CN105596314B - A kind of preparation method of the molten natural astaxanthin microcapsule formulation of high stability cold water - Google Patents
A kind of preparation method of the molten natural astaxanthin microcapsule formulation of high stability cold water Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of the molten natural astaxanthin microcapsule formulation of high stability cold water.Concrete operation step is as follows：Prepared oil phase is well mixed by astaxanthin oil, under oil-soluble inhibitor and water soluble emulsifier heating condition；By in wall material, water soluble antioxidant and filler addition pure water, stirring and dissolving adjusts pH value, and water phase is obtained；Oil phase is added in water phase and is stirred, crossed sand mill and be ground, emulsion is carried out into a step granulation with cold spray starch fluid-bed drying, obtain the microcapsule formulation that particle diameter is 40 100 mesh.The microcapsule formulation that the present invention is provided place 6 months under the conditions of 40 DEG C, the RH75% after content retention rate dissolved in 100ml water more than 95%, 0.1g products after clear without oil slick, in can be applied to the aqueous foods such as beverage.
Description
Technical field
The invention belongs to carotenoid microcapsules technology, and in particular to a kind of molten natural astaxanthin of high stability cold water is micro-
The preparation method of capsule preparations.
Background technology
Astaxanthin (Astaxanthin) is a kind of former carotenoid of keto-acid non-vitamin A.Because astaxanthin has
Color, anti-oxidant, light protection, promotion breeding, enhancing are immunized, safeguard the various biological function such as central nervous system health, in recent years
To be paid close attention to by industries such as domestic and international food, medicine, cosmetics, aquacultures deeply.Astaxanthin mainly by chemical synthesis and by
Extracted in natural materials and obtained.Chemical synthesis astaxanthin is very limited due to its safety issue in application aspect.
At present, in the biogenetic derivation of natural astaxanthin, haematococcus pluvialis (Haematococcus pluvialis) in astaxanthin
Content highest, is acknowledged as producing the best biogenetic derivation of astaxanthin in nature, and turned into recent domestic astaxanthin
The focus of research.
Entitled 3,3 '-dihydroxy -4,4 '-diketo-β, β '-carrotene of astaxanthin chemistry.In astaxanthin molecular structure
Containing 13 conjugated double bonds, the α that hydroxyl present on terminal ring structure and unsaturated ketone group and hydroxyl and ketone group are constituted-
Hydroxy-ketone, the multiple unsaturated double-bond structures shape of astaxanthin its easy light, oxygen, heat effect degraded oxidation, on the other hand, carries
The astaxanthin for taking from haematococcus pluvialis exists in the form of ester, and content accounts for 5% of astaxanthin oil or so, cannot directly apply to water
The environment of property.
Microcapsules technology is then the effective ways for solving the above problems, and is formed because astaxanthin is wrapped in continuous capsule material
Small capsule in, it is to avoid directly contact with environment, so as to keep its stabilization during storage, transport and use
Property, the emulsifying technology that microcapsules are included can be dispersed in water astaxanthin oil, be more easy to be absorbed by the body.
Report about astaxanthin microencapsulation or similar formulations mainly has：
CN200810244049.6 (CN101439029A) is related to a kind of micro-encapsulated astaxanthin with pure glue as wall material
Preparation method, astaxanthin is dissolved in soybean oil under 160 DEG C of -200 DEG C of hot conditions by 3% content, with pure glue be main original
The emulsion that the wall material solution of material is stablized through 40Mpa homogeneous together, then with 190 DEG C of inlet temperature, 90 DEG C of outlet temperature
Condition be spray-dried obtaining microcapsules.With astaxanthin crystal as raw material, raw material prepares cumbersome, microcapsules work to the patent
Skill is also operated including high-temperature fusion unit, more cumbersome.
CN201210561599.7 (CN103875918A) is related to a kind of astaxanthin microcapsule preparation process, and wall material adds water
Wall material solution is mixed into, the emulsifying agent that concentration is 6% is added, wall material emulsifier solution is made, the shrimp that concentration is 3% is added blue or green
Then vegetable oil solution, strong agitation stirs 1min, with 30000r/min into astaxanthin emulsifying agent with 30000r/min twice dispersings
Three dispersion stirring 1min, finally carry out spray drying and are made astaxanthin capsule.The method is not adopted only with emulsification pretreatment
Grinding or high-pressure homogeneous further reduction emulsion particle diameter are taken, products obtained therefrom is dispersed in water rear poor transparency, and spray drying is only entered
Go and once embed, stability has needed further to improve.
