CN107496604A - A kind of camellia oil nanometer emulsion oral liquid and preparation method thereof - Google Patents

A kind of camellia oil nanometer emulsion oral liquid and preparation method thereof Download PDF

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CN107496604A
CN107496604A CN201710901690.1A CN201710901690A CN107496604A CN 107496604 A CN107496604 A CN 107496604A CN 201710901690 A CN201710901690 A CN 201710901690A CN 107496604 A CN107496604 A CN 107496604A
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camellia oil
oral liquid
parts
nanometer emulsion
oil
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陈岗宁
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Guizhou Yihang Ecological Agriculture And Animal Husbandry Science And Technology Development Co Ltd
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Guizhou Yihang Ecological Agriculture And Animal Husbandry Science And Technology Development Co Ltd
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Abstract

The invention belongs to medicine, food, health product technology field, more particularly to a kind of camellia oil nanometer emulsion oral liquid, it is made up of following mass parts raw material:Surfactant, cosurfactant, camellia oil, oil phase, aqueous phase;Camellia oil nanometer emulsion oral liquid outward appearance prepared by the present invention is homogeneous, and camellia oil nanometer emulsion oral liquid form is spheroidal under transmission electron microscope, is evenly distributed, average grain diameter 43nm.

Description

A kind of camellia oil nanometer emulsion oral liquid and preparation method thereof
Technical field
The invention belongs to medicine, food, health product technology field, more particularly to a kind of camellia oil nanometer emulsion oral liquid And preparation method thereof.
Background technology
Camellia oil is the distinctive oil tree in China, and yield is big, has original producton location advantage and trump-cards in the export of.It is rich in camellia oil The unrighted acid that contains, reach as high as more than 85%, in addition, rich in carrotene, vitamin, squalene, camellin, saponin(e, The active principles such as Tea Polyphenols, mineral matter, its vitamin E are several times of olive oil, and this is unnecessary in human body with regard to that can effectively reduce Cholesterol, prevent rubbish toxin from being deposited in vascular wall, and powerful antioxidant vitamin E can keep blood vessel elasticity, throughout the year Eat camellia oil and can substantially reduce cardiovascular and cerebrovascular diseases risk, strengthen internal system function, camellia oil can improve organism Metabolic function.Result of study shows that after Healthy People eats camellia oil, internal glucose content can reduce by 12%.Institute The best edible oil for preventing and controlling diabetes is turned into current camellia oil.In addition, camellia oil has anti-oxidant, antitumor, drop The effects such as blood pressure, hypoglycemic, anti-inflammatory, antibacterial, promotion percutaneous drug absorption, anti-obstructive jaundice and protect liver, can be used as nutrition food With, regulation immunologic function, preventing and treating obesity, Recovery, prevention of cardiovascular disease and cutaneous diseases etc..
Because camellia oil is in thick, not only sensory effects are poor, and its particle diameter is big, and dispersive property in media as well is poor, no Beneficial to being absorbed by the body, its development and application in food, cosmetic field greatly limit.In order to improve camellia oil-dispersing property, Be prepared into microemulsion, but emulsion intercalation method can be poor, be easily delaminated after standing for a long time, be equally difficult to improvement camellia oil Dispersiveness, thus cause to camellia oil absorption difference, cause the waste of product.
The content of the invention
The present invention is in order to solve the above technical problems, provide a kind of camellia oil nanometer emulsion oral liquid and preparation method thereof.
Realized particular by following technical scheme:
A kind of camellia oil nanometer emulsion oral liquid, it is made up of following mass parts raw material:Surfactant 30-60 parts, help surface Activating agent 0.5-20 parts, camellia oil 0.1-15 parts, oil phase 1-10 parts, aqueous phase 20-70 parts.
Further, described camellia oil nanometer emulsion oral liquid, it is made up of following mass parts raw material:Surfactant 57-60 Part, cosurfactant 3-7 parts, camellia oil 7-12 parts, oil phase 7-9 parts, aqueous phase 50-55 parts.
Further, described surfactant, be castor oil polyoxyethylene ether, rilanit special APEO, tween- 80 according to mass ratio 31.3-32.7:18.6-19:3.5-4.2 mix.
