CN102038644A - Lutein water-soluble powder and preparation process thereof - Google Patents
Lutein water-soluble powder and preparation process thereof Download PDFInfo
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- CN102038644A CN102038644A CN2010106019319A CN201010601931A CN102038644A CN 102038644 A CN102038644 A CN 102038644A CN 2010106019319 A CN2010106019319 A CN 2010106019319A CN 201010601931 A CN201010601931 A CN 201010601931A CN 102038644 A CN102038644 A CN 102038644A
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Abstract
The invention relates to a preparation process of a lutein water-solubility powder with good water-solubility, stable properties and good liquidity, which belongs to the technical field of medicines. The lutein water-soluble powder disclosed in the invention comprises the following prescription components in proportion by weight: lutein powder to a carrier to an additive of 1: (1-10):(0-3). The lutein water-solubility powder prepared by adopting a dissolvent way can be prepared into various dissolvent forms or added to various functional foods. In the lutein water-soluble powder prepared by the process, the dissolution rate of lutein can reach 96%. The lutein water-soluble powder has the advantages of good water-solubility, high stability, good liquidity, 34 DEG of angle of repose and good dispersity, and can be applied to various fields such as foods, medicines, cosmetics and the like.
Description
Technical field
The invention belongs to medical technical field, relate to a kind of lutein water-soluble powder and preparation technology thereof, be specifically related to a kind of in water the lutein water-soluble powder and the preparation technology thereof of instant and good stability.
Background technology
Phylloxanthin has another name called " plant progesterone ", exists jointly at occurring in nature and zeaxanthin.Be the key component that constitutes plant pigment such as corn, vegetable, fruit, flowers, be contained in the chloroplast of leaf, the luminous energy that absorbs can be passed to chlorophyll a, infer that photooxidation, photo damage are had protective effect.It also is the main pigment that constitutes human eye retina's macular region.Contained natural carotenol is a kind of antioxidant of excellent performance in the medical experiment proof plant, in food, add a certain amount of phylloxanthin and can prevent cell ageing and biological organs aging, the visual deterioration that also can prevent senile eyeball macula retinae to degenerate simultaneously to cause is with blind, by a series of medical research, phylloxanthin has been proposed as the cancer prevention agent, life prolongs agent, the ulcer inhibitor, the inhibitor of heart attack and coronary artery disease. simultaneously, phylloxanthin also can be used as feed additive and is used for the painted of poultry meat egg, also has been used as painted and nourishing healthy agent simultaneously in food industry.
Phylloxanthin has important protective effect to the macula lutea in the retina, easily draws macular degeneration and blurred vision during shortage.And then symptoms such as visual deterioration, myopia appear.Phylloxanthin is as antioxidant and photoprotection to the major physiological function of eyes.The Oxidation that phylloxanthin is stronger, the activity that can suppress reactive oxygen free radical, stop reactive oxygen free radical to Normocellular destruction. relevant experimental results show that, reactive oxygen free radical can react with DNA, protein, lipid, weaken their physiological function, and then cause such as cancer, arteriosclerosis, increase the generation of the yellow film degeneration of rheological properties disease chronic diseases.Phylloxanthin can pass through physics or chemical cancellation effect deactivation singlet oxygen, thereby the protection body escapes injury the immunocompetence of enhancing body.Cataract is to cause the main ophthalmic of losing one's sight in the world wide, the up-to-date intake by the increase phylloxanthin that studies have shown that can reach the purpose of living rate, think that at present its mechanism is lower macular pigment density and the higher crystalline lens visual density tight association of middle-aged and elderly people, and higher crystalline lens visual density is considered to the obvious characteristic of cataract morbidity.Nearest result of study shows that phylloxanthin has retarding action to early stage arteriosclerosis process.It mainly is the relation between the lutein content in the variation of tremulous pulse major trunk roads tunica intima thickness and the blood.Lutein content is lower in the blood, very easily causes the arteries