CN108185424A - Carotenoid microparticle formulation and preparation method thereof - Google Patents
Carotenoid microparticle formulation and preparation method thereof Download PDFInfo
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- CN108185424A CN108185424A CN201711456450.1A CN201711456450A CN108185424A CN 108185424 A CN108185424 A CN 108185424A CN 201711456450 A CN201711456450 A CN 201711456450A CN 108185424 A CN108185424 A CN 108185424A
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- Prior art keywords
- carotenoid
- microparticle formulation
- gelation
- wall material
- mixture
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- 239000004261 Ascorbyl stearate Substances 0.000 description 1
- LITUBCVUXPBCGA-WMZHIEFXSA-N Ascorbyl stearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@H](O)[C@H]1OC(=O)C(O)=C1O LITUBCVUXPBCGA-WMZHIEFXSA-N 0.000 description 1
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- 235000007688 Lycopersicon esculentum Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 240000003768 Solanum lycopersicum Species 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
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- 235000019276 ascorbyl stearate Nutrition 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 235000019282 butylated hydroxyanisole Nutrition 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
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- 239000000706 filtrate Substances 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 150000008131 glucosides Chemical class 0.000 description 1
- 239000007887 hard shell capsule Substances 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- KCYQMQGPYWZZNJ-BQYQJAHWSA-N hydron;2-[(e)-oct-1-enyl]butanedioate Chemical compound CCCCCC\C=C\C(C(O)=O)CC(O)=O KCYQMQGPYWZZNJ-BQYQJAHWSA-N 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000009610 hypersensitivity Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 150000002772 monosaccharides Chemical group 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 210000002394 ovarian follicle Anatomy 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000001054 red pigment Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
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- 235000015424 sodium Nutrition 0.000 description 1
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- 238000011105 stabilization Methods 0.000 description 1
- ANOBYBYXJXCGBS-UHFFFAOYSA-L stannous fluoride Chemical compound F[Sn]F ANOBYBYXJXCGBS-UHFFFAOYSA-L 0.000 description 1
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- 239000010409 thin film Substances 0.000 description 1
- 210000004291 uterus Anatomy 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/20—Agglomerating; Granulating; Tabletting
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/045—Hydroxy compounds, e.g. alcohols; Salts thereof, e.g. alcoholates
- A61K31/07—Retinol compounds, e.g. vitamin A
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Pharmacology & Pharmacy (AREA)
- General Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Mycology (AREA)
- Nutrition Science (AREA)
- Medicinal Preparation (AREA)
- Cosmetics (AREA)
Abstract
Carotenoid microparticle formulation and preparation method thereof, the preparation are the microparticle formulations obtained by the raw mixture containing carotenoid and gelation wall material is pelletized after emulsification treatment；It is characterized in that, the gelation wall material is starch and carbohydrate according to mass ratio 15:1 wall material mixture handles gained through gelation.The present invention overcomes carotenoid raw material in the application it is intrinsic the defects of, the problems such as it is low to solve bioavilability, poorly water-soluble；And pass through the selection and combination of gelation wall material and deoxidier, the mechanical strength and stability of carotenoid microparticle formulation are substantially increased, can be applied to prepare food, drug, health products, functional food field.
Description
Technical field
The present invention relates to a kind of carotenoid formulation and preparation methods.
Background technology
Carotenoid (carotenoids) is a kind of in yellow, orange red or red polyenoid class substance, generally by 8
Isoprenoid unit forms, and molecular formula is generally C40H56.It is well known that carotenoid has beneficial effect to health
Fruit, if it is provitamin A, can prevent yctalopia, being capable of anti-oxidant, anti-cancer, strong coloring force etc..Carotenoid is a kind of
Physiology antioxidant can hinder the peroxidating of lipoid, so as to protect the Steroidgenesis cell of ovarian follicle and uterus not oxidized.But
It is that carotenoid is all not soluble in water, and the solubility in fat and oil is very low, while unstable to light, oxygen, heat.It is this
Limited solubility and the hypersensitivity to oxygen, greatly limit the application of carotenoid.
Many improvement tinctorial yields have been disclosed and improve absorptivity or the method for bioavailability, and microencapsulation method is exactly
One of most effective, most succinct method.Micro-capsule be by solid, liquid or gaseous matter embedding, seal up for safekeeping in a kind of microcapsules into
For a kind of technology of solid granulates product.The ingredient being embedded can be protected in this way, be allowed to it is extraneous should not environment want to completely cut off, reach
The original color, smell and taste of holding, performance and bioactivity to the limit, and prevent the destruction and loss of nutriment.By micro-
Capsule technology, which prepares Beadlets particles, can also expand its application field.Carotenoid microparticle formulation product hardness is high, main to be applicable in
In production tablet and hard shell capsules class product.Carotenoid formulation simultaneously, also can by sensitive carotenoid crystals or ointment,
Its stability is improved using the protection of protecting colloid.