Further, described cosurfactant, it is according to quality by PEG-4000, glycerine, n-butanol, ethanol Compare 3.7-4.5:1-2:0.8-1.3:7-10 is mixed.
Further, described oil phase, it is one kind or several in vitamin E oil, wheat-germ oil, olive oil, jojoba oil Kind.
Further, described aqueous phase, including following mass parts raw material:Hawthorn 30-33 parts, Momordica grosvenori 20-23 parts, spirit Sesame 17-20 parts, pawpaw 10-14 parts, glutinous rice root 7-10 parts.
Further, described aqueous phase, including following preparation process:
1) hawthorn, Momordica grosvenori, ganoderma lucidum, pawpaw, glutinous rice root co-grinding, addition mixed liquor 1, it is 50- that water content, which is made, 70% compound, 40-55 DEG C stands 40-55min, is fermented 3-4 days at 30-35 DEG C, obtains fermentation material, adds 3-4 times of fermentation material The clear water of quality, 80-90 DEG C of refluxing extraction 3-4h, obtains extract solution 1;
2) alkali lye of the 1/3-1/4 times of mass of extract solution 1 is added, 40-50r/min stirring 30-50min, filtering, obtains filtrate 1;
3) ethanol of the 1/2-1/3 times of volume of filtrate 1 is added, 2-8 DEG C of standing 12-14h, filtering, obtains filtrate 2;
4) reduced-pressure backflow of filtrate 2 recovery ethanol, obtains residual solution, adds the deionized water mixing of 4-7 times of residual solution quality, both ;
Wherein, described mixed liquor 1, is the mixed liquor of cellulase, pectase, and concentration is respectively 0.03-0.1mol/L And 0.05-0.07mol/L;
Wherein, described alkali lye is 0.5-0.7mol/L sodium hydroxide solution.
Further, described camellia oil nanometer emulsion oral liquid, including following preparation process:
1) surfactant, cosurfactant are weighed in proportion, and 50-55 DEG C is stirred, and obtains material 1;
2) oil phase mixes, and obtains material 2;
3) 20-25 DEG C, material 2, aqueous phase are added drop-wise in material 1 under the conditions of 33-40r/min, stir 2-3h, 10-12 DEG C of standing 2-3h, 18-22 DEG C, 10-20r/min stirrings 70-80min both.
Further, the particle diameter of camellia oil nanometer emulsion oral liquid is in 10-100nm.
Beneficial effects of the present invention:Camellia oil nanometer emulsion oral liquid outward appearance prepared by the present invention is homogeneous, transmission electron microscopy Camellia oil nanometer emulsion oral liquid form is spheroidal under mirror, is evenly distributed, average grain diameter 43nm, thermostatic accelerated experiment, Qiang Guang Exposure experiment shows, camellia oil nanometer emulsion oral liquid in -4 DEG C, 40 DEG C, 60 DEG C and relative humidity under 75% after 5d, 10d Still uniformly, without lamination, camellia oil nanometer emulsion oral liquid also keeps uniform, existing without layering after 10000r/imn centrifuges 5min As.
Further carry out rat model, the results showed that camellia oil nanometer emulsion oral liquid prepared by the present invention can be effective The blood pressure for reducing rat is controlled in normal range (NR).
Embodiment
The embodiment of the present invention is described in further detail below, but the invention is not limited in these realities Mode is applied, any improvement or replacement on the present embodiment essence spirit, it is claimed to still fall within the claims in the present invention Scope.
Embodiment 1
A kind of camellia oil nanometer emulsion oral liquid, it is made up of following mass parts raw material:Surfactant 57g, help surface-active Agent 3g, camellia oil 7g, oil phase 7g, aqueous phase 50g.
Described surfactant, be castor oil polyoxyethylene ether, rilanit special APEO, Tween-80 according to Mass ratio 31.3:18.6:3.5 mix.
Described cosurfactant, it is according to mass ratio 3.7 by PEG-4000, glycerine, n-butanol, ethanol: 1:0.8:7 mix.
Described oil phase, it is that vitamin E oil, wheat-germ oil, olive oil, jojoba oil mix in equal volume.
