pulp, pericarp are extracted out.Hylocereus undatus pulp, pericarp, in ultrasonic extraction process, can be subject to damage in various degree, use polygalacturonase can accelerate or improve dipping, the dissolving of tannin and coloring matter, improve its stability.
6, in the inventive method, ultrasonic wave is utilized to extract red heart Hylocereus undatus pigment, produce the multistage effect such as emulsification, diffusion, vibration, destroy the structure containing pigment plant tissue, accelerate the transfer of pigment composition, diffusion thus improve the leaching efficiency of pigment, the purity of pigment product.Ultrasonic extraction is compared with traditional extraction, and have the features such as speed is faster, extraction yield is higher, saving solvent, and it is by the restriction of compositional polarity, molecular size range, being widely used, is one of a kind of efficient, quick, energy-conservation present new and high technology.
7, in the inventive method, in the extraction, purifying of red heart Hylocereus undatus pigment, adopt macroporous adsorbent resin separation and purification, not only whole process less energy consumption, cost is low, and technique is simple, and the more traditional extraction process of the natural pigment product of gained soak, filter, concentrated, quality significantly improves, and pigment product impurities is few, and look valency is high.
8, in the present invention, elutriant is inserted the dialysis tubing that molecular weight cut-off is 3500, extraneous solution is deionized water, the biomacromolecule of the macromolecule in elutriant is trapped within bag, as pigment, and inorganic salt and molecular weight be 180.16 glucose and the continuous diffusion dialysis of carbohydrate small-molecule substance such as fructose to outside bag, until the concentration on both sides reaches balance inside and outside bag, thus the material such as the inorganic salt removed in elutriant and carbohydrate.
9, why the present invention adds NaCl and KCl in pigment extract, is to find to add Na because study contriver
+, K
+be conducive to Hylocereus undatus pulp, pericarp red pigments extracting solution stable, and color is more bright-coloured.
Accompanying drawing explanation
The chemical structural formula of Fig. 1 Hylocereus undatus pigment;
Ultraviolet ~ the visible spectrum of Fig. 2 Hylocereus undatus pigment;
Fig. 3 Hylocereus undatus pigment HPLC schemes.
Embodiment
Embodiment 1
Hylocereus undatus pulp, pericarp red pigments, pigmentary structures is as follows:
Hylocereus undatus pulp, pericarp red pigments extracting method, comprise the pre-treatment of pulp, pericarp, and pulp lixiviate is filtered, degumming process, macroporous adsorbent resin pre-treatment, polymeric adsorbent separation, enrichment, elutriant dialysis, the drying of elutriant concentrated spray, concrete steps are as follows:
(1) pre-treatment of pulp, pericarp: select medium well above, without rotting, without going mouldy, without disease and pest, fresh " imperial No. 1 of match " Hylocereus undatus, first with Hylocereus undatus fruit face under clean water, then water is outwelled, soak 10-15 minute with the sodium hexametaphosphate solution that mass percent is 0.01% again, thoroughly wash away the metal ion of remained on surface; Finally clean with clear water, after draining away the water, remove the cyan base of leaf on pericarp, separating pericarp and pulp, be cut into small pieces pulp and pericarp, uses hollander pulping, obtain pulp, for subsequent use;
(2) pulp lixiviate is filtered: the pulp that step (1) obtains is delivered to pure water extractor in soak at room temperature 60min, and adds the L-AA of pulp gross weight 0.5%, extend fading of haematochrome as antioxidant, obtains pulp liquid after extraction terminates; Then pulp liquid is delivered to ultrasonic extraction tank and carry out ultrasonic extraction, extraction time is 90min, and Extracting temperature is 45 DEG C, extracts after terminating, and adopts separating centrifuge to carry out filtering separation to pulp liquid, gets upper strata extracting solution;
(3) degumming process: stir after adding polygalacturonase in the upper strata extracting solution that the volume proportion adding 1.5 milliliters of polygalacturonases according to often liter of parting liquid obtains toward step (2) and come unstuck, upper strata extracting solution is made to become clear, upper strata extracting solution temperature when coming unstuck is 48 DEG C, usually time is 60min, come unstuck centrifugal after terminating, centrifugal rotational speed is 4000 revs/min, gets upper solution;
(4) macroporous adsorbent resin pre-treatment: X-5 macroporous adsorbent resin is placed in clean brown bottle, add the alcohol immersion 24 hours that volume fraction is 95%, outwell upper strata suspended substance, and activated resin, carry out degassed by vacuum outgas method to resin simultaneously, then adopting wet method dress post, is the ethanol-eluting resin column of 95% with triploid integration number, adds the not muddy and elutriant uv scan of isopyknic distilled water can't check absorption peak to washings in test tube; Be washed with distilled water to without ethanol taste again, effluent liquid is neutral, saves backup;
