CN107296152A - Emulsion compositions containing 25 hydroxycholecalciferols and preparation method thereof - Google Patents
Emulsion compositions containing 25 hydroxycholecalciferols and preparation method thereof Download PDFInfo
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- CN107296152A CN107296152A CN201710740622.1A CN201710740622A CN107296152A CN 107296152 A CN107296152 A CN 107296152A CN 201710740622 A CN201710740622 A CN 201710740622A CN 107296152 A CN107296152 A CN 107296152A
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/174—Vitamins
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K40/00—Shaping or working-up of animal feeding-stuffs
- A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K50/00—Feeding-stuffs specially adapted for particular animals
- A23K50/30—Feeding-stuffs specially adapted for particular animals for swines
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K50/00—Feeding-stuffs specially adapted for particular animals
- A23K50/70—Feeding-stuffs specially adapted for particular animals for birds
- A23K50/75—Feeding-stuffs specially adapted for particular animals for birds for poultry
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Abstract
The invention discloses emulsion compositions containing 25 hydroxycholecalciferols and preparation method thereof, including the hydroxycholecalciferol of active component 25, lipophilic emulsifier, hydrophilic emulsifier, antioxidant, dispersed phase oil phase solvent and continuous phase aqueous phase solvent, the present invention is by optimizing emulsifier and ratio, adjust aqueous phase, the species and ratio of oil phase, prepare more stable oil-in-water emulsion formulation, product stability is good, it is easy to prepare, transport and storage, it is more applicable for industrial applications, emulsion prepared by this preparation method is able to maintain that preferable preparation stability, being scattered in drinking water for dosage can be determined, 25 hydroxycholecalciferols are made more to be conveniently applied in the feed of poultry and pig, it is used as the nutritious supplementary pharmaceutical of poultry and pig, improve its bone density or bone strength.
Description
Technical field
The invention belongs to animal health field, and in particular to emulsion compositions and its system containing 25-hydroxyvitamin D3
Preparation Method.
Background technology
Vitamin D (such as ergocalciferol D2 and cholecalciferol D3) is that one group defined by its bioactivity is fat-soluble
Compound, vitamin D can promote the re-absorption of bone, also cardiovascular, immune and muscle systems the function of controllable.Epidemiology is ground
Study carefully and be found that vitamin D intake and its to the association between blood pressure or glucose metabolism.The activity of vitamin D is by parathyroid hormone
The negative feedback control of element.Vitamin D deficiency causes rickets in children, and malacosteon is caused in adult.But it is slow in the several months
Property intake recommend daily allowance (i.e. 5~15 μ g or 200~600IU) vitamin Ds more than 100 times after may occur toxicity,
More than can occur hypercalcinemia under the blood concentration of 375nmol/L25 hydroxy-vitamine Ds.For vitamin D, toxicity threshold is
Daily 500~600mcg/kg body weight, adult generally should not consume three times more than RDA for a long time.In recent years, safe vitamin D
Upper limit level is accredited as at least 250 μ g/ days (10000IU), and the intake of such dietary supplements, which has been shown, to be caused about
The blood concentration of 200nmol/L25- hydroxycholecalciferols.
Vitamin D is a kind of prohormone, and it must produce 25-hydroxyvitamin D3 (25- in liver by hydroxylating
OHD3), it then undergoes other hydroxylating in kidney and its hetero-organization, produces the active hormone form of vitamin D --- and 1,25-
Dihydroxyvitamin D.1,25- dihydroxyvitamin D is released in blood, 1,25- dihydroxyvitamin D and vitamin D knot
Hop protein (DBP) is combined, and is transported to destination organization.Combination between 1,25- dihydroxyvitamin Ds and vitamin D receptor
Compound is allowed to play the effect of transcription factor in nucleus.For these reasons, it regard 25-hydroxyvitamin D3 as nutrition
Supplement is supplied to animal to be beneficial.
The composition of vitamin D and 25-hydroxyvitamin D3 is used in animal feed.Patent US2005/
0064018 discloses the combination that 25-hydroxyvitamin D3 and vitamine D3 are added to animal feed, to promote the bone strength of pig.