However carotenoid is even across microencapsulation, in product storage and application process, by light, oxygen, heat, acid
It influences, the content of carotenoid can also decline.The quality of microencapsulation is decided by the quality of wall material and preparation method, this field skill
Art personnel also never stop the optimization exploration of carotenoid micro-capsule wall material and preparation method.How the embedding of wall material is improved
Property, optimize preparation process, influence of the oxygen to carotenoid when prepared by removal in system, while obtain hardness height, stability
Good carotenoid microparticle formulation is the emphasis that the present invention studies.
Invention content
An object of the present invention first consists in and provides a new class of carotenoid microparticle formulation, is containing carotenoids
Element and gelation wall material raw mixture pelletize after emulsification treatment obtained by microparticle formulation；The gelation wall material is to form sediment
Powder and carbohydrate are according to mass ratio 1-5:1 wall material mixture handles gained through gelation.
Further, the present invention is intended to provide the preparation method of above-mentioned carotenoid microparticle formulation, includes the following steps
A) by raw mixture through the lotion that grain size is 0.5-1 μm is made；
B) it pelletizes, obtains carotenoid microparticle formulation.
The present invention with microencapsulation overcome carotenoid raw material in the application it is intrinsic the defects of, solve biology
The problems such as availability is low, poorly water-soluble；And pass through the selection and combination of gelation wall material and deoxidier, substantially increase class Hu trailing plants
The mechanical strength and stability of Bu Su microparticle formulations.Based on this, further aspect of the present invention provides the carotenoid microparticle formulation
Application in food, drug, health products, functional food is prepared.
Specific embodiment
The present invention provides Carotenoids microparticle formulation and preparation method thereof.
Heretofore described carotenoid microparticle formulation is containing carotenoid and the mixing of the raw material of gelation wall material
Object pelletize after emulsification treatment gained microparticle formulation；The wherein described gelation wall material is starch and carbohydrate according to matter
Amount compares 1-5:1 wall material mixture handles gained through gelation.
In the wall material mixture addressed, the selection of starch and carbohydrate and ratio are that effect of the present invention is able to reality
Existing important technology feature.In specific embodiment, the starch is converted starch；It is preferred that starch Sodium Octenyl Succinate.
The carbohydrate is selected from the sugar that 10 and following monosaccharide form linear chain or branch chain by glucosides key connection, can illustrate but
It is not limited to sucrose, glucose, glucose syrup, fructose, maltose, lactose, xylose, oligoisomaltose, oligofructose, solid jade
Rice syrup, stachyose, galactooligosaccharide or its mixture.Wherein particularly preferably glucose, solid content be 40-90% glucose
Slurry or its mixture according to arbitrary proportion.In terms of dosage determines, the mass ratio of starch and carbohydrate is 1-5:1, it is excellent
Select 1-4:1, most preferably 3:1.Without specified otherwise, described in this specification and and its mixture, refer to arbitrary 2 in aforementioned each component
In or 2 in above component, according to the mixture of arbitrary proportion.
Another important feature is that the gelation processing of wall material mixture in the present invention.The gelation processing is by wall material
Mixture is configured to after the aqueous solution of 45-70% solid contents, and 60 DEG C are dispersed with stirring dissolving 30min, then in 70-90 DEG C of condition
Lower stirring 15-100min.In preferred embodiment, stirring operation carries out under the conditions of 80-90 DEG C, mixing time 15-60min,
It is preferred that 15-30min.Under the described conditions, the size of the gelation wall material particle prepared through starch fluidized-bed process is 1-2mm,
Heap density can reach 0.75-0.8g/ml, and for particle hardness up to more than 100N, it is 70-100bloom that gel, which freezes power intensity,.
The dosage of gelation wall material is calculated based on carotenoid microparticle formulation finished product quality, and dosage is finished product
The 30-65% of quality, preferably 40%-60%, more preferable 45-55%.
In another embodiment of the present invention, in the raw mixture in addition to carotenoid and gelation wall material, also contain
There is antioxidant, the antioxidant is selected from tocopherol, aliphatic acid acid ascorbyl ester, butylated hydroxytoluene
(BHT), butylated hydroxy anisole (BHA), propyl gallate, t-butyl hydroxy quinoline or its mixture；It is described
The dosage of antioxidant is the 0.1%-10% of carotenoid microparticle formulation quality.It is preferred that 1%-5%.
