CN1205690A - Natural carotenoid concentrates from plant material and process for preparing same - Google Patents
Natural carotenoid concentrates from plant material and process for preparing same Download PDFInfo
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- CN1205690A CN1205690A CN 96199330 CN96199330A CN1205690A CN 1205690 A CN1205690 A CN 1205690A CN 96199330 CN96199330 CN 96199330 CN 96199330 A CN96199330 A CN 96199330A CN 1205690 A CN1205690 A CN 1205690A
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Abstract
Chromoplasts and/or chloroplasts are isolated from plant material. This wet mass is digested in aqueous medium with pectin- and/or protein-cleaving enzymes, insoluble substances are removed, and a carotinoid-rich sediment is obtained after acidifying the separated colloid disperse system. The sediment is heated at alkaline pH with aqueous ethanol or isopropyl alcohol to remove the major part of cleaved proteins, lipides and other accompanying substances. The sediment with enriched carotenoid content is mixed with antioxidants and, if desired, dried, providing a carotenoid concentrate free of toxic solvent residues.
Description
Invention field
The present invention relates to carotenoid concentrates that the chromoplastid that separates by vegetable material by processing and chloroplast(id) obtain and preparation method thereof.
Background of invention
Here said carotenoid is the additional mixture of the fat of a class unsaturated hydrocarbons and they, i.e. isopentene fat, and unsaturated hydrocarbons contains isoprene unit or their derivative that replaced by various functional groups.
As everyone knows, Jian Kang diet comprises the consumption of an amount of high-quality vegetables and fruit.Compare with the heterogeneity of these foods, carotenoid is the essential composition of keeping body health.Carotenoid is efficient antioxidants as Lyeopene, can catch the harmful free free radical that constantly produces in the human body.In addition, some carotenoid also have vitaminogenic function.
Except vitaminogenic function, the main task of carotenoid is to make the human body internal cause such as smog, the uv-radiation of increase, increasing environmental hazard such as atmospheric pollution and a large amount of free free radical inactivations that form.But, even best diet can not provide the supply of sufficient successive carotenoid, according to different scientists' data, grownup's every day, required carotenoid was supplied as 6-15mg, therefore provided carotenoid compositions to become more urgent as the demand that diet replenishes.
Epidemiology survey and other testing data confirm, the sickness rate and the mortality ratio that cause because of various cancers in high area of vegetables and fruit consumption and crowd are low.Data show that this diet provides competent carotenoid supply, and this prompting carotenoid perhaps has prevention effects aspect healthy keeping.
Since provide quite difficulty of successive carotenoid supply by diet, even not possible sometimes, thus need replenish diet with the carotenoid compositions of various sources preparation, and guarantee required carotenoid supply in this way.
What be worth emphasizing is that it is the prerequisite of best effect that successive carotenoid is taken in.Free free radical constantly produces in organism so they also must constantly be detoxified.The antioxidant of enough levels is finished in this reliable body, carotenoid is not unique compound with antioxidation property, tocopherol also is an antioxidant, but carotenoid is indispensable, with tocopherol they in addition can bring into play synergistic activity.
In a word, carotenoid should constantly exist in human body and proper level is arranged in blood plasma, prophylactically to protect organism, avoids the exception procedure that is caused by free free radical.Because this effect is preventative, the diet arrangement will correspondingly design, and promptly adds carotenoid in the diet and will make a practice of.
Consider above several aspect, as the successive foodstuff additive, therapeutic maybe may be that the carotenoid compositions of medicine (as vitamin preparation) should satisfy following requirement:
A) scope of carotenoid should with human plasma in similar, according to data in literature, this scope is as follows:
Alpha-carotene 0.12-0.05 μ mol/l,
β-Hu Luobusu 0.40-0.80 μ mol/l,
Xenthophylls (lutein+zeaxanthin) 0.28-0.35 μ mol/l,
Lyeopene 0.49-0.74 μ mol/l;
B) starting material that are used to prepare said composition can not cause any toxicity injury, promptly can not cause any nutrient health problem;
C) because said composition will constantly be used as therapeutical agent, the design of its production method must be guaranteed the finished product nontoxicity pollutent (such as residual solvent).
D) said composition must contain enough high-load activeconstituents, thus avoid making in a large number with medicament or food additive [correspondingly, a) in indicated carotenoid concentration should increase at least 10 to 100 times.Therefore our target is that to prepare concentration from carotene carotene content is the Radix Dauci Sativae of 100-200mg/kg be 50,000-100, the product of 000m/kg].