wall thickening, and along with the increase gradually of lutein content, arterial wall thickens trend to be reduced, and arterial thrombosis also significantly reduces.Simultaneously, the phylloxanthin in the arterial wall cell also can reduce the oxidisability of LDL cholesterol.Multinomial studies show that, phylloxanthin has inhibitory action to multiple cancer, as breast carcinoma, carcinoma of prostate, rectal cancer, skin carcinoma etc. according to the nearest research of medicine institute of New York University, between the sickness rate that reduces breast carcinoma and phylloxanthin intake relation is very closely arranged, investigation finds that the breast cancer incidence of the experimental group that the phylloxanthin intake is low is the high group of intake (2.08～2.21) times.This effect may relate to the indirect immunoregulation effect collaborative with other organ-tissues. and the research is reached a conclusion, and takes the photograph people's phylloxanthin and can not only suppress tumor even can play the effect that prophylaxis of tumours takes place in meals.Retinitis pigmentosa (RP) is a kind of chronic, carrying out property, heritability, dystrophic retinal pigment pathological changes.Mainly comprise primary pigmentary degeneration of the retina, crystallinity retinitis pigmentosa, white point shape retinitis pigmentosa and retinitis pigmentosa sine pigment.Additional phylloxanthin can increase retinal pigment density, improves RP patient's vision, improves the treatment rate of RP.Phylloxanthin, zeaxanthin can significantly improve VAR, recover the balance that the inside and outside osmotic pressure of blood vessel loses, and reduce vascular permeability, have suppressed material seepage in the blood vessel, guarantee the integrity of eyes blood vessel, allow eyes obtain competent blood supply.Can prevent simultaneously that free radical and eyes collagen protein are in conjunction with causing damage, strengthen the retina collagen structure, thereby improve various retinal diseases (as: diabetic retinopathys, the retinitis pigmentation, hemorrhagic and hypertension retinopathy, and macular degeneration etc.) treatment rate improves, recovers the visual loss that therefore causes.
But to be a kind of water insoluble and the material of poor stability for phylloxanthin, its water-insoluble and poor stability have limited its application in every field, a kind of like this use with material of better prevention and therapeutic effect is restricted, therefore how to improve its water solublity and stability, enlarging its scope of application is that those skilled in the art are making great efforts always.
Publication number CN101177540A has described a kind of preparation method of food stage lutein water-soluble dry powder.Earlier with behind the organic solvent dissolutions such as phylloxanthin acetone, ethyl acetate, get mixed liquor after the emulsifying with the aqueous solution of modified starch, glucose, by the emulsifying of high pressure dispersing emulsification machine, remove moisture content in the emulsion with spray drying method or spraying-starch fluid-bed drying at last again, get dry powder.This technology is complicated, and needs the even and spray drying device of high pressure breast.
Publication number CN1757315A has related to Technology, the prescription that a kind of lutein ester is modified as water-soluble lutein.Adopt chemical method and physics method modified technique technology, to the emulsifying of lutein ester heating liquefaction after saponification, then through the degassing of high pressure homogenization final vacuum, last sterilization filling.This technology is carried out saponification, emulsifying then, process complexity earlier.More to the pressure requirement, advanced high pressure homogenization, vacuum outgas then is to the equipment requirements height.
Publication number CN101433528A has described a kind of method for preparing the dispersive Xanthophyll micro-capsule of stabilize water from lutein crystal.Adopt 60-150 ℃ of fusion method of TRANSIENT HIGH TEMPERATURE that lutein crystal is dissolved, add emulsifying base and carry out emulsifying, through high pressure homogenizer with the reactive compound homogenizing, be prepared into nanoscale phylloxanthin solution, adopt the fluidized bed granulation coating, the capsule material by droplet surface adsorption and condensation molding, is sieved packing.This technology is unsuitable for the phylloxanthin crude product to phylloxanthin purity requirement height.Constant-pressure and high-temperature 60-150 ℃ can not guarantee the lutein crystal fusion, and phylloxanthin character instability, may go bad in the heating process.