Described aqueous phase, including following mass parts raw material:Hawthorn 30g, Momordica grosvenori 20g, ganoderma lucidum 17g, pawpaw 10g, Glutinous rice root 7g.
Described aqueous phase, including following preparation process:
1) hawthorn, Momordica grosvenori, ganoderma lucidum, pawpaw, glutinous rice root co-grinding, addition mixed liquor 1, it is 50% that water content, which is made, Compound, 40 DEG C stand 40min, are fermented 3 days at 30 DEG C, obtain fermentation material, add the clear water of 3 times of fermentation material quality, 80 DEG C of backflows 3h is extracted, obtains extract solution 1;
2) alkali lye of 1/3 times of mass of extract solution 1 is added, 40r/min stirring 30min, filtering, obtains filtrate 1;
3) ethanol of 1/2 times of volume of filtrate 1 is added, 2 DEG C of standing 12h, filtering, obtains filtrate 2;
4) reduced-pressure backflow of filtrate 2 recovery ethanol, obtains residual solution, adds the deionized water mixing of 4 times of residual solution quality, both ;
Wherein, described mixed liquor 1, is the mixed liquor of cellulase, pectase, concentration be respectively 0.03mol/L and 0.05mol/L;
Wherein, described alkali lye is 0.5mol/L sodium hydroxide solution.
Described camellia oil nanometer emulsion oral liquid, including following preparation process:
1) surfactant, cosurfactant are weighed in proportion, and 50 DEG C are stirred, and obtain material 1;
2) oil phase mixes, and obtains material 2;
3) 20 DEG C, material 2, aqueous phase are added drop-wise in material 1 under the conditions of 33r/min, stir 2h, 10 DEG C stand 2h, 18 DEG C, 10r/ Min stirrings 70min was both obtained.
The particle diameter of camellia oil nanometer emulsion oral liquid is in 10-100nm.
Embodiment 2
A kind of camellia oil nanometer emulsion oral liquid, it is made up of following mass parts raw material:Surfactant 58g, help surface-active Agent 5g, camellia oil 10g, oil phase 8g, aqueous phase 53g.
Described surfactant, be castor oil polyoxyethylene ether, rilanit special APEO, Tween-80 according to Mass ratio 31.8:18.8:3.7 mix.
Described cosurfactant, it is according to mass ratio 4.0 by PEG-4000, glycerine, n-butanol, ethanol: 1.5:1.0:8 mix.
Described oil phase, it is that vitamin E oil, wheat-germ oil, olive oil mix in equal volume.
Described aqueous phase, including following mass parts raw material:Hawthorn 31g, Momordica grosvenori 21v, ganoderma lucidum 18g, pawpaw 12g, Glutinous rice root 8g.
Described aqueous phase, including following preparation process:
1) hawthorn, Momordica grosvenori, ganoderma lucidum, pawpaw, glutinous rice root co-grinding, addition mixed liquor 1, it is 60% that water content, which is made, Compound, 50 DEG C stand 5min, are fermented 3.4 days at 33 DEG C, obtain fermentation material, add the clear water of 3.4 times of fermentation material quality, and 85 DEG C are returned Stream extraction 3.4h, obtains extract solution 1;
2) alkali lye of 1/4 times of mass of extract solution 1 is added, 45r/min stirring 40min, filtering, obtains filtrate 1;
3) ethanol of 1/3 times of volume of filtrate 1 is added, 6 DEG C of standing 13h, filtering, obtains filtrate 2;
4) reduced-pressure backflow of filtrate 2 recovery ethanol, obtains residual solution, adds the deionized water mixing of 5 times of residual solution quality, both ;
Wherein, described mixed liquor 1, is the mixed liquor of cellulase, pectase, concentration be respectively 0.07ol/L and 0.06mol/L;
Described alkali lye is 0.6mol/L sodium hydroxide solution.
Described camellia oil nanometer emulsion oral liquid, including following preparation process:
1) surfactant, cosurfactant are weighed in proportion, and 53 DEG C are stirred, and obtain material 1;
2) oil phase mixes, and obtains material 2;
3) 22 DEG C, material 2, aqueous phase are added drop-wise in material 1 under the conditions of 37r/min, stir 2.3h, 11 DEG C of standing 2.3h, 20 DEG C, 15r/min stirrings 75min was both obtained.