(5) polymeric adsorbent separation, enrichment: the upper solution that step (3) obtains is entered X-5 macroporous adsorptive resins with the adsorption flow rate of 2BV/h, when the absorbancy of effluent liquid is substantially equal with the absorbancy of pigment, be that eluent is to colourless with the aqueous solution of mass concentration to be 0.2%HCl-mass concentration be 40% ethanol, elution flow rate is 2BV/h, enrichment elutriant;
(6) elutriant dialysis: the elutriant A that step (5) obtains is inserted the dialysis tubing that molecular weight cut-off is 3500, and extraneous solution is deionized water, changes once extraneous solution every 5 hours, and dialysis time is 13 hours, after dialysis terminates, obtains dialyzate A;
(7) dialyzate concentrated spray is dry: the NaCl adding 1% of dialyzate A gross weight in the dialyzate A that step (6) obtains, and the KCl of dialyzate A gross weight 0.5%, obtains dialyzate B; By dialyzate B concentrating under reduced pressure, after rotary evaporation, carry out spraying dry 5min, obtain powder-type and medicinal extract type two kinds of pigment products, by pigment product cooling storage.
Embodiment 2
Hylocereus undatus pulp, pericarp red pigments, pigmentary structures is as follows:
Hylocereus undatus pulp, pericarp red pigments extracting method, comprise the pre-treatment of pulp, pericarp, and pulp lixiviate is filtered, degumming process, macroporous adsorbent resin pre-treatment, polymeric adsorbent separation, enrichment, elutriant dialysis, the drying of elutriant concentrated spray, concrete steps are as follows:
(1) pre-treatment of pulp, pericarp: select medium well above, without rotting, without going mouldy, without disease and pest, fresh " imperial No. 1 of match " Hylocereus undatus, first with Hylocereus undatus fruit face under clean water, then water is outwelled, soak 13 minutes with the sodium hexametaphosphate solution that mass percent is 0.07% again, thoroughly wash away the metal ion of remained on surface; Finally clean with clear water, after draining away the water, remove the cyan base of leaf on pericarp, separating pericarp and pulp, be cut into small pieces pulp and pericarp, uses hollander pulping, obtain pulp, for subsequent use;
(2) pulp lixiviate is filtered: the pulp that step (1) obtains is delivered to pure water extractor in soak at room temperature 70min, and adds the L-AA of pulp gross weight 0.8%, extend fading of haematochrome as antioxidant, obtains pulp liquid after extraction terminates; Then pulp liquid is delivered to ultrasonic extraction tank and carry out ultrasonic extraction, extraction time is 110min, and Extracting temperature is 48 DEG C, extracts after terminating, and adopts separating centrifuge to carry out filtering separation to pulp liquid, gets upper strata extracting solution;
(3) degumming process: stir after adding polygalacturonase in the upper strata extracting solution that the volume proportion adding 2.5 milliliters of polygalacturonases according to often liter of parting liquid obtains toward step (2) and come unstuck, upper strata extracting solution is made to become clear, upper strata extracting solution temperature when coming unstuck is 50 DEG C, usually time is 70min, come unstuck centrifugal after terminating, centrifugal rotational speed is 4000 revs/min, gets upper solution;
(4) macroporous adsorbent resin pre-treatment: X-5 macroporous adsorbent resin is placed in clean brown bottle, add the alcohol immersion 24 hours that volume fraction is 95%, outwell upper strata suspended substance, and activated resin, carry out degassed by vacuum outgas method to resin simultaneously, then adopting wet method dress post, is the ethanol-eluting resin column of 95% with triploid integration number, adds the not muddy and elutriant uv scan of isopyknic distilled water can't check absorption peak to washings in test tube; Be washed with distilled water to without ethanol taste again, effluent liquid is neutral, saves backup;
(5) polymeric adsorbent separation, enrichment: the upper solution that step (3) obtains is entered X-5 macroporous adsorptive resins with the adsorption flow rate of 2BV/h, when the absorbancy of effluent liquid is substantially equal with the absorbancy of pigment, be that eluent is to colourless with the aqueous solution of mass concentration to be 0.2%HCl-mass concentration be 40% ethanol, elution flow rate is 2BV/h, enrichment elutriant;
(6) elutriant dialysis: the elutriant that step (5) obtains is inserted the dialysis tubing that molecular weight cut-off is 3500, and extraneous solution is deionized water, changes once extraneous solution every 5 hours, and dialysis time is 13 hours, after dialysis terminates, obtains dialyzate A;
(7) dialyzate concentrated spray is dry: the NaCl adding 1.2% of dialyzate A gross weight in the dialyzate A that step (6) obtains, and the KCl of dialyzate A gross weight 0.8%, obtains dialyzate B; By dialyzate B concentrating under reduced pressure, after rotary evaporation, carry out spraying dry 8min, obtain powder-type and medicinal extract type two kinds of pigment products, by pigment product cooling storage.