The content of the invention
The technical problems to be solved by the invention are the defects for overcoming above-mentioned prior art to exist, there is provided one kind is easy to industry
The preparation method of the molten astaxanthin microcapsule formulation of high stability cold water that metaplasia is produced.The astaxanthin microcapsule formulation that the method is obtained
Good stability, cold water-dispersible is good.
The method is comprised the following steps：A kind of preparation method of the molten natural astaxanthin microcapsule formulation of high stability cold water,
Comprise the following steps that：
1）It is well mixed by astaxanthin oil, under the conditions of 50-60 DEG C of oil-soluble inhibitor and water soluble emulsifier and oil is obtained
Phase；
2）Under the conditions of 50-80 DEG C, by wall material, water soluble antioxidant and filler add pure water in, stirring and dissolving,
Regulation pH value is obtained water phase to 7.5-8.0；
3）Oil phase is added in water phase and is stirred, crossed sand mill and be ground, make the emulsion particle particle diameter after grinding
Below 100nm is reached, emulsion is carried out into a step granulation with cold spray-starch fluid-bed drying, obtain particle diameter for 40-100 purposes
Spherical shape microcapsule formulation.
Step 3 of the present invention）In cold spray-starch fluid-bed drying condition be：Spraying EAT is 0-50 DEG C, is formed sediment
Powder fluid bed blast temperature is 60-80 DEG C.
Step 1 of the present invention）Oil-soluble antioxidant be one kind in natural VE or Rosmarinus officinalis extract or
Two kinds；Addition is the 10-50% of astaxanthin oil quality.
Step 1 of the present invention）HLB value >=13 of middle water soluble emulsifier；Addition is the 10- of astaxanthin oil quality
50%。
Step 1 of the present invention）Middle water soluble emulsifier be polyglyceryl fatty acid ester, sucrose fatty ester, polysorbate-
80th, in polyoxyethylene sorbitan fatty acid ester any one or a few；Addition is the 10-50% of astaxanthin oil quality.
Step 2 of the present invention）Middle wall material is one or two in Arabic gum or starch Sodium Octenyl Succinate；Add
Dosage is 2-3 times of astaxanthin oil quality.
Step 2 of the present invention）Middle filler be hydroxyl isomaltulose, sucrose or glucose in one or two；Addition
Measure is 2-3 times of astaxanthin oil quality.
Step 2 of the present invention）Middle water soluble antioxidant is sodium ascorbate and the mixture of Tea Polyphenols, or Vitamin C
The mixture of sour sodium and citric acid；Addition is 0.1-0.3 times of astaxanthin oil quality.
Step 2 of the present invention）The quality of middle addition pure water is 6-10 times of astaxanthin oil quality.
Using having the beneficial effect that produced by such scheme：
1st, Microcapsules Size reaches below 100nm so that the aqueous dispersions clear of product；By adjusting water phase pH
Value makes wall material reach highest to the embedding rate of astaxanthin；A step granulation is carried out using starch, spherical shape micro-capsule is obtained, can either be risen
Effect to secondary embedding improves stability, can overcome spray drying process gained powder resistance to pressure poor again, is not suitable for carrying out compressing tablet
（Poor fluidity）, the shortcomings of be not suitable for filling hard shell capsules.
2nd, stability test：The microcapsule formulation that the present invention is provided place 6 months under the conditions of 40 DEG C, the RH75% after contain
Amount retention rate is more than 95%.
Specific embodiment
With reference to specific embodiment, the present invention is further detailed explanation.
Embodiment 1
1. astaxanthin oil that 30g contents are 10%, 3.0g natural VEs, 3.0g polyoxyethylene sorbitan monoleates are stirred in 55 DEG C of mixing
15 minutes are mixed to uniform, oil phase is obtained.
2. by 68g Arabic gums, 88g sucrose, 4.0g sodium ascorbates and 4.0g Tea Polyphenols add 300g pure water in, 75
Regulation pH value was obtained water phase to 7.6 to being completely dissolved in 30 minutes for DEG C stirring.