The particle diameter of camellia oil nanometer emulsion oral liquid is in 10-100nm.
Embodiment 3
A kind of camellia oil nanometer emulsion oral liquid, it is made up of following mass parts raw material:Surfactant 60g, help surface-active Agent 7g, camellia oil 12g, oil phase 9g, aqueous phase 55g.
Described surfactant, be castor oil polyoxyethylene ether, rilanit special APEO, Tween-80 according to Mass ratio 32.7:19:4.2 mix.
Described cosurfactant, it is according to mass ratio 4.5 by PEG-4000, glycerine, n-butanol, ethanol: 2:1.3:10 mix.
Described oil phase, it is that wheat-germ oil, jojoba oil mix in equal volume.
Described aqueous phase, including following mass parts raw material:Hawthorn 33g, Momordica grosvenori 23g, ganoderma lucidum 20g, pawpaw 14g, Glutinous rice root 10g.
Described aqueous phase, including following preparation process:
1) hawthorn, Momordica grosvenori, ganoderma lucidum, pawpaw, glutinous rice root co-grinding, addition mixed liquor 1, it is 70% that water content, which is made, Compound, 55 DEG C stand 55min, are fermented 4 days at 35 DEG C, obtain fermentation material, add the clear water of 4 times of fermentation material quality, 90 DEG C of backflows 4h is extracted, obtains extract solution 1;
2) alkali lye of 1/4 times of mass of extract solution 1 is added, 50r/min stirring 50min, filtering, obtains filtrate 1;
3) ethanol of the 1/2-1/3 times of volume of filtrate 1 is added, 2-8 DEG C of standing 12-14h, filtering, obtains filtrate 2;
4) reduced-pressure backflow of filtrate 2 recovery ethanol, obtains residual solution, adds the deionized water mixing of 7 times of residual solution quality, both ;
Wherein, described mixed liquor 1, is the mixed liquor of cellulase, pectase, concentration be respectively 0.1mol/L and 0.07mol/L;
Described alkali lye is 0.7mol/L sodium hydroxide solution.
Described camellia oil nanometer emulsion oral liquid, including following preparation process:
1) surfactant, cosurfactant are weighed in proportion, and 55 DEG C are stirred, and obtain material 1;
2) oil phase mixes, and obtains material 2;
3) 25 DEG C, material 2, aqueous phase are added drop-wise in material 1 under the conditions of 40r/min, stir 3h, 12 DEG C stand 3h, 22 DEG C, 20r/ Min stirrings 80min was both obtained.
The particle diameter of camellia oil nanometer emulsion oral liquid is in 10-100nm.
Embodiment 4
The difference of embodiment 4 and embodiment 3 is to be formulated, the surfactant of embodiment 4 be castor oil polyoxyethylene ether, Rilanit special APEO, Tween-80 are according to mass ratio 1:1:1 mixes, and preparation method is identical.
Embodiment 5
The difference of embodiment 5 and embodiment 3 is, the cosurfactant of embodiment 5 is by PEG-4000, the third three The mass mixings such as alcohol, n-butanol, ethanol form, and preparation method is identical.
Embodiment 6
The difference of embodiment 6 and embodiment 3 is that the aqueous phase in embodiment 6 is deionized water, and preparation method is identical.
Embodiment 7
The difference of embodiment 7 and embodiment 3 is, the aqueous phase of embodiment 7 is by hawthorn, Momordica grosvenori, ganoderma lucidum, pawpaw, glutinous Rice root co-grinding, add 4 times of clear water and decoct 3-6h, filter and obtain.
Embodiment 8
The difference of embodiment 8 and embodiment 3 is that preparation process when prepared by embodiment 8 is as follows:
1) surfactant, cosurfactant are weighed in proportion, and 55 DEG C are stirred, and obtain material 1;
2) oil phase mixes, and obtains material 2;
3) 25 DEG C, material 2, aqueous phase are added drop-wise in material 1 under the conditions of 40r/min, stir 3.5h, both.