Embodiment 3
Hylocereus undatus pulp, pericarp red pigments, pigmentary structures is as follows:
Hylocereus undatus pulp, pericarp red pigments extracting method, comprise the pre-treatment of pulp, pericarp, and pulp lixiviate is filtered, degumming process, macroporous adsorbent resin pre-treatment, polymeric adsorbent separation, enrichment, elutriant dialysis, the drying of elutriant concentrated spray, concrete steps are as follows:
(1) pre-treatment of pulp, pericarp: select medium well above, without rotting, without going mouldy, without disease and pest, fresh " imperial No. 1 of match " Hylocereus undatus, first with Hylocereus undatus fruit face under clean water, then water is outwelled, soak 15 minutes with the sodium hexametaphosphate solution that mass percent is 0.1% again, thoroughly wash away the metal ion of remained on surface; Finally clean with clear water, after draining away the water, remove the cyan base of leaf on pericarp, separating pericarp and pulp, be cut into small pieces pulp and pericarp, uses hollander pulping, obtain pulp, for subsequent use;
(2) pulp lixiviate is filtered: the pulp that step (1) obtains is delivered to pure water extractor in soak at room temperature 80min, and adds the L-AA of pulp gross weight 1%, extend fading of haematochrome as antioxidant, obtains pulp liquid after extraction terminates; Then pulp liquid is delivered to ultrasonic extraction tank and carry out ultrasonic extraction, extraction time is 120min, and Extracting temperature is 50 DEG C, extracts after terminating, and adopts separating centrifuge to carry out filtering separation to pulp liquid, gets upper strata extracting solution;
(3) degumming process: stir after adding polygalacturonase in the upper strata extracting solution that the volume proportion adding 3 milliliters of polygalacturonases according to often liter of parting liquid obtains toward step (2) and come unstuck, upper strata extracting solution is made to become clear, upper strata extracting solution temperature when coming unstuck is 52 DEG C, usually time is 80min, come unstuck centrifugal after terminating, centrifugal rotational speed is 4000 revs/min, gets upper solution;
(4) macroporous adsorbent resin pre-treatment: X-5 macroporous adsorbent resin is placed in clean brown bottle, add the alcohol immersion 24 hours that volume fraction is 95%, outwell upper strata suspended substance, and activated resin, carry out degassed by vacuum outgas method to resin simultaneously, then adopting wet method dress post, is the ethanol-eluting resin column of 95% with triploid integration number, adds the not muddy and elutriant uv scan of isopyknic distilled water can't check absorption peak to washings in test tube; Be washed with distilled water to without ethanol taste again, effluent liquid is neutral, saves backup;
(5) polymeric adsorbent separation, enrichment: the upper solution that step (3) obtains is entered X-5 macroporous adsorptive resins with the adsorption flow rate of 2BV/h, when the absorbancy of effluent liquid is substantially equal with the absorbancy of pigment, be that eluent is to colourless with the aqueous solution of mass concentration to be 0.2%HCl-mass concentration be 40% ethanol, elution flow rate is 2BV/h, enrichment elutriant;
(6) elutriant dialysis: the elutriant that step (5) obtains is inserted the dialysis tubing that molecular weight cut-off is 3500, and extraneous solution is deionized water, changes once extraneous solution every 5 hours, and dialysis time is 13 hours, after dialysis terminates, obtains dialyzate A;
(7) dialyzate concentrated spray is dry: the NaCl adding 1.5% of dialyzate A gross weight in the dialyzate A that step (6) obtains, and the KCl of dialyzate A gross weight 1%, obtains dialyzate B; By dialyzate B concentrating under reduced pressure, after rotary evaporation, carry out spraying dry 10min, obtain powder-type and medicinal extract type two kinds of pigment products, by pigment product cooling storage.