Specifically, added into pig feed the μ g/kg of about 10 μ g/kg~100 25-hydroxyvitamin D3 and about 200IU/kg~
4000IU/kg vitamine D3.Patent US5695794 is disclosed adds 25-hydroxyvitamin D3 and vitamin to poultry feed
D3 combination, to improve the influence of poultry tibial dyschondroplasia.Patent US5043170 discloses vitamine D3 and 1- α-hydroxyl
The combination of base cholecalciferol or 1 α, 25- hydroxyl cholecalciferol, in laying hens and old hen improve egg intensity and
Leg intensity.But it is under customary storage conditions and unstable to be directly added into the 25-hydroxyvitamin D3 in feed, during storage
It is easy to oxidation, this degraded has a negative impact to the dosage of the 25-hydroxyvitamin D3 in animal feed, thus needs to provide
Form is stabilized in extensive condition 25-hydroxyvitamin D3 composition.
Chinese patent CN1278690C discloses the composition containing 25-hydroxyvitamin D3, formulation include fluid composition,
Emulsion, microencapsulated oil composition.Wherein, its emulsion formulation is the state that microencapsulated oil composition is not spray-dried, its viscosity
It is very high, it is unfavorable for practical application.And 25-hydroxyvitamin D3 is unstable under conventional preparation condition, causes unit dose
Time dependence loss is presented in activity, especially at a higher temperature, and active component is easy to degraded, this during use
Degrade and have a negative impact to the dosage of 25-hydroxyvitamin D3.Chinese patent 201610070588.7 discloses boar use
The medium chain triglycerides cost of 80% composition described above composition is higher in quick-acting complementary energy B B-complex microemulsion preparations, composition,
Obtain to be water in oil microemulsion can produce during dilution use that demulsification causes is inconvenient for use, need to prevent during storage
Become sour, product stability is poor, the preparation, storage and traffic condition to product require harsher.
The content of the invention
One of the object of the invention is to provide the emulsion compositions containing 25-hydroxyvitamin D3, is used by optimizing emulsifying agent
Amount and ratio, adjust the species and ratio of oil phase, prepare more stable oil-in-water emulsion formulation, make 25- hydroxy vitamins
D3 is more conveniently applied in the feed of poultry and pig, improves its bone density or bone strength.
The two of the object of the invention are to provide the preparation method of the emulsion compositions containing 25-hydroxyvitamin D3, this preparation
Emulsion prepared by method is able to maintain that preferable preparation stability, can determine being scattered in drinking water for dosage, be used as poultry and pig
Nutritious supplementary pharmaceutical.
To achieve the above object, the present invention is adopted the following technical scheme that：
Emulsion compositions containing 25-hydroxyvitamin D3, are made up of the component of following mass percent：Active component
25-hydroxyvitamin D3 0.001~5%, antioxidant 0.5~1.5%, lipophilic emulsifier 2.0~2.8%, hydrophily breast
Agent 4.0~5.0%, dispersed phase oil phase solvent 5~10% and continuous phase aqueous phase solvent 65.0~90.0%.
By optimizing emulsifier and ratio, regulation aqueous phase, the species of oil phase and ratio prepare more stable water bag
Oil type emulsion dosage form, the process of 25-hydroxyvitamin D3 is diluted when using need to only be added to the water emulsion compositions of the present invention, directly
The change diluted without causing character outward appearance is connect, overcomes water-in-oil emulsion to produce demulsification in dilution and cause and use
The defect of inconvenience, it is easy-to-use.And the oil-in-water emulsifiers product stability of the present invention is good, be easy to prepare, transport and
Storage, is more applicable for industrial applications.The aqueous phase solvent of the present invention accounts for more than the 65% of composition quality, and cost advantage is not sayed
And explain.
It is preferred that, it is 10~11 that described emulsion compositions adjust its hydrophilic and oleophilic value (HLB) by emulsifying agent.
It is preferred that, the oil phase solvent is medium chain triglycerides, glycerin diacetate, glycerol triacetate, corn oil, sesame
Sesame oil, soya-bean oil, apricot kernel oil, peanut oil, persic oil, rapeseed oil, cottonseed oil, sunflower oil, castor oil, olive oil, hydrogenated castor
One or more in oil, coconut oil.