3. 55 DEG C of oil phase is added in the water phase in 75 DEG C of stirrings, continues to stir 30 minutes, then crossed sand mill and follow
Ring is processed 30 minutes, and sand mill rotating speed 2200rpm makes the emulsion particle particle diameter after grinding reach below 100nm, the emulsion for obtaining
Granulated with cold-starch fluid-bed drying is sprayed, obtained astaxanthin micro-capsule, spray drying condition is：40 DEG C of EAT, forms sediment
65 DEG C of powder fluid bed blast temperature.
Embodiment 2
1. by astaxanthin oil that 300g contents are 10%, 60g Rosmarinus officinalis extracts, 30g sucrose fatty esters in 55 DEG C of mixing
Stirring is obtained oil phase in 15 minutes to uniform.
2. 660g starch Sodium Octenyl Succinates, 900g glucose, 25g sodium ascorbates and 25g Tea Polyphenols are added
In 2.5kg pure water, 75 DEG C are stirred 30 minutes to being completely dissolved, and regulation pH value is obtained water phase to 7.8.
3. 55 DEG C of oil phase is added in the water phase in 75 DEG C of stirrings, continues to stir 30 minutes, then crossed sand mill and follow
Ring is processed 30 minutes, and sand mill rotating speed 2000rpm makes the emulsion particle particle diameter after grinding reach below 100nm, the emulsion for obtaining
Granulated with cold spray-starch fluid-bed drying, obtained astaxanthin micro-capsule, spray drying condition is：45 DEG C of EAT, forms sediment
60 DEG C of powder fluid bed blast temperature.
Embodiment 3
Astaxanthin oil that 6kg contents are 10%, 3kg natural VEs, 1.2kg polyglyceryl fatty acid esters is mixed in 55 DEG C 1.
Stirring is closed 30 minutes to uniform, and oil phase is obtained.
2. 17.2kg Arabic gums, 12.0kg hydroxyl isomaltuloses, 0.3kg sodium ascorbates and 0.3kg citric acids are added
In 40kg pure water, 75 DEG C are stirred 1 hour to being completely dissolved, and regulation pH value is obtained water phase to 7.6.
3. 55 DEG C of oil phase is added in the water phase in 75 DEG C of stirrings, continues to stir 30 minutes, then crossed sand mill and follow
Ring is processed 30 minutes, and sand mill rotating speed 2100rpm makes the emulsion particle particle diameter after grinding reach below 100nm, the emulsion for obtaining
Granulated with cold spray-starch fluid-bed drying, obtained astaxanthin micro-capsule, spray drying condition is：40 DEG C of EAT, forms sediment
60 DEG C of powder fluid bed blast temperature.
Embodiment 4：
1. astaxanthin oil, 0.3kg natural VEs and 0.3g Rosmarinus officinalis extracts, 0.9kg that 6kg contents are 10% are gathered
Oxygen ethene sorbitan fatty acid ester mixes 30 minutes in 50 DEG C to uniform, and oil phase is obtained.
2. by 12kg Arabic gums and 6kg starch Sodium Octenyl Succinates, 6kg hydroxyl isomaltuloses and 3.5kg glucose,
0.4kg sodium ascorbates and 0.4kg citric acids are added in 36kg pure water, and 50 DEG C are stirred 1 hour to being completely dissolved, and adjust pH value
To 7.5, water phase is obtained.
3. 50 DEG C of oil phase is added in the water phase in 50 DEG C of stirrings, continues to stir 30 minutes, then crossed sand mill and follow
Ring is processed 30 minutes, and sand mill rotating speed 2100rpm makes the emulsion particle particle diameter after grinding reach below 100nm, the emulsion for obtaining
Granulated with cold spray-starch fluid-bed drying, obtained astaxanthin micro-capsule, spray drying condition is：0 DEG C of EAT, forms sediment
70 DEG C of powder fluid bed blast temperature.
Embodiment 5：
1. by astaxanthin oil that 6kg contents are 10%, 1.5kg natural VEs, 1.5kg polyglyceryl fatty acid esters with
1.5kg sucrose fatty esters mix 30 minutes in 60 DEG C to uniform, and oil phase is obtained.
