CN105746730A - Nano-emulsion containing vitamin D and linseed oil as well as preparation method and application of nano-emulsion - Google Patents

Nano-emulsion containing vitamin D and linseed oil as well as preparation method and application of nano-emulsion Download PDF

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Publication number
CN105746730A
CN105746730A CN201610096942.3A CN201610096942A CN105746730A CN 105746730 A CN105746730 A CN 105746730A CN 201610096942 A CN201610096942 A CN 201610096942A CN 105746730 A CN105746730 A CN 105746730A
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China
Prior art keywords
nanoemulsions
linseed oil
vitamin
oil
nano
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CN201610096942.3A
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Chinese (zh)
Inventor
高山
李宏
岳昌林
钟己未
刘楠
郑攀
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ZHEJIANG JIUXU PHARMACEUTICAL CO Ltd
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ZHEJIANG JIUXU PHARMACEUTICAL CO Ltd
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Priority to CN201610096942.3A priority Critical patent/CN105746730A/en
Publication of CN105746730A publication Critical patent/CN105746730A/en
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/007Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • A23D9/04Working-up
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Edible Oils And Fats (AREA)
  • Medicinal Preparation (AREA)

Abstract

The invention relates to a nano-emulsion prepared from vitamin D and linseed oil as well as a preparation method and application of the nano-emulsion. The nano-emulsion is prepared from the following raw materials by mass percent: 0.02-1% of the vitamin D, 1-10% of the linseed oil, 0.5-3% of an emulsifying agent, 0.005-0.5% of an antioxidant, 0.005-0.5% of a preservative and the balance of water. The vitamin D and the linseed oil are prepared into nanoparticles by the food grade emulsifying agent, a proper dosage of the emulsifying agent and an appropriate PH value are determined, and granulation is realized by a two-step method, so that the problems that the vitamin D and the linseed oil are easily oxidized, and emulsion particles are poor in stability can be effectively solved.