It is preferred that, the lipophilic emulsifier is Masine 35-1, ethylene glycol monostearate, ethylene glycol list oleic acid
The one or more of the pungent decylate of ester, glycerol tristearate, glyceryl monostearate, triglycerin.
It is preferred that, the hydrophilic emulsifier includes Tween-60, Tween-20, Tween-80, lauryl sodium sulfate, ten
The one or more of dialkyl group potassium sulfate, lauric isopropropanolamide.
It is preferred that, described antioxidant is 2,6- di-tert-butyl-4-methy phenols, ethylenediamine tetra-acetic acid, dibutyl hydroxyl
Base toluene, xylitol, fumaric acid, alpha-tocopherol, gentisic acid ethanolamine, ascorbic acid, sodium ascorbate, the one of gallic acid
Plant or a variety of.
It is preferred that, the 25-hydroxyvitamin D3 structural formula is as shown in Equation 1：
The present invention also provides a kind of preparation method of the emulsion compositions containing 25-hydroxyvitamin D3, including following step
Suddenly：
(1) prepared by oil phase：
Under 10~100 DEG C of water bath conditions, antioxidant is dissolved in oiliness dispersed phase, 5~60min is stirred, adds 25-
Hydroxycholecalciferol, stirs 5~60min；
(2) prepared by emulsifying agent：
Lipophilic emulsifier and hydrophilic emulsifier are well mixed；
(3) prepared by colostrum
Emulsifying agent prepared by step (2) is added in oil phase prepared by step (2), and stirring is allowed to be formed colostrum, and stirring 3~
30min, becomes colostrum；
(4) water process
Water is maintained and step (1) oil phase identical temperature under water bath condition, standby；
(5) prepared by emulsion
Colostrum prepared by step (3) is added in the water of step (4), is prepared using high-speed shearing equipment or other are even
Matter equipment prepares emulsion, and shear rate is set to 25000rpm, and the shearing suitable time prepares emulsion, and preparation is let cool to room after finishing
Temperature.
It is preferred that, each component and mass ratio are in the above-mentioned emulsion compositions preparation process containing 25-hydroxyvitamin D3：
It is preferred that, the emulsion is packaged as loading emulsion 1000ml white high-density polyethylene bottle, sealing.
It is preferred that, the condition of storage of the emulsion should be stored under conditions of less than 15 DEG C sealing lucifuges for composition, had
The effect phase is 12 months.
The present invention also provides the emulsion compositions containing 25-hydroxyvitamin D3 prepared by a kind of above-mentioned preparation method, breast
Liquid composition is oil-in-water emulsion, and character is milky white liquid, does not occur layering under 4000rpm15min centrifugal conditions existing
As.
It is preferred that, the mass percent of 25-hydroxyvitamin D3 is 0.001~5% in emulsion compositions.
The above-mentioned emulsion compositions for containing 25-hydroxyvitamin D3 answering as feed addictive is additionally provided in the present invention
With.
Relative to prior art, the beneficial effects of the invention are as follows：
(1) present invention is by optimizing emulsifier and ratio, and regulation aqueous phase, the species of oil phase and ratio are prepared more
Surely
Fixed oil-in-water emulsion formulation, product stability is good, is easy to prepare, transport and store, is more applicable for work
Industry
Using.
(2) process of dilution 25-hydroxyvitamin D3 only need to be by the present invention when emulsion compositions prepared by the present invention are used
Emulsion compositions are added to the water, and directly occur change of the dilution effect without causing character outward appearance, overcome water-in-oil emulsion to exist
Demulsification can be produced in dilution and awkward defect is caused, it is easy-to-use.
(3) aqueous phase solvent of the invention accounts for more than the 65% of composition quality, and cost advantage is self-evident.
(4) emulsion prepared by this preparation method is able to maintain that preferable preparation stability, can determine being scattered in for dosage and drink
In water, 25-hydroxyvitamin D3 is more conveniently applied in the feed of poultry and pig, be used as the nutritional supplementation of poultry and pig
Agent, improves its bone density or bone strength.