Containing aerobic in lotion obtained by raw mixture, in microencapsulation, preparation of the oxygen to particle in lotion
Process and products obtained therefrom have a larger impact, and common process vacuumizes, logical nitrogen etc. can only take off the method for lotion deoxidation
Except the bubble of system, and being dissolved in the dissolved oxygen in lotion can not be removed by this method.To remove dissolved oxygen, this hair is provided
Bright another specific embodiment adds in deoxidier removing lotion in raw mixture after emulsification treatment in the lotion of gained
Oxygen.The deoxidier available for lotion deoxidation described in the prior art is numerous.In embodiments of the present invention, Vitamin C is selected
Acid and/or sodium ascorbate, the residual oxygen amount (remaining oxygen) of obtained lotion
For 0.1-0.3mg/L.Other than it can effectively remove the oxygen in lotion, it was also found that selecting anti-bad in experiment
Hematic acid and/or sodium ascorbate are as deoxidier, moreover it is possible to increase the stability of product, and the number of contrast test is it was demonstrated that this is steady
It is qualitative not only related to the low oxygen content in solution.This effect is de- in combination ascorbic acid and ascorbic acid composition of sodium
It is especially pronounced during oxygen agent.In the ascorbic acid and ascorbic acid composition of sodium, ascorbic acid and sodium ascorbate are according to matter
Measure ratio 1:1-5 is mixed, and preferably 1:1-4.
In technical scheme of the present invention, the deoxidier dosage is the 1- of carotenoid microparticle formulation finished product quality
10%, preferably 2-7%, more preferable 3-6%.The pH that the deoxidier uses in lotion is 3-6, preferably 3.5-4.5.Lotion
PH be adjusted by 0.1M sodium hydroxide solutions and anhydrous citric acid.
In carotenoid microparticle formulation of the present invention, the carotenoid be selected from lutein, zeaxanthin, kind
Lycopene, alpha-carotene, beta carotene, canthaxanthin, lutein ester, astaxanthin or its mixture.
On the other hand, the preparation method of carotenoid microparticle formulation of the invention includes the following steps：
A) by raw mixture through the lotion that grain size is 0.5-1 μm is made；
B) it pelletizes, obtains carotenoid microparticle formulation.
It is described when preparation applied to the carotenoid microparticle formulation, the i.e. product containing deoxidier of preferred embodiment
Preparation method should adaptability comprising correlation step, i.e., the method includes following step：
A) by raw mixture through the lotion that grain size is 0.5-1 μm is made；
B) deoxidier is added in, removes the oxygen in lotion；
C) it pelletizes, obtains carotenoid microparticle formulation.
In the concrete scheme of above-mentioned arbitrary preparation method, in the step a), raw mixture is prepared as lotion
Method, Ke Yishi：Raw mixture through 120 degree of instantaneous melting 5s, then carried out under 45 ± 5Mpa pressure it is high-pressure homogeneous twice
Or colloid mill high speed dispersion 30min is used, the lotion that grain size is 0.5-1 μm is made.
In the concrete scheme of above-mentioned arbitrary preparation method, the step c), i.e., in granulation step, the method for granulation can be with
It is the granulations modes such as well known wet granulation in industry, dry granulation, spray drying, starch fluidized bed granulation, spray congealing.
The carotenoid microparticle formulation heap density 0.8g/ml of the present invention, product is at 40 DEG C, relative humidity (RH) 75%
Under under part, 6 months stable contents；Under gained tablet is under the conditions of 40 DEG C, relative humidity (RH) 75% after tabletting, 6 months contents
Stablize.It can be used as a kind of raw material, be processed further piece agent, capsule form dietary supplements or solid beverage, energy is made
The food and functional food of length bar or candy form.
Following non-limiting examples will be evident from the present invention, but be not construed as any form of to the present invention
It limits, unless otherwise specified, product is measured and evaluated using following methods in the application.
The hardness of gelation wall material of the present invention is measured by the automatic detector for strength of particles FT801 of Rui Ke, described
Gelation wall material gel freeze power pass through rising sun sun JS- II freeze force tester measure.
Residual oxygen amount of the present invention is measured by plum Teller S4 model dissolved oxygen meters.
In the present invention, encapsulation efficiency is represented using surface pigment content, surface pigment content is higher, and encapsulation efficiency is got over
Low, the carotenoid not embedded is more, and Simultaneous Stabilization is poorer.The assay method of surface pigment content of the present invention is：
5g micro-capsule products to be measured are added to eggplant-shape bottle, add in 20ml petroleum ethers (30-60 DEG C) thereto, turn to filter after shaking 20s, repetition is washed
It washs twice, merging filtrate, revolving removing petroleum ether, 105 DEG C drying to constant weight, the dry weight of remaining solid and micro-capsule product to be measured
Mass ratio is the content of surface pigment, as a percentage.