Based on the consideration of Bioavailability of Carotenoids, in order to satisfy the demand of carotenoid 10-15mg/kg every day, a grownup must consume about 1 every day to 2kg Radix Dauci Sativae and tomato.Nature can cause bad diet side effect like this, consumes palatability difference and unbalanced complicated diet as the excess carbon hydrate.In addition, except aforementioned aspect, from competent vegetables and fruit supply, obtain satisfied carotenoid levels and be subjected to geographic restriction, even be subjected to the restriction of financial resources under the more susceptible condition.
Comprehensive above-mentioned aspect produces and uses a kind of suitable carotenoid compositions to have tangible benefit.
Although if consider fresh, the content of carotene reaches 150-200mg/kg in the Radix Dauci Sativae that does not have to cook, but it is quite low to make in (processing or culinary art) food carotene carotene content: 7.5-8.1mg α-and β-Hu Luobusu/100g[M.S.Micozzi etc., J Nat.Cancer.Inst.82,282-285 (1990); With Heinonen etc., J.Agric.Food Chem.37,655-659 (1989)], the advantage of carotene compositions is more outstanding.This new goods can be avoided a large amount of losses of carotene, and have higher absorption and bioavailability.
Prior art
The characteristics of existing products and production method thereof have significantly different with product of the present invention and method.
United States Patent (USP) 3,206, the 316 disclosed water-soluble compositions that maybe can be scattered in the water are by the preparation of synthetic carotenoid most probably, then do not use the chlorinated solvents of using in this method in the method for the invention.
WO 86/04059 mentions a method, wherein smashs and squeezes Radix Dauci Sativae machinery to pieces gained juice and handle with pectin degrading enzyme, and ultrafiltration and concentration.Residue is used with wet enriched material or dried forms, chromoplastid is not further purified, thereby concentration is 500-600mg carotene/100g product in the finished product, and according in the product of the present invention, carotene carotene content exceeds 10-20 doubly, be 2500-5000-10,000mg carotene/100g product.
WO 92/18471 mentions from natural matter, especially in the Radix Dauci Sativae, extracts carotenoid, thereby obtains in fact and WO 86/04059 described identical product.In the chromoplastid that is precipitated out as subsidiary material with calcium chloride (obtaining as the finished product), concentration of carotene equals the 12.44mg/g dry-matter, and the method according to this invention can make concentration increase by ten times.
United States Patent (USP) 2.412,707 mentions that a kind of starting material that wet by the cooking (heating) in edible (culinary art) oil obtain oily emulsion.Be that its product or method all can not be compared with method with product of the present invention.
United States Patent (USP) 2,412,707 disclose a kind of method, and wherein the plant chromoplastid is separated from aq suspension, and then is precipitated out by aggegation.Chromoplastid does not have purifying, does not handle yet, and does not attempt to increase concentration of carotene yet.
Ind.Eng.Chem., 46,2279 (1954) mention a kind of extracting method of complexity, wherein utilize all kinds of SOLVENTS that carotenoid is optionally separated from starting material.Used unfavorable solvent in this method, as hexane, heptane, acetone etc.Opposite with our purification process, be not that activeconstituents leaches from chromoplastid in this method, but other composition together is removed.
Also have a kind of method, wherein carotenoid is separated from plam oil, and carotenoid is dissolved in the plam oil here.Heating (boiling) plam oil is used hexane extraction carotenoid subsequently under alkaline condition.
Hungarian patent application P 93 03605 mentions a kind of method, chromoplastid part is being flocculated in the pressed liquor of the Radix Dauci Sativae of mechanical workout (smash to pieces, squeeze), most of then albumen protease digestion forms the precipitation that contains carotenoid when pH3.5-4.5, make it dry.
Summary of the invention
The composition of finding to have advantageous feature in experimentation can be by refining, promptly concentrated from vegetable material the carotenoid in isolated chromoplastid and the chloroplast(id) prepare.
This method is based on such observation: carotenoid in the chromoplastid and lipoprotein in conjunction with or and various lipids form the adduction body, form the particle in the colloid scope.If remove these lipids or a part wherein with lipophilic solvent, thereby destroy lipoprotein/lipid system, then need not of non-ideal use or high toxicity solvent (ethane or chlorinated hydrocarbon), carotenoid concentration just can improve several times in the resistates, this residual kind solvent, even trace, also has high toxicity, because they and carotenoid (because they have the lipotropy similar with carotene) permanent consumption together, thereby cause moving about target cell and tissue, also can't remove in the there accumulation, thereby cause huge injury.