Experimental example
1st, camellia oil nanometer emulsion oral liquid stability test
1) the camellia oil nanometer emulsion oral liquid 0.lmL prepared by Example 1-8, after 10 times of dilution, by 2% phosphotungstic acid Dyeing, observes its form under transmission electron microscope after sample drying, separately takes camellia oil nanometer emulsion oral liquid 20mL, uses 5 times of distilled water diluting, its particle diameter is determined with laser granulometry.
2) thermostatic accelerated experiment:Take camellia oil nanometer emulsion oral liquid in -4 DEG C, 40 DEG C, 60 DEG C and relative humidity 75% Under the conditions of preserve, after 5d, 10d, sampling observation camellia oil nanometer emulsion oral liquid outward appearance, take the camellia oil nanometer emulsion mouth Liquid is taken in centrifuge tube, 10000r/min centrifugation 5min, observes camellia oil nanometer emulsion oral liquid.
3) strong illumination is tested:Camellia oil nanometer emulsion oral liquid is placed under 2,000 1 40001x illumination, 5d, 10d Determine the stability of camellia oil nanometer emulsion oral liquid.
Experimental result:By above stability test result, camellia oil nanometer emulsion mouth that embodiment 1,2,3,6,7 is prepared It is homogeneous to take liquid outward appearance, camellia oil nanometer emulsion oral liquid form is spheroidal under transmission electron microscope, is evenly distributed, average grain diameter For 43nm, thermostatic accelerated experiment, strong illumination experiment show that camellia oil nanometer emulsion oral liquid is in -4 DEG C, 40 DEG C, 60 DEG C and phase To humidity under 75% after 5d, 10d still uniformly, centrifuged through 10000r/imn without lamination, camellia oil nanometer emulsion oral liquid Also kept uniformly, without lamination after 5min.
Because prepared by embodiment 4 and the surfactant used in embodiment 5, cosurfactant difference, embodiment 8 Method is different, so as to cause camellia oil nanometer emulsion oral liquid prepared by these three embodiments after 10000r/imn centrifuges 5min, There is layering, the inhomogenous phenomenon of emulsion.
2nd, influence experiment of the camellia oil nanometer emulsion oral liquid to rat blood pressure and heart rate
Method (Wu Xujin, the preparation of Zhu's Xiao Pu perilla oil nano-emulsions and its to Hypertensive Rats of reference literature report Influence [J] the China Veterinary Journal of blood pressure and heart rate, 2010,46,28-29.) measure camellia oil nanometer prepared by embodiment 1-8 Newborn oral liquid, control group application number CN201310230698.1 (camellia oil microemulsion and preparation method thereof) are to rats blood pressure Influence.
By SD rats 130,13 groups are randomly divided into, every group 10, male and female half and half, is divided into normal group (normal feeding), mould Type group (gavaging physiological saline 2.5g/kg daily), blank nano-emulsion group (gavaging blank nano-emulsion 2.25g/kg daily), embodiment 1-8 groups (gavage purple camellia oil nanometer emulsion oral liquid 2.25g/kg) daily, and control group (gavages camellia oil microemulsion 2.25g/ daily Kg), positive controls (gavaging Bezoar pill for lowering blood pressure 0.12g/kg daily), after successive administration 15d, measurement each group rat tail artery is received The change of contractive pressure and heart rate.Minute schedules 8:00-9:00.Cardiac index is represented with cardiac weight (mg)/body weight (g) ratio, As a result it is as shown in table 1.
Influence of the camellia oil nanometer emulsion oral liquid of table 1 to hypertensive rat blood pressure, heart rate and cardiac index
Group Blood pressure (mmHg) Heart rate (secondary/min) Cardiac index
Normal group 112±8 386±9 3.11±0.15
Model group 162±7 342±6 3.85±0.17
Blank nano-emulsion group 161±5 340±9 3.82±0.14
Embodiment 1 110±7 380±8 3.10±0.16
Embodiment 2 111±4 379±8 3.08±0.11
Embodiment 3 108±5 380±3 3.09±0.06
Embodiment 4 121±4 399±7 3.13±0.22
Embodiment 5 130±6 401±3 3.14±0.17
Embodiment 6 135±5 403±8 3.15±0.21
Embodiment 7 130±8 400±2 3.14±0.15
Embodiment 8 115±7 384±9 3.11±0.13
Control group 121±8 394±7 3.12±0.16
Positive controls 110±6 390±8 3.10±0.16
It is demonstrated experimentally that camellia oil nanometer emulsion oral liquid prepared by the present invention can effectively reduce the blood of rat more than Pressure reaches normal range (NR), suitable with the effect of comparison medicine Bezoar pill for lowering blood pressure.