Product accelerated stability evaluation method of the present invention is the method that Chinese Pharmacopoeia provides：40 DEG C, 75%RH conditions
Under, the pigment content of the different time of measure is good and bad with its determining stability.And product stability is carried out with following methods fast
Speed evaluation：Opening is positioned in 60 DEG C of baking ovens, measures initial (0 day), and the pigment content of 5 days, 10 days and 20 days is retained with pigment
Rate represents product stability.The ratio of product content and initial content when pigment retention rate is different time, with percentage table
Show.
Embodiment 1：Investigate gelation process molding influence on starch granules
(1) by cornstarch 500g, maltose 500g, the aqueous solution of 45% solid content is configured to, after 60 DEG C are dispersed with stirring,
70 DEG C are warming up to, at the uniform velocity stirs 30min.Deaerate 30min under -0.07MPa, pelletizes under starch fluid unit, emulsion temperature
60 DEG C, inlet air temperature is 100 DEG C, king-tower air inlet 20Hz, exhaust blower 45Hz, atomizing pressure 29Hz, feed flow rate 9ml/min, stream
Change bed wind turbine 20Hz, 50 DEG C of fluidized-bed temperature obtains gelling starches A, and heap density is 0.35mg/ml, hardness 15N, is coagulated
Gelatinization intensity 10Bloom.
(2) by starch Sodium Octenyl Succinate 300g, glucose 60g, the aqueous solution of 55% solid content is configured to, 60 DEG C are stirred
After mixing dispersion, 90 DEG C are warming up to, at the uniform velocity stirs 15min.Deaerate 30min under -0.1MPa, pelletizes under starch fluid unit,
The preparation method is the same as that of Example 1 (1), obtain gelling starches B, heap density be 0.8mg/ml, hardness 105N, gelation intensity
90Bloom。
(3) by starch Sodium Octenyl Succinate 300g, glucose syrup (state's label：GB/T 20885-2007) 100g, is prepared
Into the aqueous solution of 60% solid content, after 60 DEG C are dispersed with stirring, 90 DEG C are warming up to, at the uniform velocity stirs 60min.It deaerates under -0.1MPa
30min pelletizes under starch fluid unit, and the preparation method is the same as that of Example 1 (1), obtains gelling starches C, and heap density is
0.80mg/ml, hardness 135N, gelation intensity 100Bloom.
(4) by starch Sodium Octenyl Succinate 300g, sucrose 100g, the aqueous solution of 70% solid content is configured to, 60 DEG C are stirred
After mixing dispersion, 90 DEG C are warming up to, at the uniform velocity stirs 100min.Deaerate 30min under -0.1MPa, pelletizes under starch fluid unit,
The preparation method is the same as that of Example 1 (1), obtain gelling starches D, heap density be 0.46mg/ml, hardness 38N, gelation intensity
50Bloom。
(5) comparative example：300g, glucose (are purchased from Wuhan and remotely create Science and Technology Ltd.) to pre-gelatinized cornstarch
100g is starched, the aqueous solution of 60% solid content is configured to, after 60 DEG C are dispersed with stirring, are warming up to 90 DEG C, at the uniform velocity stir 60min.-
Deaerate 30min under 0.1MPa, pelletizes under starch fluid unit, and the preparation method is the same as that of Example 1 (1), obtains gelling starches
E, heap density are 0.41mg/ml, hardness 32N, gelation intensity 15Bloom.
(6) comparative example：By starch Sodium Octenyl Succinate 300g, oligofructose (GB/T23528-2009) 100g, prepare
Into the aqueous solution of 60% solid content, after 60 DEG C are dispersed with stirring, 90 DEG C are warming up to, at the uniform velocity stirs 60min.It deaerates under -0.1MPa
30min pelletizes under starch fluid unit, and the preparation method is the same as that of Example 1 (1), obtains gelling starches F, and heap density is
0.38mg/ml, hardness 29N, gelation intensity 23Bloom.
(7) comparative example：By starch Sodium Octenyl Succinate 300g, glucose syrup (state's label：GB/T 20885-2007)
100g is configured to the aqueous solution of 60% solid content, and after 45 DEG C are dispersed with stirring, deaerate 30min under -0.1MPa, in starch fluid bed
It pelletizes under equipment, the preparation method is the same as that of Example 1 (1), obtains gelling starches G, and heap density is 0.42mg/ml, and hardness is
52N, gelation intensity 39Bloom.
In summary, treated that starch granules hardness, heap density and gel strength all increase for gelation.Octenyl
Succinic acid starch sodium and glucose syrup, according to 3:The hardness of 1 ratio gained gelatinized starch granule after gelation is most strong, heap
Density highest, gel strength highest.