Do not resemble United States Patent (USP) 3,206,316 method, method of the present invention is not used chlorinated solvent, does not use aproticapolar solvent, as hexane yet.
Detailed Description Of The Invention
The present invention relates to a kind of product with the chromoplastid/lipoprotein complex body that is enriched to various types of concentration of carotene, it has following character:
A) with respect to starting material, carotenoid concentration increases 400-500 doubly, and with respect to the chromoplastid first lees, carotenoid concentration improves 2-15 doubly.
B) by protein/lipid composition in the cracking lipoprotein complex body, and by removing polypeptide by the dissolving of carotenoid side chain, the salt of amino acid and lipid acid increases concentration.
C) come the cracking mixture by the solvability of considering degraded product, degraded product is at water/alcohol (ethanol, refining alcohol, Virahol) solubleness in the mixture is than high several magnitude in the ethanol, and the toxic solvents in the finished product is residual so can not be higher than alcoholic acid LD
50
D) can satisfy general requirement in the best way by the carotenoid scope of handling the product that isolating chromoplastid obtains from the starting material of suitable selection such as Radix Dauci Sativae or tomato, as be similar to the carotenoid scope in the human plasma.
The invention still further relates to a kind of preparation and possess the method for the product of above-mentioned character, this method comprises by currently known methods separates the chromoplastid that contains carotenoid, preferably from Radix Dauci Sativae and tomato, separate, by sedimentation or centrifugation, then by enzymically treat chromoplastid part cracking lipoprotein.After material is followed in removal, the liquid phase of acidifying gained, thus precipitate partially purified carotenoid crude extract, in this throw out, add basic solution, with the alcohol reflux of fresh aqueous several times, the basic salt of the peptide that is discharged when removing the cracking mixture, amino acid, lipid acid etc.Add SODIUM PHOSPHATE, MONOBASIC and the slight acidifying carotenoid concentrates of citric acid suspension, sedimentation or centrifugal product and antioxidant mix, and after this, if necessary, carry out drying.
Enzymatic lysis finish preferred adding dry weight 3-5 water doubly, make the chromoplastid and/or the homogenate of chloroplast(id) part that obtain by vegetable material, the pH value of homogenate is adjusted to about 8.5 with sodium hydroxide, then with proteolytic degradation enzyme (preferably also having some lipase activity), in 37-38 ℃ of enzymatic digestion mixture 2-3 hour, with repeatedly add sodium hydroxide solution adjustment pH is original level constantly simultaneously as zymine.Behind the enzymolysis, mixture is centrifugal through 1200g, isolates brown gelatinous precipitate.Liquid phase or " supernatant " or " enriched material " are adjusted pH then to 3.5-4.0, preferably with the acid of approving in the foodstuffs industry.Preferably use 3000g centrifugation material.
Further refining (the purifying of carotenoid part, concentrate) as follows: the precipitation that the acidifying mixture behind the centrifugal enzymolysis obtains was suspended in 60: 40 to 80: 20, preferred 70: in the ethanol-water mixture of 30v/v, add 35g sodium hydroxide (calculating) according to the 1kg dry-matter, sodium hydroxide preferably adds with the 10-35% in water or the said mixture (w/w) solution, and mixture refluxed 2 hours.Infusible precipitate is centrifugal, and the sodium hydroxide solution that adds same amount repeats this process.
70: 30 ethanol-water mixtures of 8 times of volumes are used in preferred alkaline purification for the first time, and 80: 20 ethanol-water mixtures of 5 times of volumes are used in alkaline purification for the second time.
Refluxed in 2 hours for the second time centrifugal repeat to finish after, precipitation is suspended in the solvent mixture (not adding alkali) of 4 times of volumes again, refluxes for the third time, half hour before finishing to reflux,, adding contains 30g SODIUM PHOSPHATE, MONOBASIC (NaH
2PO
4) and the solution of 200g citric acid (for the 1kg dry-matter).This solution by with above used identical ethanol-water solution [i.e. (80: 20)] in the dissolving said compound prepare.
Through after centrifugal, obtain the 45-50% of original dry-matter usually, rest part removes as the sodium salt drip washing of peptide, amino acid, lipid acid etc., and the loss of carotenoid is very little, and it is lost in the assurance skill that depends on to a great extent in the sepn process.
Through behind the aforesaid operations, the carotene carotene content of chromoplastid part is 2 times of starting materials or even higher.
By this method, the processing carotene carotene content is the fresh carrot of 150mg/kg, after finishing the chromoplastid precipitation operation, obtains containing the dry-matter of carotene 7.5-8.5%.