In a word, operating condition is had relatively high expectations in the preparation method of the lutein water-soluble preparation that above-mentioned these known technologies disclose, and complicated operating process, suitability for industrialized production are difficult.Operating process of the present invention is simple, and is less to equipment requirements, is beneficial to suitability for industrialized production.
Summary of the invention
The lutein water-soluble powder process that the purpose of this invention is to provide the good and stable in properties of a kind of water solublity.
Of the present invention being achieved by the following scheme:
The prescription of lutein water-soluble powder of the present invention is formed and weight ratio is a phylloxanthin: carrier: additives are 1:1-10:0-3.
Wherein said phylloxanthin is the phylloxanthin powder or the lutein crystal of lutein content at least 50%;
Wherein said carrier is:
A. polyvidone be among C15, C30, K-25, K29/32, K90, the K90D any one or they arbitrarily than mixture;
B. Polyethylene Glycol be in polyethylene glycol 1500, Macrogol 2000, Macrogol 3000, Macrogol 4000, polyethylene glycol 6000, the Polyethylene Glycol 8000 any one or they arbitrarily than mixture;
C. any one in mannose, galactose, the cholic acid or they arbitrarily than mixture.
Wherein said additives are:
A. Polysorbate be in polysorbate60, tween 61, polysorbate65, Tween 80, sorbimacrogol oleate100, the polysorbate85 any one or they arbitrarily than mixture;
B. Span be in sorbester p18, sorbester p38, sorbester p17, span 83, the sorbester p37 any one or they arbitrarily than mixture;
C. fatty acid cane sugar ester be among SE12, SE13, SE14, the SE15 any one or they arbitrarily than mixture;
D. a kind of in tocopherol, ascorbic acid, the tert-butyl group hydroxyphenyl methyl ether or they arbitrarily than mixture.
The present invention prepares as follows:
After at least two kinds of mixing in phylloxanthin, carrier material and the additives, add the organic solvent stirring and dissolving, heating-up temperature is 20-50 ℃, and temperature retention time is 5-30 minute, and then at temperature 30-85 ℃, vacuum is evaporate to dryness under the 0-1 MPa condition, pulverizes, promptly.
Whole process of preparation is carried out under the lucifuge condition.
Wherein said solvent is: a kind of in acetone, dehydrated alcohol, 95 ethanol, the ethyl acetate or they arbitrarily than mixture.
The lutein water-soluble powder of the present invention's preparation and the carrier of pharmaceutically accepting mix, and can be made into tablet, capsule, powder or make quick releasing formulation, or the functional food of arbitrary form.
The present invention is easy and simple to handle, good, the stable height of lutein water-soluble powder water solublity and the good fluidity that make, and dissolution rate can reach more than 96%, can be applicable to various dosage forms or joins in the various food with the form of food additive.Also can be made into the medicine or the functional food of arbitrary form.
Advantage of the present invention:
1. the lutein water-soluble powder that makes of the present invention improves its water solublity greatly, changes the dissolubility of phylloxanthin, enlarges the range of application of phylloxanthin.
2. increased the stability of phylloxanthin.Good flowability makes it can be used for tabletting, and is encapsulated, or is added in the various functional food.
3. the lutein water-soluble powder that makes of the present invention can add beverage, and milk product is in the oral liquid.
Description of drawings:
Fig. 1 is a lutein water-soluble powder stripping curve:
The specific embodiment:
Following example helps us further to elaborate the present invention, and should not be interpreted as limiting the scope of the invention.
The absorbency detection method of phylloxanthin is the ultraviolet-visible photometry among the present invention, and blank solution is a purified water, and the detection wavelength is 446nm.
The three therapeutic methods of traditional Chinese medicine (little agar diffusion method) mensuration medicine dissolution in vitro in 2010 editions appendix of Chinese Pharmacopoeia is pressed in the dissolution in vitro test.Medium is 30% alcoholic solution, rotating speed 50rpm, and temperature is 37 ± 0.5 ℃.