Embodiment
It is noted that described further below is all exemplary, it is intended to provide further instruction to the application.Unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in this manual using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
Term explains part：
Emulsion system, refers to immiscible two kinds of liquid mixing, wherein one is scattered in another phase liquid with drop state
The heterogeneous liquid preparation of formation, belongs to thermodynamic unstable system.In general emulsion is by aqueous phase, oil phase and emulsifying agent group
Into, water-in-oil type, oil-in-water type and complex emulsions can be divided into, wherein oil-in-water emulsion can cover the bad stink of medicine, and
Characteristic is diluted with good water, it is adaptable to the good active constituents of medicine of oil-soluble.
25-hydroxyvitamin D3 of the present invention, its information and physicochemical property are as shown in table 1 below
Table 1
| Title | 25-hydroxyvitamin D3 |
| Chemical name | (3β,5Z,7E)-9,10-secocholesta-5,7,10(19)-triene-3,25-diolmonahydrate |
| Molecular formula | C27H44O2· |
| Molecular weight | 400.66 |
| Fusing point | 100~120 DEG C |
| Character | White is to pink crystalline powder |
| Dissolubility | It is water insoluble, dissolve in acetonitrile, ethanol, DMSO and other organic solvents |
Embodiment 1：
Emulsion compositions constituent containing 25-hydroxyvitamin D3 is as shown in table 2：
Table 2
| Constituent | Recipe quantity/g | Prescription ratio/% | Effect |
| 25-hydroxyvitamin D3 | 1.584 | 0.176 | Active component |
| Medium chain triglyceride | 63.0 | 7.00 | Oil dephasing |
| 2,6 di tert butyl 4 methyl phenol | 9.0 | 1.00 | Antioxidant |
| Masine 35-1 | 21.9 | 2.44 | Lipophilic emulsifier |
| Tween-60 | 41.1 | 4.50 | Hydrophilic emulsifier |
| Water | 763.4 | 84.8 | Continuous phase |
| It is total | About 900g | 100 | -- |
The above-mentioned emulsion compositions containing 25-hydroxyvitamin D3 are prepared using following technical process：
1st, prepared by oil phase：
70 DEG C of bath temperatures are maintained using water-bath, medium chain triglycerides are added in beaker, detection temperature is to 70 DEG C；
Recipe quantity 2 is added thereto, and 6- di-tert-butyl-4-methy phenols are allowed to dissolve, mixing time using magnetic stirring equipment stirring
15min；Recipe quantity 25-hydroxyvitamin D3 is added, stirring is allowed to dissolve, mixing time 10min.
2nd, prepared by emulsifying agent
The Masine 35-1 and Tween-60 of recipe quantity are well mixed；
3rd, prepared by colostrum
Recipe quantity emulsifying agent is poured into oil phase, stirring is allowed to form colostrum, mixing time 5min；
4th, water process
Aqueous phase maintains 70 DEG C in a water bath, standby；
5th, prepared by emulsion
The colostrum of preparation is added in the water of recipe quantity, emulsion is prepared using high-speed shearing equipment, shear rate is set to
25000rpm, the shearing suitable time prepares emulsion, and preparation is let cool to room temperature after finishing
6th, pack
Above-mentioned emulsion is loaded to 1000ml white high-density polyethylene bottle, sealing.Less than 15 DEG C sealings should be stored in keep away
Under conditions of light, the term of validity is 12 months.
Product prepared by embodiment 1 has following formulation properties as shown in table 3：
Table 3
| Formulation properties | Case study on implementation 1 |
| Character | Milky white liquid |
| Appearance stability | 4000rpm15min centrifugations occur without layering |
| Density | ~1.00g/ml |
| pH | 5.50 |
| Loading amount | 900ml |
| Content | 0.176%w/w |
Embodiment 2
Emulsion compositions constituent containing 25-hydroxyvitamin D3 is as shown in table 4：
Table 4
The above-mentioned emulsion compositions containing 25-hydroxyvitamin D3 are prepared using following technical process：
1st, prepared by oil phase：
70 DEG C of bath temperatures are maintained using water-bath, medium chain triglycerides are added in beaker, detection temperature is to 70 DEG C；
Recipe quantity 2 is added thereto, and 6- di-tert-butyl-4-methy phenols are allowed to dissolve, mixing time using magnetic stirring equipment stirring
15min；Recipe quantity 25-hydroxyvitamin D3 is added, stirring is allowed to dissolve, mixing time 60min.