Repeat alkaline purification, concentration of carotene can further be increased to more than the 10-15%, and some method can also obtain greater concn, but because higher solvent, energy and manpower requirement have some problems economically, even can loss carotenoid in these sepn processes.
After repeating alkaline purification, calculate according to the dry-matter that separates the back gained, add 80: 20 v/v ethanol-water solutions of 6 times of amounts, mixture under agitation refluxed 2 hours.
Adding an amount of SODIUM PHOSPHATE, MONOBASIC and citric acid then in stirred mixture, adjust pH to 7.0-7.2, promptly approximately is neutral range.
The material of centrifugal gained mixes (kneading) with tocopherol and Quicifal, is being no more than under 60 ℃ the temperature dryly with ethanol wetted form, but wet form also can be used.
The dry powder of sieving is carried out vacuum packaging.
Can similarly handle from the chloroplast(id) that photosynthetic plant materials obtains.Yet in this case, if this product design is used for the human consumption, chlorophyllous degraded product should remove very carefully as phoeophytin and pheophorbide.
The conspicuous innovative point of method of the present invention is:
---by the mechanical workout that part is carried out chromoplastid and chloroplast(id) cellular constituent are transferred to liquid phase (pressed liquor, decantation parting liquid) in alkaline medium.
---the chromoplastid in liquid phase or in suspension makes its sex change by adjusting pH value or heating or being used in combination these two kinds of means, causes them to be precipitated out from liquid phase.
---the floss (decantation separates) of precipitation separation, remove water soluble component, with respect to starting material, the concentration of carotenoid obviously increases in the isolating floss.
---chromoplastid and chloroplast(id) contain coloring matter, comprise carotenoid, they are to have the very lipid-protein complex of high lipid content, lipid-protein complex in colloidal solution association class carotene (these carotenoid are in fact water insoluble, even and in organic solvent also indissoluble extremely), and in organism these pigments of transportation.The part lipid of mixture is retained in the product, and improves Bioavailability of Carotenoids.
New thinking is for being that carotenoid should remove from follow material, but follows material to remove from carotenoid as much as possible.This realizes by the following method: cracking lipid-protein complex in alkaline medium, and transfer in aqueous ethanol solution with its sodium-salt form most of lipid and remove them.
By selecting suitable starting material, by the thick enriched material of they preparation carotenoid, mix then, may obtain the product that the carotenoid scope satisfies the needs of human body and is similar to the carotenoid scope in the human plasma.
Can be by avoiding using noxious solvent to reach above-mentioned advantage, these noxious solvents are generally used for dissolving carotenoid.Consequently the byproduct of this method and the refuse that wherein produces are free from environmental pollution, are biodegradable, in most of the cases can be used as food or fodder additives.
Following embodiment describes the said products and preparation method thereof in detail, rather than limits the scope of the invention.If not explanation in addition, % value representation w/w.
Carry out the analysis of carotenoid according to following method:
A) the Booth spectrophotometry [M.A.vander Meer et a1. (Wageningen), Z.Lebensmittel Untersuch.und Forschung.185.461-467 (1987)] of improvement is adopted in the analysis of β-Hu Luobusu.
B) scope of carotenoid is measured and is adopted high performance liquid chromatography (HPLC) at Waters600 multi-solvent transfer system (Waters.Milford, USA) finish on, adopt anti-phase LiChrosorbRP-18 (10 μ m, 250 * 4.6mm) and Spherisorb ODS (5 μ m, 250 * 4.6mm) pillars, (75: 15: 10v/v) mixture was as eluent for acetonitrile-methyl alcohol-tetrahydrofuran (THF), photodiode sensor (Photo Diode Array Detector 990 (DAD), Waters, Milford is USA) as the detector of wavelength region 190-800nm.The purifying reference material is as interior mark.
Embodiment
Preparation contains the enriched material of 5% carotenoid from Radix Dauci Sativae (Daucus carota).
1000kg defoliation Radix Dauci Sativae (the Radix Dauci Sativae body of carotenoid content 180-200mg/kg) adopts methods known in the art to handle according to flow process shown in Figure 1.The clean Radix Dauci Sativae body of rinsing is through milling, and squeezing is milled a blob of slag once more, add water homogenate and squeezing repeatedly, through milling repeatedly, the fiber cake of squeezing carries out the extraction of the 3rd step with the sodium hydroxide solution of pH8.5 then, and the pen type whizzer separates residue and extracting solution (decantation concentrated solution) by inclining.Merge pressed liquor and decantation concentrated solution, adjust amalgamation liquid pH to 4.0 with 10% citric acid.Chromoplastid is cotton-shaped cohesion, places to make it sedimentation.