Embodiment 2：Ascorbic acid and sodium ascorbate test newborn deoxidation effect of the invention
(1) by starch Sodium Octenyl Succinate 300g, fructose 100g, the aqueous solution of 45% solid content is configured to, 60 DEG C are stirred
After mixing dispersion, 90 DEG C, gelation 30min are warming up to, it is 7.2mg/L to measure lotion remaining oxygen, and rear remaining oxygen is 7.5mg/L for 24 hours.
Add in astaxanthin oil resin (being purchased from Dalian Yi Nuo Biological Co., Ltd.) 100g, through high-pressure homogeneous under 45 ± 5Mpa pressure or
After colloid mill dispersion 30min, the lotion below 1 μm of grain size is obtained, through wet granulation, 2000 turns/min of cutter, 2500 turns of stirring/
Min, Granulation time 80s, drying time 30min, drying temperature enter the wind 55 DEG C, obtain astaxanthin microparticle formulation 1, said preparation 60
DEG C, when opening is placed 5 days, 10 days and 20 days, pigment retention rate is respectively 70.1%, 62.1% and 43.6%.
(2) starch Sodium Octenyl Succinate 300g, xylose (GB/T23532-2009) 75g are configured to 70% solid content
Aqueous solution, after 60 DEG C are dispersed with stirring, be warming up to 90 DEG C, gelation 30min.Nitrogen, flow 0.1ml/ are passed through in lotion
Min, maintaining nitrogen purge 30min, it is 0.3mg/L to measure lotion remaining oxygen, and rear remaining oxygen is 6.5mg/L for 24 hours.Add in astaxanthin oil
Resin 100g after high-pressure homogeneous under 45 ± 5Mpa pressure or colloid mill dispersion 30min, obtains the lotion below 1 μm of grain size, passes through
Wet granulation obtains astaxanthin microparticle formulation 2, and 60 DEG C of said preparation, when opening is placed 5 days, 10 days and 20 days, pigment retention rate divides
It Wei 77.1%, 69.1% and 60.6%.
(3) by starch Sodium Octenyl Succinate 300g, maltose 60g, the aqueous solution of 45% solid content is configured to, 60 DEG C are stirred
After mixing dispersion, 90 DEG C are warming up to, gelation 30min.Lotion vacuumizes under -0.09MPa, and it is 3.4mg/ to measure lotion remaining oxygen
L, rear remaining oxygen is 6.7mg/L for 24 hours.Astaxanthin oil resin 100g is added in, through high-pressure homogeneous or colloid mill under 45 ± 5Mpa pressure
After disperseing 30min, the lotion below 1 μm of grain size is obtained, through wet granulation, obtains astaxanthin microparticle formulation 3,60 DEG C of said preparation,
When opening is placed 5 days, 10 days and 20 days, pigment retention rate is respectively 73.4%, 65.5% and 55.3%.
(4) starch Sodium Octenyl Succinate 300g, xylose (GB/T23532-2009) 75g are configured to 70% solid content
Aqueous solution, after 60 DEG C are dispersed with stirring, be warming up to 90 DEG C, gelation 30min.It is adjusted with anhydrous citric acid and 0.1M sodium hydroxides
PH is 3.0, adds ascorbic acid 1.25g, sodium ascorbate 6.25g, and it is 0.2mg/L to measure lotion remaining oxygen, for 24 hours rear residual oxygen
It measures as 0.2mg/L.Astaxanthin oil resin 100g is added in, after high-pressure homogeneous under 45 ± 5Mpa pressure or colloid mill dispersion 30min,
The lotion below 1 μm of grain size is obtained, through wet granulation, obtains astaxanthin microparticle formulation 4,60 DEG C of said preparation, opening is placed 5 days,
At 10 days and 20 days, pigment retention rate is respectively 94.1%, 94.7% and 94.2%.
(5) by starch Sodium Octenyl Succinate 200g, glucose syrup 50g, it is configured to the aqueous solution of 53% solid content, 60 DEG C
After being dispersed with stirring, 90 DEG C are warming up to, gelation 30min.It is 4.5 to adjust pH with anhydrous citric acid and 0.1M sodium hydroxides, is added in
Ascorbic acid 3g, sodium ascorbate 12g, it is 0.1mg/L to measure lotion remaining oxygen, and rear remaining oxygen is 0.0mg/L for 24 hours.Add in shrimp
Green vegetable oil resin 100g after high-pressure homogeneous under 45 ± 5Mpa pressure or colloid mill dispersion 30min, is obtained below 1 μm of grain size
Lotion through wet granulation, obtains astaxanthin microparticle formulation 5,60 DEG C of said preparation, when opening is placed 5 days, 10 days and 20 days, pigment
Retention rate is respectively 99.8%, 98.9% and 99.0%.