2nd, prepared by emulsifying agent
The Masine 35-1 and Tween-20 of recipe quantity are well mixed with beaker；
3rd, prepared by colostrum
Recipe quantity emulsifying agent is poured into oil phase, stirring is allowed to form colostrum, mixing time 5min；
4th, water process
Aqueous phase maintains 70 DEG C in a water bath, standby；
5th, prepared by emulsion
The colostrum of preparation is added in the water of recipe quantity, emulsion is prepared using high-speed shearing equipment, shear rate is set to
25000rpm, shear time is 15min, and preparation is let cool to room temperature after finishing
6th, pack
Above-mentioned emulsion is loaded to 1000ml white high-density polyethylene bottle, sealing.Less than 15 DEG C sealings should be stored in keep away
Under conditions of light, the term of validity is 12 months.
Product prepared by case study on implementation has following formulation properties as shown in table 5：
Table 5
| Formulation properties | Case study on implementation 2 |
| Character | Milky white liquid |
| Appearance stability | 4000rpm15min centrifugations occur without layering |
| Density | ~1.00g/ml |
| pH | 5.50 |
| Loading amount | 900ml |
| Content | 0.176%w/w |
Embodiment 3
Stability test：Sample prepared by case study on implementation 1 and case study on implementation 2 is placed on 25 DEG C, under conditions of 60%RH,
Investigate the items such as its content, character, pH.
Stability result is as shown in table 6：
Table 6
As a result show, case study on implementation 1 and case study on implementation 2 are respectively provided with good stability, accelerating 25 DEG C, 60%RH bar
Under part, 90 days stabilizations are placed.
Although the above-mentioned embodiment to the present invention is described, not to the limit of the scope of the present invention
System, one of ordinary skill in the art should be understood that on the basis of technical scheme those skilled in the art need not pay
Go out various modifications or deform still within protection scope of the present invention that creative work can make.
Claims (10)
1. the emulsion compositions containing 25-hydroxyvitamin D3, are made up of the component of following mass percent：Active component 25-
Hydroxycholecalciferol 0.001~5%, antioxidant 0.5~1.5%, lipophilic emulsifier 2.0~2.8%, hydrophilic emulsifier
Agent 4.0~5.0%, dispersed phase oil phase solvent 5~10% and continuous phase aqueous phase solvent 65.0~90.0%.
2. the emulsion compositions as claimed in claim 1 containing 25-hydroxyvitamin D3, it is characterised in that described emulsion
It is 10~11 that composition adjusts its hydrophilic and oleophilic value by emulsifying agent.
3. the emulsion compositions as claimed in claim 1 containing 25-hydroxyvitamin D3, it is characterised in that the oil phase is molten
Agent be medium chain triglycerides, glycerin diacetate, glycerol triacetate, corn oil, sesame oil, soya-bean oil, apricot kernel oil, peanut oil,
One or more in persic oil, rapeseed oil, cottonseed oil, sunflower oil, castor oil, olive oil, rilanit special, coconut oil.
4. the emulsion compositions as claimed in claim 1 containing 25-hydroxyvitamin D3, it is characterised in that the lipophile
Emulsifying agent is Masine 35-1, ethylene glycol monostearate, ethylene glycol monoleate, glycerol tristearate, glycerine list
The one or more of the pungent decylate of stearate, triglycerin.
5. the emulsion compositions as claimed in claim 1 containing 25-hydroxyvitamin D3, it is characterised in that the hydrophily
Emulsifying agent includes Tween-60, Tween-20, Tween-80, lauryl sodium sulfate, dodecyl sulphate potassium, laurate isopropanol
The one or more of acid amides.
6. the emulsion compositions as claimed in claim 1 containing 25-hydroxyvitamin D3, it is characterised in that described antioxygen
Agent be 2,6 di tert butyl 4 methyl phenol, ethylenediamine tetra-acetic acid, dibutyl hydroxy toluene, xylitol, fumaric acid,
Alpha-tocopherol, gentisic acid ethanolamine, ascorbic acid, sodium ascorbate, the one or more of gallic acid.