The 220 liters of precipitations that can cross pump, after decantation separates, adjust pH to 8.5 with 10% sodium hydroxide solution, in 37 ℃ of vigorous stirring processes, add 10 liters of aqeous suspension digesting proteins that contain the 100g pancreatin, and constantly proofread and correct the pH value that descends with 10% sodium hydroxide solution.Handled lasting 3 hours, with the undissolved particle that does not belong to colloidal solution in the centrifugal removal mixture of pen type whizzer (pH8.5) that inclines.Through inclining the pen type whizzer separately, being deposited in of obtaining is in the past dry and edible partially mixed.
The decantation concentrated solution also comprises carotenoid, makes pH to 4.0 with 10% citric acid acidifying, and sedimentary throw out is separated.
Drift separately contains the dry-matter of 16-18%, wherein contain 2.5% carotenoid (calculating) according to dry-matter, its weight in wet base is 45-50kg, mix with 90 liters of 80: 20 (v/v) ethanol-water mixtures, add 3 liter of 10% sodium hydroxide solution then, mixture refluxed 2 hours under vigorous stirring.
The mixture of heat is through separating, and isolated precipitation (weight in wet base 28-30kg) adds 50 liters of aqueous ethanols (80: 20) and 2 liter of 10% sodium hydroxide solution repeats alkaline purification, and mixture refluxed 2 hours then.Repeat this step sepn process and obtain the 16-20kg moist precipitate.
Moist precipitate refluxed 1 hour for 40 liters with above used aqueous ethanol earlier, added 10% citric acid and 3: 1 blended aqueous solution of SODIUM PHOSPHATE, MONOBASIC in this process, made its pH be substantially to neutrality (7.0-7.2).This approximately needs 300g citric acid and 100g SODIUM PHOSPHATE, MONOBASIC.
After separating, obtain the 14-16kg precipitation, amount to dry-matter 3.2kg, wherein contain 0.19kg carotenoid.
Add 150-300g antioxidant blends (alpha-tocopherol acetate, alpha-tocopherol and Quicifal were by 2: 2: 1w/w mixes) in precipitation.Mixture thorough mixing (kneading) is being no more than vacuum-drying under 50 ℃ the temperature.
Exsiccant the finished product index:
Solid substance 3.4kg
Carotenoid content 5.5%
Drying loss maximum 5% (105 ℃, 3 hours)
The color reddish-brown
Carotenoid scope 60-65% β-Hu Luobusu
The 28-30% alpha-carotene
Other carotenoid of 5-10%
Under vacuum condition or in shielding gas, stablized at least 1 year.
Preparation contains the enriched material of 7-8% carotenoid
Application Example 1 the operation described process, but adopt the Radix Dauci Sativae that contains carotenoid 220-250mg/kg as starting material, bacterium (Bacillus subtillis) proteolytic enzyme is adopted in proteinic digestion.
The finished product: 3kg reddish-brown dried powder or particle, carotenoid content 7.5-8.0% has the carotenoid scope similar with product among the embodiment 1.
Preparation contains the enriched material of 10% carotenoid approximately
Handle with the starting material among the embodiment 2.On the basis of two step alkaline purifications, the solvent and the alkali of utilization and the equivalent of alkaline purification are for the second time handled for the third time.Then, according to embodiment 1, moist precipitate refluxed 1 hour with 40 liters of 80: 20 ethanol-water mixtures, pressed embodiment 1 again with the neutralization of gained mixture, isolated precipitation, mixed antioxidant blends, vacuum-drying.
Finished product: 1.6kg reddish-brown dryed product
Drying loss maximum 6%
Carotenoid minimum content 10.5% (0.17kg)
A same embodiment of carotenoid scope.
The enriched material of Lyeopene is rich in preparation from Radix Dauci Sativae and tomato
The chromoplastid that contains carotenoid is separated from Radix Dauci Sativae and tomato respectively, then the material of collecting is handled (making with extra care).
500kg being cleaned the Radix Dauci Sativae (the Radix Dauci Sativae body of carotenoid content 220mg/kg) of defoliation handles.Obtain juice according to flow process shown in Figure 1.Make the chromoplastid sedimentation of the flocculation that (10% citric acid solution) obtains when pH4.0, separate by decantation.The rare drift that approximately contains 8% dry-matter concentrates in separator, obtains the precipitation that dry matter content is 16-20%.Be directly used in alkaline purification without protein degradation.Every 20-25kg moist precipitate adds 3 times of amounts (approximately 75kg) ethanol-water mixture (80: 20) and 1.5 liter of 10% sodium hydroxide solution, and mixture refluxed 2 hours, the mixture of heat of dissociation, re-treatment precipitation then.After twice alkaline purification, by separate or the centrifugal precipitation that obtains by the method for embodiment 1, through aqueous ethanol rinsing and neutralization.The precipitation that the separation in two hours that refluxes obtains is first kind of composition of the finished product.