(6) starch Sodium Octenyl Succinate 500g, solid high fructose corn (GB/T26762-2011) 167g are configured to 62%
The aqueous solution of solid content after 60 DEG C are dispersed with stirring, is warming up to 90 DEG C, gelation 30min.With anhydrous citric acid and 0.1M hydroxides
It is 3.5 that sodium, which adjusts pH, adds in ascorbic acid 10.0g, sodium ascorbate 10.0g, and it is 0.1mg/L to measure lotion remaining oxygen, for 24 hours after
Remaining oxygen is 0.1mg/L.Astaxanthin oil resin 100g is added in, is disperseed through high-pressure homogeneous under 45 ± 5Mpa pressure or colloid mill
After 30min, the lotion below 1 μm of grain size is obtained, through wet granulation, obtains astaxanthin microparticle formulation 6,60 DEG C of said preparation is open
When placing 5 days, 10 days and 20 days, pigment retention rate is respectively 92.1%, 91.7% and 91.0%.
In summary, under the conditions of pH is 3.5-4.5, ascorbic acid and sodium ascorbate are according to mass ratio 1:4 cooperations make
With best for the deoxidation effect of lotion of the present invention, the stability of products obtained therefrom is best.Although vacuumize or be passed through nitrogen
Also there is certain effect, but lotion oxygen content increases after placing for a long time, this is unfavorable in Workshop Production.Ascorbic acid and
Being applied in combination for sodium ascorbate can keep low oxygen content in lotion, oxygen be avoided to reenter in lotion so that from producing
Process control is more effective.
Embodiment 3：The preparation of lutein grain preparation and characterization
(1) by starch Sodium Octenyl Succinate 175.5g, glucose 58.5g, it is configured to the aqueous solution of 60% solid content, 60
After DEG C being dispersed with stirring, 90 DEG C are warming up to, gelation 30min.Add in mixed tocopherol 20g, ascorbyl palmitate 4g, leaf Huang
Cellulose crystal 34g, colloid mill grinding and thin film evaporation degassing, it is 3.0 to adjust pH with citric acid and sodium hydroxide, adds Vitamin C
Sour 20g, sodium ascorbate 20g pelletize under starch fluid unit, 65 DEG C of emulsion temperature, and inlet air temperature is 100 DEG C, king-tower
Enter the wind 20Hz, exhaust blower 45Hz, atomizing pressure 29Hz, feed flow rate 9ml/min, fluid bed wind turbine 20Hz, fluidized-bed temperature 50
DEG C, obtain lutein particles A, content 5.95%, heap density be 0.7mg/ml, surface pigment content be 0.03%, 40 DEG C,
When being stored 6 months under the conditions of 75%RH, pigment content 5.94%.
(2) by starch Sodium Octenyl Succinate 43.5g, glucose syrup 87g, it is configured to the aqueous solution of 60% solid content, 60
After DEG C being dispersed with stirring, 85 DEG C are warming up to, gelation 30min.Dl- alpha-tocopherol 40g, ascorbyl palmitate 10g are added in,
BHT10g, lutein crystal 150g, colloid mill grinding and vacuum outgas, it is 3.5, then add to adjust pH with citric acid and sodium hydroxide
Enter ascorbic acid 12g, sodium ascorbate 48g, spray congealing granulation, 60 DEG C of emulsion temperature, inlet air temperature is 80 DEG C, king-tower air inlet
25Hz, exhaust blower 37Hz, atomizing pressure 29Hz, feed flow rate 12ml/min, fluid bed wind turbine 20Hz, -15 DEG C of fluidized-bed temperature,
Obtain lutein particles B, content 10.5%, heap density be 0.75mg/ml, surface pigment content be 0.05%, 40 DEG C,
When being stored 6 months under the conditions of 75%RH, pigment content 10.6%.
(3) by hydroxypropyl PASELLI EASYGEL 43.5g, glucose syrup 87g, it is configured to the aqueous solution of 60% solid content, 60
After DEG C being dispersed with stirring, 85 DEG C are warming up to, gelation 30min.Dl- alpha-tocopherol 40g, ascorbyl palmitate 10g are added in,
BHT10g, lutein crystal 150g, colloid mill grinding and vacuum outgas, it is 3.5, then add to adjust pH with citric acid and sodium hydroxide
Enter ascorbic acid 12g, sodium ascorbate 48g, spray-drying process, 60 DEG C of emulsion temperature, inlet air temperature is 160 DEG C, king-tower into
Wind 20Hz, exhaust blower 47Hz, atomizing pressure 0.3Mpa, feed flow rate 9ml/min, 80 DEG C of leaving air temp obtain lutein particle
C, content 10.9%, heap density are 0.37mg/ml, and surface pigment content is 4.95%, 40 DEG C, is stored under the conditions of 75%RH
At 6 months, pigment content 4.04%.