2. 12kg Arabic gums, 10.5kg hydroxyl isomaltuloses, 0.9kg sodium ascorbates and 0.9kg citric acids are added
In 60kg pure water, 80 DEG C are stirred 1 hour to being completely dissolved, and regulation pH value is obtained water phase to 8.0.
3. 60 DEG C of oil phase is added in the water phase in 80 DEG C of stirrings, continues to stir 30 minutes, then crossed sand mill and follow
Ring is processed 30 minutes, and sand mill rotating speed 2100rpm makes the emulsion particle particle diameter after grinding reach below 100nm, the emulsion for obtaining
Granulated with cold spray-starch fluid-bed drying, obtained astaxanthin micro-capsule, spray drying condition is：50 DEG C of EAT, forms sediment
80 DEG C of powder fluid bed blast temperature.
Product 1-5 is prepared by embodiment 1-5 respectively, its product index is as shown in table 1：
The astaxanthin micro-capsule product index testing result of table 1
Note：Content retention rate design conditions are：40 DEG C, RH75% place 6 months.
The present invention has been described in detail above by embodiment, but the content is only preferable implementation of the invention
Example, is designed using technical solutions according to the invention, or those skilled in the art under the inspiration of technical solution of the present invention
Similar technical scheme, and above-mentioned technique effect is reached, it is to fall into protection scope of the present invention.
Claims (2)
1. the preparation method of the molten natural astaxanthin microcapsule formulation of a kind of high stability cold water, it is characterised in that specific steps are such as
Under：
1）Prepared oil phase, institute are well mixed by astaxanthin oil, under the conditions of 50-60 DEG C of oil-soluble inhibitor and water soluble emulsifier
Oil-soluble inhibitor is stated for one or two in natural VE or Rosmarinus officinalis extract, addition is astaxanthin oil
The 10-50% of amount；HLB value >=13 of the water soluble emulsifier, addition is the 10-50% of astaxanthin oil quality；
2）Under the conditions of 50-80 DEG C, by wall material, water soluble antioxidant and filler addition pure water, stirring and dissolving is adjusted
PH value is obtained water phase to 7.5-8.0, and the wall material is one or two in Arabic gum or starch Sodium Octenyl Succinate,
Addition is 2-3 times of astaxanthin oil quality；The filler is the one kind or two in hydroxyl isomaltulose, sucrose or glucose
Kind, addition is 2-3 times of astaxanthin oil quality；The water soluble antioxidant is the mixing of sodium ascorbate and Tea Polyphenols
Thing, or sodium ascorbate and citric acid mixture, addition is 0.1-0.3 times of astaxanthin oil quality；The addition is pure
The quality of water is 6-10 times of astaxanthin oil quality；
3）Oil phase is added in water phase and is stirred, crossed sand mill and be ground, reach the emulsion particle particle diameter after grinding
Below 100nm, a step granulation is carried out by emulsion with cold spray-starch fluid-bed drying, obtains the ball that particle diameter is 40-100 mesh
Shape microcapsule formulation；The cold spray-starch fluid-bed drying condition is：Spraying EAT is 0-50 DEG C, starch fluid bed
Blast temperature is 60-80 DEG C.
2. the preparation method of the molten natural astaxanthin microcapsule formulation of a kind of high stability cold water according to claim 1, its
It is characterised by, the step 1）Middle water soluble emulsifier is polyglyceryl fatty acid ester, sucrose fatty ester, polyoxyethylene sorbitan mountain
Any one or a few in pears alcohol fatty acid ester；Addition is the 10-50% of astaxanthin oil quality.
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| CN107307403B (en) * | 2017-07-12 | 2021-01-01 | 日照职业技术学院 | Astaxanthin micro-nano solid preparation |
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| CN103406079B (en) * | 2013-06-28 | 2016-07-06 | 大连医诺生物有限公司 | Do not use the method that organic solvent prepares cold water dispersion type carotenoid micro-capsule powder |
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| CN104705654A (en) * | 2015-04-02 | 2015-06-17 | 徐权汉 | Preparation method for astaxanthin microcapsules |
| CN104856051B (en) * | 2015-04-10 | 2017-07-14 | 杭州鑫伟低碳技术研发有限公司 | A kind of method of utilization Haematococcus pluvialis production micro-capsule astaxanthin powder |
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