Embodiment 1
Get 5g high purity lutein crystal, 5g 30 POVIDONE K 30 BP/USP 90,70,50 milliliters of acetone stirrings of 2.5g tween fully dissolving after 5 minutes, 60 ℃ of evaporates to dryness of normal pressure water-bath.After treating embrittlement, take out and pulverized 80 mesh sieves promptly.
Embodiment 2
Get 10g80% phylloxanthin, 20g Macrogol 2000,10g polysorbate65,60 milliliters of ethyl acetate stir fully dissolving after 10 minutes, 30 ℃ of evaporates to dryness of vacuum 0.7 MPa water-bath.After treating embrittlement, take out and pulverized 80 mesh sieves promptly.
Embodiment 3
Get 15g70% phylloxanthin, 45g 30 POVIDONE K 30 BP/USP 29 and 10g fatty acid cane sugar ester SE15,100 milliliters of dehydrated alcohol stir fully dissolving after 20 minutes, 35 ℃ of evaporates to dryness of vacuum 0.9 MPa water-bath.After treating embrittlement, take out and pulverized 80 mesh sieves promptly
Embodiment 4
Get 20g60% phylloxanthin, 100g 30 POVIDONE K 30 BP/USP 30 and 75,200 milliliter of 95 ethanol of 10g span, stir fully dissolving after 30 minutes, 35 ℃ of evaporates to dryness of vacuum 1 MPa water-bath.After treating embrittlement, take out and pulverized 80 mesh sieves promptly.
Embodiment 5
Get the anti-bad 100 milliliters of ethyl acetate of 15g70% phylloxanthin, 105g Macrogol 4000,5g ten polyglycereol stearates and 9g, stir fully dissolving after 10 minutes, 30 ℃ of evaporates to dryness of vacuum 0.7 MPa water-bath.After treating embrittlement, take out and pulverized 80 mesh sieves promptly.
Embodiment 6
Get 20g60% phylloxanthin, 200g galactose, 5g span 20,5g tween 70 and 150 milliliter of 95 ethanol of 30g α-tocopherol, stir fully dissolving after 25 minutes, 35 ℃ of evaporates to dryness of vacuum 1 MPa water-bath.After treating embrittlement, take out and pulverized 80 mesh sieves promptly.
Solubility test:
Get the lutein water-soluble powder 20g that embodiment 1 makes, adopt the solute mass method to measure its dissolubility.Take by weighing 100g water in the 250ml beaker, add water-soluble lutein 20g, 20 ℃ of water-baths are constantly stirred.The unnecessary powder long period (5min) no longer dissolves, and then obtains the saturated solution of lutein water-soluble powder.By heating evaporation, weighing, obtaining wherein, the solute quality is 11.5g.Calculating dissolubility is 11.5g, wherein contains phylloxanthin 4.6g.Can get the lutein water-soluble powder thus for easily molten, and phylloxanthin is increased to dissolving by insoluble.
S=solute quality (g)/solvent quality (g) * 100g
The dissolution test:
Get the lutein water-soluble powder 100g that embodiment 2 makes, be divided into two parts.A W
1Dissolve fully with the 1000ml simulated gastric fluid, be put in 37 ℃ ± 0.5 ℃ water-bath and leave standstill 30min, sampling filters, and measures its absorbance E value in the 446nm place with ultraviolet spectrophotometer.Another part W
2Add the stirring paddle dissolving with 37 ℃ ± 0.5 ℃ simulated gastric fluid 1000ml,, survey its absorbance E every sampling in 5 minutes
i, calculate its percentage stripping quantity.The results are shown in Table 1 and Fig. 1
Percentage stripping quantity=W
1* E
i/ W
2* E
Get the lutein water-soluble powder 100g that embodiment 5 makes, and same batch lutein crystal raw material 100g, according to the illumination effect factor, study on the stability is done in the temperatures involved factorial experiments.
The illumination effect factorial experiments:
Get each 10g of above-mentioned sample, break into portions places the 4500LX lamp box, and respectively at 0 o'clock, 1 o'clock, 2 o'clock, 4 o'clock, 8 o'clock, 12 o'clock, 24 o'clock, the absorbance of 48 o'clock sampling and measuring phylloxanthins calculated storage rate.