Embodiment 4
Hylocereus undatus pulp, pericarp red pigments are making the application in the characteristic reel powder of Guangxi, and concrete steps are as follows:
(1), 1000g rice in steep 6-12 hour is got, saturated to rice water suction;
(2), step (1) is absorbed water saturated after rice wear into Rice & peanut milk, denseness resemble cows milk;
(3), according to 1000g rice add haw fruit pulp, pericarp red pigments 2g standard in the Rice & peanut milk of step (2) gained, add pigment, obtain the Rice & peanut milk of red pigments, and stir;
(4), in caldron add water, after water boils, steaming plate is put in pot, micro-rolling steaming plate allows the Rice & peanut milk of red pigments tile and tries to get to the heart of a matter, and rotates steaming plate immediately, allow the Rice & peanut milk of red pigments be evenly distributed after putting into pot, thermally equivalent, cover pot cover, bean sheet jelly bloats bubble and can take the dish out of the pot in dish, after bean sheet jelly cooling, scrape surrounding off gently, turn-over, puts filling toward the smooth side according to personal like, can obtain red reel powder.
Embodiment 5
Hylocereus undatus pulp, pericarp red pigments are preparing the application in milk tea, and concrete steps are as follows:
(1), 500ml pure milk is heated to 80-85 DEG C;
(2), put into 2g tealeaves and stir a little, cover the vexed 5min of pot cover;
(3), filter after tealeaves and again milk tea is heated, add animality unsalted butter 100g;
(4), like that adding appropriate castor sugar is stirred to thawing according to individual;
(5), cooling after add Hylocereus undatus pulp of the present invention, pericarp red pigments 3g, namely available milk tea presents red-purple.
Pigment detects
The Hylocereus undatus pigment obtained by extracting method of the present invention is delivered to Guangxi University and is detected, and obtain the chemical structural formula of Fig. 1 Hylocereus undatus pigment, the ultraviolet ~ visible spectrum of Fig. 2 Hylocereus undatus pigment, Fig. 3 Hylocereus undatus pigment HPLC schemes.
Claims (4)
1. Hylocereus undatus pulp, pericarp red pigments, is characterized in that: pigmentary structures is as follows:
。
2. Hylocereus undatus pulp according to claim 1, pericarp red pigments extracting method, it is characterized in that: the pre-treatment comprising pulp, pericarp, pulp lixiviate is filtered, degumming process, macroporous adsorbent resin pre-treatment, polymeric adsorbent separation, enrichment, elutriant dialysis, the drying of elutriant concentrated spray, concrete steps are as follows:
(1) pre-treatment of pulp, pericarp: select medium well above, without rotting, without going mouldy, without disease and pest, fresh Hylocereus undatus, first with Hylocereus undatus fruit face under clean water, then water is outwelled, soak 10-15 minute with the sodium hexametaphosphate solution that mass percent is 0.01%-0.1% again, thoroughly wash away the metal ion of remained on surface; Finally clean with clear water, after draining away the water, remove the cyan base of leaf on pericarp, separating pericarp and pulp, be cut into small pieces pulp and pericarp, uses hollander pulping, obtain pulp, for subsequent use;
(2) pulp lixiviate is filtered: the pulp that step (1) obtains is delivered to pure water extractor in soak at room temperature 60-80min, and adds the L-AA of pulp gross weight 0.5-1%, obtains pulp liquid after extraction terminates; Then pulp liquid is delivered to ultrasonic extraction tank and carry out ultrasonic extraction, extract after terminating, adopt separating centrifuge to carry out filtering separation to pulp liquid, get upper strata extracting solution;
(3) degumming process: stir after adding polygalacturonase in the upper strata extracting solution that the volume proportion adding 1.5-3 milliliter polygalacturonase according to often liter of parting liquid obtains toward step (2) and come unstuck, upper strata extracting solution is made to become clear, come unstuck centrifugal after terminating, centrifugal rotational speed is 4000 revs/min, gets upper solution;