Embodiment 4：The preparation of beta carotene microparticle formulation and characterization
By starch Sodium Octenyl Succinate 273g, sucrose 68.25g, it is configured to the aqueous solution of 55% solid content, 60 DEG C of stirrings
After dispersion, 80 DEG C are warming up to, gelation 15min.Add in mixed tocopherol 9g, ascorbyl palmitate 4g, beta carotene crystalline substance
Body 110g, colloid mill grinding and vacuum outgas, it is 4.0 to adjust pH with citric acid and sodium hydroxide, adds ascorbic acid 5.8g,
Sodium ascorbate 29.2g pelletizes under starch fluid unit, 63 DEG C of emulsion temperature, and inlet air temperature is 60 DEG C, king-tower air inlet
18Hz, exhaust blower 37Hz, atomizing pressure 27Hz, feed flow rate 9ml/min, fluid bed wind turbine 20Hz, 45 DEG C of fluidized-bed temperature obtain
Beta carotene particle D, content 21.34%, heap density be 0.45mg/ml, surface pigment content be 1.74%, 40 DEG C,
When being stored 6 months under the conditions of 75%RH, pigment content 10.19%.
Embodiment 5：The preparation of zeaxanthin microparticle formulation and characterization
(1) starch Sodium Octenyl Succinate 226g, oligofructose (GB/T23528-2009) 45.2g are configured to 63%
The aqueous solution of solid content after 60 DEG C are dispersed with stirring, is warming up to 75 DEG C, gelation 60min.BHT2g, alpha-tocopherol 8g are added in, it is beautiful
Cream-coloured matter crystal 34g, colloid mill grinding and falling liquid film degassing, it is 4.0 to adjust pH with citric acid and sodium hydroxide, adds Vitamin C
Sour 2g, sodium ascorbate 6g, spray-drying process obtain zeaxanthin PARTICLE E, content 5.53%, and heap density is
0.49mg/ml, surface pigment content are 0.53%, and 40 DEG C, when being stored 6 months under the conditions of 75%RH, pigment content is
2.26%.
(2) by starch Sodium Octenyl Succinate 226g, glucose 45.2g, it is configured to the aqueous solution of 63% solid content, 60 DEG C
After being dispersed with stirring, 75 DEG C are warming up to, gelation 60min.Add in BHT 2g, alpha-tocopherol 8g, zeaxanthin crystals 34g, shearing
Simultaneously vacuum outgas is emulsified, it is 4.0 to adjust pH with citric acid and sodium hydroxide, adds ascorbic acid 2g, sodium ascorbate 6g, is sprayed
Mist drying and granulating obtains zeaxanthin particle F, content 5.43%, and heap density is 0.77mg/ml, and surface pigment content is
0.01%, 40 DEG C, when being stored 6 months under the conditions of 75%RH, pigment content 5.49%.
Embodiment 6：The preparation of astaxanthin microparticle formulation and characterization
Starch Sodium Octenyl Succinate 254.4g, oligoisomaltose 63.6g are configured to the water-soluble of 70% solid content
Liquid after 45 DEG C are dispersed with stirring, is warming up to 75 DEG C, gelation 100min.Propyl gallate 12g, astaxanthin oil resin 126g, cuts
Simultaneously vacuum outgas after emulsifying is cut, it is 4.5 to adjust pH with citric acid and sodium hydroxide, adds ascorbic acid 6g, sodium ascorbate
24g, spray congealing granulation obtain astaxanthin particle G, content 2.12%, and heap density is 0.38mg/ml, and surface pigment contains
It is 3.51% to measure, 40 DEG C, when being stored 6 months under the conditions of 75%RH, pigment content 0.50%.
Embodiment 7：The preparation of lycopene microparticle formulation and characterization
By starch Sodium Octenyl Succinate 155.1g, maltose 30.6g, it is configured to the aqueous solution of 60% solid content, 60 DEG C
After being dispersed with stirring, 80 DEG C are warming up to, gelation 50min.Mixed tocopherol 6.6g, ascorbyl stearate 2.4g are added in, kind
Lycopene crystal 40.8g, colloid mill grind and deaerate, and it is 5.0 to adjust pH with citric acid and sodium hydroxide, adds ascorbic acid
0.75g, sodium ascorbate 2.25g pelletize under dry granulating machine, 150 DEG C of inlet air temperature, 100 DEG C of temperature of outgoing air, obtain tomato
Red pigment particle H, content 10.88%, heap density be 0.66mg/ml, surface pigment content be 0.2%, 40 DEG C, 75%RH items
When being stored 6 months under part, pigment content 3.81%.