Storage rate=(measuring absorbance/initial absorbance) * 100%
The results are shown in Table 2.
The temperatures involved test:
Get each 10g of above-mentioned sample, break into portions places 70 ℃ of calorstats, and respectively at 0 o'clock, 1 o'clock, 2 o'clock, 4 o'clock, 8 o'clock, 12 o'clock, 24 o'clock, the absorbance of 48 o'clock sampling and measuring phylloxanthins calculated storage rate.
The fluidity test of micropowder:
Get the lutein water-soluble powder that an amount of embodiment 6 is worth, 4 * 1 * 1 centimetre rectangular box is filled, its Strobilus Pini degree is suitable, till box is progressively tilted to the lutein water-soluble powder and begins to flow out.The angle that box tilts is angle of repose.Parallel assay 3 times, 35 degree, 34 degree, 34 degree, be 34 degree the average angle of repose that gets lutein solid dispersoid, can satisfy industrial need for liquidity.
The results are shown in Table 3.
The dissolution determination data of phylloxanthin and result of calculation (E=0.51) in the table 1 lutein water-soluble powder
| Sample time (min) | Absorbance E i | Percentage stripping quantity (%) | The residual molten amount (%) for the treatment of |
| 0 | 0.0617 | 12.1 | 87.9 |
| 5 | 0.1237 | 24.25 | 75.75 |
| 10 | 0.2809 | 55.08 | 44.92 |
| 15 | 0.3701 | 72.57 | 27.43 |
| 20 | 0.4552 | 89.25 | 10.75 |
| 25 | 0.4889 | 95.86 | 4.14 |
| 30 | 0.4909 | 96.25 | 3.75 |
| 35 | 0.501 | 98.23 | 1.77 |
| 40 | 0.5061 | 99.23 | 0.77 |
| 45 | 05073 | 99.47 | 0.53 |
Table 2 illumination (4500LX) is to the influence of phylloxanthin stability:
| Time | | Storage rate | |
| 0 | Lutein crystal | 100% | |
| ? | The lutein water- |
100% | |
| 1 o'clock | Lutein crystal | 63% | |
| ? | The lutein water-soluble powder | 98% | |
| 2 o'clock | Lutein crystal | 52% | |
| ? | The lutein water-soluble powder | 96% | |
| 4 o'clock | Lutein crystal | 36% | |
| ? | The lutein water-soluble powder | 96% | |
| 8 o'clock | Lutein crystal | 23% | |
| ? | The lutein water-soluble powder | 95% | |
| 12 o'clock | Lutein crystal | 7% | |
| ? | The lutein water-soluble powder | 95% | |
| 24 | Lutein crystal | 0% | |
| ? | The lutein water-soluble powder | 94% | |
| 48 | Lutein crystal | 0% | |
| ? | The lutein water-soluble powder | 94% |
Table 3 high temperature is to the influence of phylloxanthin stability:
| Time | | Storage rate | |
| 0 | Lutein crystal | 100% | |
| ? | The lutein water- |
100% | |
| 1 o'clock | Lutein crystal | 61% | |
| ? | The lutein water-soluble powder | 98% | |
| 2 | Lutein crystal | 50% | |
| ? | The lutein water-soluble powder | 97% | |
| 4 o'clock | Lutein crystal | 32% | |
| ? | The lutein water-soluble powder | 95% | |
| 8 o'clock | Lutein crystal | 18% | |
| ? | The lutein water-soluble powder | 93% | |
| 12 | Lutein crystal | 0% | |
| ? | The lutein water-soluble powder | 93% | |
| 24 | Lutein crystal | 0% | |
| ? | The lutein water-soluble powder | 91% | |
| 48 | Lutein crystal | 0% | |
| ? | The lutein water-soluble powder | 91% |
Claims (8)
1. lutein water-soluble powder, it is characterized in that: comprise phylloxanthin, carrier, additives, its weight ratio is a phylloxanthin: carrier: additives are 1:1-10:0-3.