Claims (9)

1. a kind of camellia oil nanometer emulsion oral liquid, it is characterised in that be made up of following mass parts raw material:Surfactant 30-60 Part, cosurfactant 0.5-20 parts, camellia oil 0.1-15 parts, oil phase 1-10 parts, aqueous phase 20-70 parts.
2. camellia oil nanometer emulsion oral liquid as claimed in claim 1, it is characterised in that described camellia oil nanometer emulsion is oral Liquid, it is made up of following mass parts raw material:Surfactant 57-60 parts, cosurfactant 3-7 parts, camellia oil 7-12 parts, oil phase 7-9 parts, aqueous phase 50-55 parts.
3. camellia oil nanometer emulsion oral liquid as claimed in claim 1, it is characterised in that described surfactant, be castor-oil plant Oily APEO, rilanit special APEO, Tween-80 are according to mass ratio 31.3-32.7:18.6-19:3.5-4.2 Mix.
4. camellia oil nanometer emulsion oral liquid as claimed in claim 1, it is characterised in that described cosurfactant, be by PEG-4000, glycerine, n-butanol, ethanol are according to mass ratio 3.7-4.5:1-2:0.8-1.3:7-10 is mixed.
5. camellia oil nanometer emulsion oral liquid as claimed in claim 1, it is characterised in that described oil phase, be vitamin E oil, One or more in wheat-germ oil, olive oil, jojoba oil.
6. camellia oil nanometer emulsion oral liquid as claimed in claim 1, it is characterised in that described aqueous phase, including it is following Mass parts raw material:Hawthorn 30-33 parts, Momordica grosvenori 20-23 parts, ganoderma lucidum 17-20 parts, pawpaw 10-14 parts, glutinous rice root 7-10 parts.
7. camellia oil nanometer emulsion oral liquid as claimed in claim 1, it is characterised in that described aqueous phase, including following preparation Step:
1) hawthorn, Momordica grosvenori, ganoderma lucidum, pawpaw, glutinous rice root co-grinding, addition mixed liquor 1, it is 50-70%'s that water content, which is made, Compound, 40-55 DEG C stands 40-55min, is fermented 3-4 days at 30-35 DEG C, obtains fermentation material, 3-4 times of fermentation material quality of addition Clear water, 80-90 DEG C of refluxing extraction 3-4h, obtains extract solution 1;
2) alkali lye of the 1/3-1/4 times of mass of extract solution 1 is added, 40-50r/min stirring 30-50min, filtering, obtains filtrate 1;
3) ethanol of the 1/2-1/3 times of volume of filtrate 1 is added, 2-8 DEG C of standing 12-14h, filtering, obtains filtrate 2;
4) reduced-pressure backflow of filtrate 2 recovery ethanol, obtains residual solution, adds the deionized water mixing of 4-7 times of residual solution quality, both;
Wherein, described mixed liquor 1, is the mixed liquor of cellulase, pectase, concentration be respectively 0.03-0.1mol/L and 0.05-0.07mol/L;
Wherein, described alkali lye is 0.5-0.7mol/L sodium hydroxide solution.
8. camellia oil nanometer emulsion oral liquid as claimed in claim 1, it is characterised in that including following preparation process:
1) surfactant, cosurfactant are weighed in proportion, and 50-55 DEG C is stirred, and obtains material 1;
2) oil phase mixes, and obtains material 2;
3) 20-25 DEG C, material 2, aqueous phase are added drop-wise in material 1 under the conditions of 33-40r/min, stir 2-3h, 10-12 DEG C of standing 2-3h, 18-22 DEG C, 10-20r/min stirrings 70-80min both.
9. camellia oil nanometer emulsion oral liquid as claimed in claim 1, it is characterised in that the particle diameter of camellia oil nanometer emulsion oral liquid In 10-100nm.
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