Description

A kind of nanoemulsions containing vitamin D linseed oil and preparation method and application
Technical field
The present invention relates to a kind of nanoemulsions containing vitamin D linseed oil and preparation method thereof With application, belong to health care of food product technical field.
Background technology
Linseed oil, also known as linseed oil or siritch, is the drying oil produced from linseed. Linseed oil contains special nutritional labeling, especially contains alpha-linolenic acid and is up to more than 50%, tool There are important physiological function and high nutritive value.
Vitamin D is steroid derivative, has anti-rachitic effect, raw also known as rickets dimension Element.It is now recognized that vitamin D is also a kind of steroid hormone, in vitamin D family member Important member is VD2 (ergocalciferol) and VD3 (Vitamin D3).
In the prior art, vitamine D3 is as a kind of liposoluble vitamin, and its solubility is low, And processing and storage condition such as light, temperature and oxygen etc. all can cause its isomerization or oxidation, Its chemical constitution and physiological function are adversely affected, also reduces the biology of active material simultaneously Utilization rate.It addition, vitamine D3 solubility is low, adds in food system and often occur A series of problem, adversely affects flavour of food products, product stability, product appearance, Add vitamine D3 difficulty in food processing process, limit answering at field of food With.
Summary of the invention
It is an object of the invention to provide a kind of nanoemulsions containing vitamin D linseed oil, pass through Use food grade emulsifier that vitamin D and linseed oil are made nanoparticle, determine appropriate Emulsifier, suitable pH value, use two-step method to pelletize, thus it is raw to efficiently solve dimension Element D linseed oil is oxidizable, the problem of breast grain poor stability.
To achieve these goals, the present invention adopts the following technical scheme that
A kind of nanoemulsions containing vitamin D linseed oil, by the raw material of following mass percent Prepare: vitamin D 0.02%-1%, linseed oil 1%-10%, emulsifying agent 0.5%-3%, anti- Oxidant 0.005%-0.5%, preservative 0.005%-0.5%, surplus is water.
It is further preferred that the described nanoemulsions containing vitamin D linseed oil, by following matter The raw material of amount percentage prepares: vitamin D 0.2-0.8%, linseed oil 2-6%, emulsifying agent 0.8-1.5%, antioxidant 0.01-0.2%, preservative 0.01-0.2%, surplus is water.
The more preferably described nanoemulsions containing vitamin D linseed oil, by following mass percent Raw material prepare: vitamin D 0.2%-0.4%, linseed oil 5%, emulsifying agent 0.8%-1.2%, Antioxidant 0.01%-0.02%, preservative 0.01%-0.02%, surplus is water.
Described emulsifying agent is selected from soybean lecithin or yolk phospholipid.
Described antioxidant is selected from ascorbyl palmitate, butylated hydroxy anisole, dibutyl hydroxyl One or more in base toluene, propylgallate, tert-butylhydroquinone or tocopherol.
Described preservative is selected from ethyl-para-hydroxybenzoate, Sodium Benzoate or potassium sorbate Plant or multiple.
In order to make nanoemulsions meet the demand of some special populations, also can in emulsion suitably Add sweet flavouring (such as glucose, xylitol etc.), osmotic pressure regulator (such as glycerine) with And thickener (such as carragheen, pectin etc.).
Additionally, in order to preferably promote that vitamin D dissolves, also can be at linseed oil in the application Middle addition vegetable oil (such as corn oil, soybean oil etc.) is configured to miscella, to improve further The dissolubility of vitamin D.Wherein, vegetable oil is 1-2:1 with the volume ratio of linseed oil.
The gained of the present invention nanoemulsions containing vitamin D linseed oil can be good at protection dimension Raw element D, linseed oil affect from undesirable element in environment.Gained nanoemulsions particle diameter is less than 800nm, even less than 600nm, pH is 5.5-8.3, preferably 6-8.3, and Zeta potential is at-36.75V ~between-13.93.It has been investigated that, Zeta potential absolute value is the highest, and emulsion system is the most stable, And less particle can improve bioavilability, there is good applicability simultaneously, permissible Arbitrarily dissolve each other with milk, beverage etc., facilitate old man to take with child.
The present invention also provides for the preparation method of a kind of nanoemulsions containing vitamin D linseed oil, Comprise the steps:
1) prepare aqueous phase: added by emulsifying agent in alkaline water, under nitrogen protection, shear to dividing Dissipate uniformly;
2) oil phase is prepared: add in linseed oil by vitamin D, antioxidant, preservative, Add thermal agitation, mixing;
3) oil phase is added in aqueous phase, shear and make colostrum, regulation system pH value to 5.5~8.3, Preferably 6~8.3;
4) use gradient boost mode to carry out high-pressure homogeneous to colostrum, prepare nanoemulsions.
In the preparation method of nanoemulsions of the present invention, step 1) in, described water also may be used Add suitable additives, the sweetest flavouring (such as glucose, xylitol etc.), osmotic pressure Conditioning agent (such as glycerine) and thickener (such as carragheen, pectin etc.).Described shearing water temperature Control at 50~60 DEG C.In this step, the pH value of described alkaline water is between 8-12.
In the preparation method of nanoemulsions of the present invention, step 2) in, described whipping temp Control at 40~50 DEG C.Additionally, in order to preferably promote that vitamin D dissolves, also can be in flax Seed oil adds vegetable oil (such as corn oil, soybean oil etc.) and is configured to miscella, with further Improve the dissolubility of vitamin D.Wherein, vegetable oil is 1-2:1 with the volume ratio of linseed oil.