Embodiment 8：The preparation of lutein ester microparticle formulation and characterization
By starch Sodium Octenyl Succinate 85.2g, glucose syrup 21.4g, it is configured to the aqueous solution of 55% solid content, 60 DEG C
After being dispersed with stirring, 90 DEG C are warming up to, gelation 30min.Add in t-butyl hydroxy quinoline 2.0g, mixed tocopherol 6.0g, leaf Huang
Plain crystalline esters 29.4g, high-pressure homogeneous and deaerate, it is 6.0 to adjust pH with citric acid and sodium hydroxide, adds ascorbic acid 2g,
Sodium ascorbate 10g pelletizes under starch fluid unit, obtains lutein ester particle I, content 11.02%, heap density
For 0.68mg/ml, surface pigment content is 0.3%, and 40 DEG C, when being stored 6 months under the conditions of 75%RH, pigment content is
10.99%.
Embodiment 9：Carotenoid product plays tablet stability test
After carotenoid particle in embodiment 3-8 and multivitamin are beaten piece auxiliary material batch mixing, day peak ZPW-8 is used
Type rotary tablet machine carries out tabletting, obtains compound carotenoid multivitamin, tablet hardness 80-100N, and friability≤
0.5%, tablet is packaged in the HDPE bottles of its lid heat-sealed aluminium foils sealing, 40 DEG C and 75% relative humidity under by tablet
Storage 6 months, product content and stability are shown in Table 1.
Table 1
Claims (11)
1. carotenoid microparticle formulation is that the raw mixture containing carotenoid and gelation wall material is made after emulsification treatment
The microparticle formulation of grain gained；It is characterized in that, the gelation wall material is starch and carbohydrate according to mass ratio 1-5:1
Wall material mixture through gelation handle gained.
2. carotenoid microparticle formulation according to claim 1, which is characterized in that
The starch is converted starch；
The carbohydrate is selected from sucrose, glucose, glucose syrup, fructose, maltose, lactose, xylose, oligomeric different malt
Sugar, oligofructose, corn syrup solid, stachyose, galactooligosaccharide or its mixture；
The gelation processing is that wall material mixture is configured to after the aqueous solution of 45-70% solid contents, 60 DEG C of stirrings point
Dissolving 30min is dissipated, 15-100min is then stirred under the conditions of 70-90 DEG C.
3. carotenoid microparticle formulation described in claim 1, which is characterized in that the starch is that ocentyl succinic forms sediment
Powder sodium, the carbohydrate are glucose sugar and/or glucose syrup.
4. carotenoid microparticle formulation according to claim 1, which is characterized in that the dosage of the gelation wall material
30-65% for carotenoid microparticle formulation quality.
5. carotenoid microparticle formulation according to claim 1, which is characterized in that also contain in the raw mixture
There is antioxidant, the antioxidant is selected from tocopherol, aliphatic acid acid ascorbyl ester, butylated hydroxytoluene, butylhydroxy fennel
Fragrant ether, propyl gallate, t-butyl hydroxy quinoline or its mixture；The dosage of the antioxidant is carotenoid particle
The 0.1%-10% of the quality of the pharmaceutical preparations.
6. carotenoid microparticle formulation according to claim 1, which is characterized in that the raw mixture is through emulsification
The oxygen in deoxidier removing lotion is added in after processing, the deoxidier is ascorbic acid and/or sodium ascorbate；Deoxidier
Dosage is the 1-10% of carotenoid microparticle formulation quality.
7. carotenoid microparticle formulation according to claim 6, which is characterized in that the deoxidier is ascorbic acid
With sodium ascorbate according to mass ratio 1:The mixture of 1-5.
8. carotenoid microparticle formulation described in claim 1, which is characterized in that the carotenoid be selected from lutein,
Zeaxanthin, lycopene, alpha-carotene, beta carotene, canthaxanthin, lutein ester, astaxanthin or its mixture.
9. carotenoid microparticle formulation described in claim 1, heap density 0.8g/ml, product is at 40 DEG C, relative humidity 75%
Under the conditions of, 6 months stable contents；Gained tablet is under the conditions of 40 DEG C, relative humidity 75% after tabletting, 6 months stable contents.
10. the preparation method of carotenoid microparticle formulation described in claim 1, includes the following steps：
A) by raw mixture through the lotion that grain size is 0.5-1 μm is made；
B) it pelletizes, obtains carotenoid microparticle formulation.
11. the preparation method of the carotenoid microparticle formulation described in claim 6, includes the following steps：
A) by raw mixture through the lotion that grain size is 0.5-1 μm is made；
B) deoxidier is added in, removes the oxygen in lotion；
C) it pelletizes, obtains carotenoid microparticle formulation.
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