Individual curing 1000kg tomato.The juice that leaches by currently known methods contains 7% dry-matter, obtains enriched material after concentrating, and contains dry-matter 20%.Enriched material Ethanol Treatment 3 times.At first use the ethanol (about 500 liters) of 2 times of bulk purity 96% to reflux two hours, separate the ethanol phase then, with aqueous ethanol (80: 20) re-treatment 2 times.When handling for the third time, add 3 liter of 10% sodium hydroxide solution in the backflow mixture that stirs.Handle residue obtainedly for the third time, mainly, before drying, join in the edible composition by pectin, polysaccharide and fibrous.Collect alcohol extractive, adjust the pH value to 7.0-7.5 by embodiment 1 described method with citric acid/SODIUM PHOSPHATE, MONOBASIC mixture, distillating mixture.Reclaim ethanol, obtain 10 liters of enriched materials, its moist precipitate as second kind of composition and processing Radix Dauci Sativae gained is mixed, mix vacuum-drying with 5% antioxidant again.
The finished product: 3.6kg reddish-brown dry-matter
Drying loss: maximum 5%
Carotenoid content: minimum 5.5%
Carotenoid scope: Lyeopene 1.8%
β-Hu Luobusu 2.0%
Alpha-carotene 1.2%
Xenthophylls+other is 0.5% years old
This product characteristics is to contain high-load Lyeopene.
Embodiment 5
The product of preparation high hycopene content
Radix Dauci Sativae is pressed embodiment 4 described methods and handles.
Handle the 3000kg tomato, the pectin of tomato juice is used by methods known in the art and is digested with polygalacturonase when the pH4.0, and polygalacturonase separates from the Aspergillus culture.The fruit juice of pectin digestion back dilution is through vacuum concentration, and dry matter content from 7% to 30% obtains the 540kg enriched material, uses Ethanol Treatment again.Handle ethanol for the first time, 80: 20 ethanol-water mixtures of ensuing twice usefulness with 3 times of bulk purity 96%.Each Ethanol Treatment all refluxed 2 hours.In Ethanol Treatment process for the third time, add 8 liter of 10% sodium hydroxide solution to the reflux solution that stirs.In the Ethanol Treatment process, ethanolic soln and insoluble part are separately.(through after the Ethanol Treatment for the third time, from the no lycopene material that obtains, remove ethanol, join in the edible composition after the drying).
The finished product: 6.2kg reddish-brown dry-matter
Drying loss maximum 5%
Carotenoid content minimum 5.5%
Carotenoid scope: Lyeopene 3.0%
β-Hu Luobusu 1.2%
Alpha-carotene 0.6%
Other carotenoid 0.7%
The feature of this product is the Lyeopene with similar content: carotene
Embodiment 6
From Radix Dauci Sativae and sprouting broccoli h, concentrate carotenoid
By flow processing 1000kg Radix Dauci Sativae shown in Figure 1 and 1000kg sprouting broccoli, preparation juice.
Juice is heated to 56 ℃, transfers pH to 4.0 with 10% lemon acid solution, solution is cooled to 20-25 ℃ then, makes sedimentary chromoplastid and the further sedimentation of chloroplast(id) throw out.
Concentrating and precipitating in separator obtains dry matter content and is 20% moist precipitate.Every 22kg dry-matter (approximately 90kg moist precipitate) adds 180 liters of aqueous ethanols (80: 20) under vigorous stirring, add 6 liter of 10% sodium hydroxide solution and regulate pH to 9.5, and mixture refluxed 2 hours.The mixture of heat of dissociation.Repeat this processing 3 times.After each the processing, the volume of sodium hydroxide solution and solvent reduces pro rata according to dry matter content.Tentative consumption (being on dry matter basis): 8-10 times of volume aqueous ethanol (80: 20) and 2.25-3.5% sodium hydroxide.
The residue of the 4th alkaline purification is suspended in 45 liters of aqueous ethanols (70: 30), presses embodiment 1 and refluxes and neutralization.Obtain 4.1kg precipitation and 5% antioxidant blends after the separation and mix, be no more than vacuum-drying under 50 ℃ of temperature.The product that obtains after the drying contains the dihydroxy carotenoid (xenthophylls, zeaxanthin) of suitable content.