7. the preparation method of the emulsion compositions containing 25-hydroxyvitamin D3 as described in claim any one of 1-6, it is special
Levy and be, comprise the following steps：
(1) prepared by oil phase：
Under 10~100 DEG C of water bath conditions, antioxidant is dissolved in oiliness dispersed phase, 5~60min is stirred, adds 25- hydroxyls
Vitamine D3, stirs 5~60min；
(2) prepared by emulsifying agent：
Lipophilic emulsifier and hydrophilic emulsifier are well mixed；
(3) prepared by colostrum
Emulsifying agent prepared by step (2) is added in oil phase prepared by step (2), and stirring is allowed to be formed colostrum, and stirring 3~
30min, becomes colostrum；
(4) water process
Water is maintained and step (1) oil phase identical temperature under water bath condition, standby；
(5) prepared by emulsion
Colostrum prepared by step (3) is added in the water of step (4), is prepared using high-speed shearing equipment or other homogeneous set
Standby emulsion is prepared, shear rate is set to 25000rpm, and the shearing suitable time prepares emulsion, and preparation is let cool to room temperature after finishing.
8. the preparation method of the emulsion compositions as claimed in claim 7 containing 25-hydroxyvitamin D3, it is characterised in that
The terms of packing of the emulsion is sealing after the white high-density polyethylene bottle that emulsion is loaded to 1000ml；The condition of storage of emulsion
It should be stored under conditions of less than 15 DEG C sealing lucifuges for composition, the term of validity is 12 months.
9. the emulsion compositions containing 25-hydroxyvitamin D3 prepared by method as claimed in claim 7, emulsion compositions are water
Oil-in emulsion, character is milky white liquid, and lamination, emulsion compositions do not occur under 4000rpm15min centrifugal conditions
The mass percent of middle 25-hydroxyvitamin D3 is 0.001~5%.
10. application of the emulsion compositions of the 25-hydroxyvitamin D3 described in claim 9 in as feed addictive.
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| CN108383767A (en) * | 2018-02-06 | 2018-08-10 | 山东海能生物工程有限公司 | 25-hydroxvcholecalciferol monohydrate crystal and preparation method thereof and use its microemulsion |
| CN116158533A (en) * | 2023-03-20 | 2023-05-26 | 上海迦蓝海纳米技术集团有限公司 | Vitamin D easy to dissolve in water 3 Emulsion and method for producing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108383767A (en) * | 2018-02-06 | 2018-08-10 | 山东海能生物工程有限公司 | 25-hydroxvcholecalciferol monohydrate crystal and preparation method thereof and use its microemulsion |
| EP3750874A4 (en) * | 2018-02-06 | 2021-03-31 | Shandong Haineng Bioengineering Co., Ltd. | 25-HYDROXYCHOLECALCIFEROL MONOHYDRATE CRYSTAL AND METHOD FOR MANUFACTURING IT, AND MICROEMULSION WITH 25-HYDROXYCHOLECALCIFEROL MONOHYDRATE CRYSTAL |
| JP2021513567A (en) * | 2018-02-06 | 2021-05-27 | シャントン ハイネン バイオエンジニアリング カンパニー リミテッドＳｈａｎｄｏｎｇ Ｈａｉｎｅｎｇ Ｂｉｏｅｎｇｉｎｅｅｒｉｎｇ Ｃｏ．， Ｌｔｄ． | 25-Hydroxycholecalciferol monohydrate crystal, its production method and microemulsion using it |
| JP7072676B2 (en) | 2018-02-06 | 2022-05-20 | シャントン ハイネン バイオエンジニアリング カンパニー リミテッド | 25-Hydroxycholecalciferol monohydrate crystal, its production method and microemulsion using it |
| US11584713B2 (en) | 2018-02-06 | 2023-02-21 | Shandong Haineng Bioengineering Co., Ltd. | 25-hydroxycholecalciferol monohydrate crystal, preparation method therefor and microemulsion using same |
| CN116158533A (en) * | 2023-03-20 | 2023-05-26 | 上海迦蓝海纳米技术集团有限公司 | Vitamin D easy to dissolve in water 3 Emulsion and method for producing the same |
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