(4) macroporous adsorbent resin pre-treatment: X-5 macroporous adsorbent resin is placed in clean brown bottle, add the alcohol immersion 24 hours that volume fraction is 95%, outwell upper strata suspended substance, and activated resin, carry out degassed by vacuum outgas method to resin simultaneously, then adopting wet method dress post, is the ethanol-eluting resin column of 95% with triploid integration number, adds the not muddy and elutriant uv scan of isopyknic distilled water can't check absorption peak to washings in test tube; Be washed with distilled water to without ethanol taste again, effluent liquid is neutral, saves backup;
(5) polymeric adsorbent separation, enrichment: the upper solution that step (3) obtains is entered X-5 macroporous adsorptive resins with the adsorption flow rate of 2BV/h, when the absorbancy of effluent liquid is substantially equal with the absorbancy of pigment, be that eluent is to colourless with the aqueous solution of mass concentration to be 0.2%HCl-mass concentration be 40% ethanol, elution flow rate is 2BV/h, enrichment elutriant;
(6) elutriant dialysis: the elutriant that step (5) obtains is inserted the dialysis tubing that molecular weight cut-off is 3500, and extraneous solution is deionized water, changes once extraneous solution every 5 hours, and dialysis time is 13 hours, after dialysis terminates, obtains dialyzate A;
(7) dialyzate concentrated spray is dry: the NaCl adding the 1-1.5% of dialyzate A gross weight in the dialyzate A that step (6) obtains, and the KCl of dialyzate A gross weight 0.5-1%, obtains dialyzate B; By dialyzate B concentrating under reduced pressure, after rotary evaporation, carry out spraying dry 5-10min, obtain powder-type and medicinal extract type two kinds of pigment products, by pigment product cooling storage.
3. Hylocereus undatus pulp according to claim 1, pericarp red pigments extracting method, it is characterized in that: the ultrasonic extraction described in step (2), extraction time is 90-120min, and Extracting temperature is 45-50 DEG C.
4. Hylocereus undatus pulp according to claim 1, pericarp red pigments extracting method, is characterized in that:
Degumming process described in step (3), upper strata extracting solution temperature when coming unstuck is 48-52 DEG C, and usually time is 60-80min.
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| CN107254387A (en) * | 2017-08-11 | 2017-10-17 | 合肥润雨农业科技有限公司 | A kind of production method rich in glutathione cherry wine |
| CN107821924A (en) * | 2017-11-14 | 2018-03-23 | 蚌埠市涂山村富民石榴专业合作社 | A kind of extraction process of garnet pigment |
| CN108760422A (en) * | 2018-05-19 | 2018-11-06 | 北京逸智联科技有限公司 | A kind of pesticide residue determination method |
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| CN112142695A (en) * | 2020-09-10 | 2020-12-29 | 万华化学集团股份有限公司 | Red-heart pitaya pulp extract and extraction method thereof |
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| CN108760422B (en) * | 2018-05-19 | 2020-09-22 | 山东宁科医疗器械有限公司 | Pesticide residue detection method |
| CN109007547A (en) * | 2018-07-18 | 2018-12-18 | 广东海洋大学 | A kind of dragon fruit pericarp natural pigment preparation method |
| CN109518486A (en) * | 2018-11-30 | 2019-03-26 | 镇宁自治县蚩尤布依民族服饰有限责任公司 | A kind of preparation method and applications using dragon fruit natural dye preparation batik cream |
| CN110903675A (en) * | 2019-07-26 | 2020-03-24 | 湖南农业大学 | Method for extracting red-pulp pitaya pigment under assistance of cellulase and ultrasonic wave |
| CN110903675B (en) * | 2019-07-26 | 2022-04-26 | 湖南农业大学 | Method for extracting red-pulp pitaya pigment under assistance of cellulase and ultrasonic wave |
| CN112142695A (en) * | 2020-09-10 | 2020-12-29 | 万华化学集团股份有限公司 | Red-heart pitaya pulp extract and extraction method thereof |
| CN115572493A (en) * | 2022-09-23 | 2023-01-06 | 廊坊师范学院 | Method for preparing natural plant toner from fruit and vegetable raw materials |
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