The finished product: green brown dry-matter
Drying loss maximum 5%
Carotenoid content minimum 6.5%
Carotenoid scope: β-Hu Luobusu 3.2%
Alpha-carotene 1.5%
Xenthophylls+zeaxanthin 1.0%
Lyeopene 0.4%
Other carotenoid 0.4%
Similar carotenoid concentrates in preparation carotenoid scope and the blood plasma
Product among the embodiment 4,5 and 6 mixes with the ratio and the antioxidant of ethanol wetted form in 1: 2: 1, stirs evenly the vacuum-drying mixture.
The finished product: green brown dry-matter
Drying loss maximum 5%
Carotenoid content minimum 6.2%
Carotenoid scope: Lyeopene 32.9%
β-Hu Luobusu 30.5%
Alpha-carotene 21.7%
Xenthophylls+zeaxanthin 11.6%
Other carotenoid 3.3%
Lyeopene in the product and dihydroxy carotenoid (xenthophylls and zeaxanthin) content and required blood plasma level are in full accord.This product not only guarantees to supply the α that makes the people satisfied-and β-Hu Luobusu, and contains the Lyeopene and the dihydroxy carotenoid of strong anti-oxidation characteristic, the advantage of having given prominence to product more.
Similar carotenoid concentrates in preparation carotenoid scope and the blood plasma
Embodiment 9
Handle Dunaliella or Blakeslea spp.
Obtaining Dunaliella or Blakeslea spp. biomass from natural resources or fermenting culture, is 8-10% by sedimentation or the centrifugal dry matter content that is concentrated to.The carotenoid dry matter content accounts for 2% in the enriched material.Make these materials be heated to 100 ℃ by feeding 3 crust saturation steams, feed steam continuously and kept this temperature 10 minutes, until this stacking yard matter plasmolysis.
Amount by the dry-matter 5% that is dissolved in 20 times of volume Virahol-water (70: 30 v/v) mixture adds sodium hydroxide adjustment plasmolysis thing pH to 11, and mixture refluxed 2 hours under whipped state, the mixture of heat of dissociation, separately precipitation and liquid phase.
Add 2 times of volume Virahol-water (80: 20) mixtures and 0.08 times of volume 10% sodium hydroxide solution in moist precipitate, mixture refluxed 2 hours, repeated above-mentioned sepn process.
This processing repeats twice again.
After handling through the 4th time, adds 2 times of volume isopropanol-water mixtures (80: 20) in moist precipitate, refluxed 1 hour, the drift of neutralization heat is pressed the method filtration of embodiment 1 description or centrifugal.
Through neutralizing and separating filter residue cake or the centrifugation that obtains, press embodiment 1 described and antioxidant mixing, last vacuum-drying.
Exsiccant reddish-brown product has following character:
Dry matter content 94-96%
Crude protein (N * 6.25) 18-22%
Robust fibre 5-6%
Sulfate ash 20-25%
Non-albumen submember 8-10%
Lipid *) 32-46%
Carotenoid content 20-25% wherein
*) lipid sample material is dissolved in chloroform and carbinol mixture (nonsaponifiable lipid part).
The carotenoid scope depends on environmental factors such as starting culture or fermentation condition in the product, but carotenoid content is no less than ten times of carotenoid dry matter content in the initial plasmolysis thing in the product, i.e. ten times of enrichments at least.
Claims (9)
1. from chromoplastid and/or chloroplast(id), separate the natural carotenoid concentrates that obtains, it is characterized in that:
A) it contains 1.5-25% (w/w) natural carotenoid and other composition that obtains from handled plant and the antioxidant that can choose interpolation wantonly;
B) it does not contain Toxic matter, especially poisonous residual solvent; And
C) its carotenoid scope can be regulated arbitrarily as required.
2. the enriched material of claim 1 is characterized in that, contains in its carotenoid content:
The 10-30% alpha-carotene
The 22-65% β-Hu Luobusu
The 6-55% Lyeopene and
5-22% dihydroxycarotene (xenthophylls, zeaxanthin) and other carotenoid; And
1.8-3.4% (w/w) alpha-tocopherol acetate,
1.8-3.4% (w/w) alpha-tocopherol and
0.9-1.7% (w/w) Quicifal
(calculating according to dry-matter) is as antioxidant.