2. by the described lutein water-soluble powder of claim 1, it is characterized in that: phylloxanthin is a content greater than 50% phylloxanthin powder or lutein crystal; Carrier be a kind of in polyvidone, Polyethylene Glycol, mannose, galactose, the cholic acid or they arbitrarily than mixture; Additives be a kind of in Polysorbate, Span, fatty acid cane sugar ester, tocopherol, ascorbic acid, the tert-butyl group hydroxyphenyl methyl ether or they arbitrarily than mixture.
3. by the described lutein water-soluble powder of claim 2, it is characterized in that: described polyvidone be among C15, C30, K-25, K29/32, K90, the K90D any one or they arbitrarily than mixture; Described Polyethylene Glycol be in polyethylene glycol 1500, Macrogol 2000, Macrogol 3000, Macrogol 4000, polyethylene glycol 6000, the Polyethylene Glycol 8000 any one or they arbitrarily than mixture.
4. by the described lutein water-soluble powder of claim 2, it is characterized in that: described Polysorbate be in polysorbate60, tween 61, polysorbate65, Tween 80, sorbimacrogol oleate100, the polysorbate85 any one or they arbitrarily than mixture; Described Span be in sorbester p18, sorbester p38, sorbester p17, span 83, the sorbester p37 any one or they arbitrarily than mixture; Described fatty acid cane sugar ester be among SE12, SE13, SE14, the SE15 any one or they arbitrarily than mixture.
5. the preparation method of a lutein water-soluble powder as claimed in claim 1 is characterized in that: described lutein water-soluble powder is to adopt the solvent method preparation, with phylloxanthin, carrier, additives with organic solvent dissolution after evaporate to dryness pulverize.
6. by the preparation method of the described lutein water-soluble powder of claim 5, it is characterized in that: described organic solvent be a kind of in acetone, dehydrated alcohol, 95 ethanol, the ethyl acetate or they arbitrarily than mixture.
7. by the preparation method of the described lutein water-soluble powder of claim 6, it is characterized in that: described dissolution conditions is 20-50 ℃, stirs 5-30 minute; Described evaporate to dryness condition is 30-85 ℃, and vacuum is the 0-1 MPa.
8. by the described lutein water-soluble powder of claim 1, it is characterized in that: described lutein water-soluble powder and the carrier of pharmaceutically accepting mix, and make tablet, capsule, powder or make medicine or the functional food of accepting clinically.
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| CN103860476A (en) * | 2014-02-28 | 2014-06-18 | 广州新济药业科技有限公司 | Lutein water soluble powder and preparation method thereof |
| CN104095816A (en) * | 2013-04-07 | 2014-10-15 | 沈阳药科大学 | Lutein ester nano particle and preparation method thereof |
| CN108294297A (en) * | 2017-02-24 | 2018-07-20 | 南通励成生物工程有限公司 | A kind of preparation method of lutein nutrition fortifier |
| CN109222093A (en) * | 2018-08-29 | 2019-01-18 | 华南理工大学 | A kind of water-soluble multi-nutrition additive and preparation and application with eye healthcare function |
| CN113491333A (en) * | 2021-07-06 | 2021-10-12 | 广西壮元医药科技有限公司 | Calcium chewable tablet added with water-soluble lutein and preparation method |
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| CN103860476B (en) * | 2014-02-28 | 2017-06-23 | 广州新济药业科技有限公司 | lutein water-soluble powder and preparation method thereof |
| CN108294297A (en) * | 2017-02-24 | 2018-07-20 | 南通励成生物工程有限公司 | A kind of preparation method of lutein nutrition fortifier |
| CN109222093A (en) * | 2018-08-29 | 2019-01-18 | 华南理工大学 | A kind of water-soluble multi-nutrition additive and preparation and application with eye healthcare function |
| CN113491333A (en) * | 2021-07-06 | 2021-10-12 | 广西壮元医药科技有限公司 | Calcium chewable tablet added with water-soluble lutein and preparation method |
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| Publication number | Publication date |
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| CN102038644B (en) | 2013-05-29 |
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