3. preparation does not contain the method for the natural carotenoid concentrates of poisonous residual solvent, it is characterized in that:
I) chloroplast(id) of separating from vegetable material and/or chromoplastid part are handled with the enzyme with pectin and/or protein degradation characteristic (also lipase activity can be arranged) in water-bearing media, after digestion is finished, insoluble substance and colloid disperse phase are separated;
But acid is used in ii) colloid disperse phase optionally heating or cooling then, and preferably with the acid of foodstuffs industry approval, acidifying mixture precipitates carotenoid, by isolating precipitation in the liquid phase;
The solid precipitation that iii) contains carotenoid heats in aqueous alcohol under alkaline pH, thereby other submember of filtering degraded product and plant origin after the neutralization, goes out carotenoid by settlement separate; With
Iv) contain precipitation and specified quantitative alpha-tocopherol and/or the VITAMIN E ACETATE and/or the Quicifal mixing of carotenoid; If desired, drying composite; With
If desired, several dryed products with inhomogeneity carotene scope mix with specified proportion; Or
If desired, several dryed products with inhomogeneity carotene scope mix, and add alpha-tocopherol and/or the VITAMIN E ACETATE and/or the Quicifal mixing of specified quantitative then, if desired, and drying composite.
4. the method for claim 3, it is characterized in that, step I) chromoplastid and/or chloroplast(id) partly use the proteolytic enzyme or the animal protease (zymine) in bacterium (as Bacillus subtillis), fungi (as aspergillus oryzae), plant (papoid) source to handle in, handling pH is 4.5 to 11, treatment temp is 28 ℃ to 60 ℃, and the treatment time is 30 to 180 minutes.
5. claim 3 or 4 each methods is characterized in that, at step I i) in add C
2-4Aliphatic carboxylic acid, single-or dihydroxy-two-or tricarboxylic acid, the salt that the oxyhydroxide of phosphoric acid or they and basic metal or alkaline-earth metal and/or basic metal and/or alkaline-earth metal forms, in 8.5 scopes, regulate the iso-electric point of pH value at pH3.0, thereby carotenoid is precipitated out to chromoplastid and/or chloroplast(id).
6. the method for claim 3 is characterized in that, at step I i) in regulate after the pH value, but the mixture optionally heating to be not higher than+60 ℃ or choose wantonly be cooled to be not less than+5 ℃.
7. the method for claim 3 is characterized in that, step I ii) in aqueous pure processing can choose wantonly and repeat several times.
8. the method for claim 3 is characterized in that, step I ii) in used water/ethanol or water/isopropanol mixture water content be 15-40% (v/v), boiling point is lower than 90 ℃.
9. the method for claim 3 is characterized in that, step I v) gained the mixture frost drying or be lower than 60 ℃ of following vacuum-dryings or with wet form utilization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96199330 CN1205690A (en) | 1995-10-27 | 1996-10-08 | Natural carotenoid concentrates from plant material and process for preparing same |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| HUP9502943 | 1996-08-09 | ||
| CN 96199330 CN1205690A (en) | 1995-10-27 | 1996-10-08 | Natural carotenoid concentrates from plant material and process for preparing same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1205690A true CN1205690A (en) | 1999-01-20 |
Family
ID=5129431
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 96199330 Pending CN1205690A (en) | 1995-10-27 | 1996-10-08 | Natural carotenoid concentrates from plant material and process for preparing same |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1205690A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100432050C (en) * | 2006-11-08 | 2008-11-12 | 江南大学 | Process for preparing corn carotinoid |
| CN103841839A (en) * | 2011-07-15 | 2014-06-04 | 捷通国际有限公司 | Multicarotenoid beadlets and related method |
| CN104974071A (en) * | 2015-06-30 | 2015-10-14 | 华南理工大学 | Preparation method of zeaxanthine |
| CN110198640A (en) * | 2016-11-10 | 2019-09-03 | Gnt集团有限公司 | The orange carrot penetrant of concentration |
-
1996
- 1996-10-08 CN CN 96199330 patent/CN1205690A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100432050C (en) * | 2006-11-08 | 2008-11-12 | 江南大学 | Process for preparing corn carotinoid |
| CN103841839A (en) * | 2011-07-15 | 2014-06-04 | 捷通国际有限公司 | Multicarotenoid beadlets and related method |
| US9265277B2 (en) | 2011-07-15 | 2016-02-23 | Access Business Group International Llc | Multicarotenoid beadlets and related method |
| CN104974071A (en) * | 2015-06-30 | 2015-10-14 | 华南理工大学 | Preparation method of zeaxanthine |
| CN110198640A (en) * | 2016-11-10 | 2019-09-03 | Gnt集团有限公司 | The orange carrot penetrant of concentration |
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