In the preparation method of nanoemulsions of the present invention, step 4) in, described gradient boost Process particularly as follows: first carry out 200~400bar low pressure recycle, its objective is particle diameter bigger Particle pulverize, prevent under high pressure damaging high pressure homogenizer;The most again 500~ 700bar cycle of higher pressure processes, and its objective is to increase the stability of breast grain.Described homogeneous processes Temperature control at 40~60 DEG C.
Present invention also offers described containing vitamin D linseed oil nanoemulsions food, Application in field of health care products.According to actual demand, can be made in food and field of health care products Conventional formulation, such as oral liquid etc..
Vitamin D and the most water insoluble solution of linseed oil, but the present invention is a small amount of single by adding Linseed oil containing vitamin D is dispersed in water by one emulsifying agent, forms a kind of oil-in-water and divides Prose style free from parallelism system;By control solution pH value between 6.0-8.3, use two-step method to pelletize, make particulate Electrically charged amount increases, and prepares degree of stability higher vitamin D linseed oil nanoemulsions.Should Method is simple to operate, and resulting dosage forms drugloading rate is relatively big, and bioavilability is high.
Gained vitamin D linseed oil nanoemulsions of the present invention provides human body two kinds useful simultaneously Replenishers, can directly be absorbed by the mucous membrane such as oral cavity, nasal cavity, thus increase substantially human body pair The absorption of vitamin D linseed oil, is primarily adapted for use in and needs vitamin D, DHA and EPA Crowd, the elderly especially failed metabolic function and metabolic function are grown the completeest Kind infant becomes apparent from.
Detailed description of the invention
Following example are used for illustrating the present invention, but are not limited to the scope of the present invention.
1 one kinds of vitamin D linseed oil nanoemulsions of embodiment
The present embodiment provides a kind of nanoemulsions containing vitamin D linseed oil, and its formula is (being calculated in mass percent): vitamin D 0.4%, linseed oil 5%, soybean lecithin 1%, Ascorbyl palmitate 0.02%, ethyl-para-hydroxybenzoate 0.02%, surplus is water.
The preparation method of 2 one kinds of vitamin D linseed oil nanoemulsions of embodiment
The present embodiment provides the nanoemulsions described in above-described embodiment 1 containing vitamin D linseed oil Preparation method, comprise the steps:
1) aqueous phase is prepared: take the purified water of recipe quantity, pure with 2% sodium hydroxide solution regulation Changing water ph value is 8~12, is added to the water by emulsifying agent, under nitrogen protection, in 50~60 DEG C Shear to being uniformly dispersed;
2) oil phase is prepared: add in linseed oil by vitamin D, antioxidant, preservative, Add thermal agitation, control at 40~50 DEG C, mixing;
3) oil phase is added in aqueous phase, shear and make colostrum, regulation system pH value to 6.7;
4) use gradient boost mode to carry out high-pressure homogeneous to colostrum, prepare nanoemulsions;
Described gradient boost is particularly as follows: first carry out 200~400bar low pressure recycle process, its mesh Be that particle bigger for particle diameter is pulverized, prevent under high pressure damaging high pressure homogenizer;So After again 500~700bar cycle of higher pressure process, its objective is to increase the stability of breast grain.Described The temperature that homogeneous processes controls at 40~60 DEG C.
The preparation method of 3 one kinds of vitamin D linseed oil nanoemulsions of embodiment
The present embodiment uses method described in embodiment 2 to prepare the raw containing dimension of formula described in embodiment 1 The nanoemulsions of element D linseed oil, differs only in, step 3) system pH is 6.0.
4 one kinds of vitamin D linseed oil nanoemulsions of embodiment
The present embodiment uses method described in embodiment 2 to prepare the raw containing dimension of formula described in embodiment 1 The nanoemulsions of element D linseed oil, differs only in, step 3) system pH is 7.6.
The preparation method of 5 one kinds of vitamin D linseed oil nanoemulsions of embodiment
The present embodiment uses method described in embodiment 2 to prepare the raw containing dimension of formula described in embodiment 1 The nanoemulsions of element D linseed oil, differs only in, step 3) system pH is 5.5.
The preparation method of 6 one kinds of vitamin D linseed oil nanoemulsions of embodiment
The present embodiment uses method described in embodiment 2 to prepare the raw containing dimension of formula described in embodiment 1 The nanoemulsions of element D linseed oil, differs only in, step 3) system pH is 8.3.
Gained nanoemulsions particle diameter be 326nm, pH be 8.3, Zeta potential is at-29.33mV.
7 one kinds of vitamin D linseed oil nanoemulsions of embodiment
The present embodiment provide a kind of use prepared by method described in embodiment 2 containing vitamin D flax The nanoemulsions of seed oil, difference is: fill a prescription as (being calculated in mass percent): vitamin D 0.2%, linseed oil 5%, soybean lecithin 0.5%, ascorbyl palmitate 0.02%, to hydroxyl Yl benzoic acid ethyl ester 0.02%, surplus is water.Step 3) system pH is 6.9.
8 one kinds of vitamin D linseed oil nanoemulsions of embodiment
The present embodiment provide a kind of use prepared by method described in embodiment 2 containing vitamin D flax The nanoemulsions of seed oil, difference is: fill a prescription as (being calculated in mass percent): vitamin D 0.2%, linseed oil 5%, soybean lecithin 3%, ascorbyl palmitate 0.02%, to hydroxyl Yl benzoic acid ethyl ester 0.02%, surplus is water.Step 3) system pH is 7.1.
The various embodiments described above gained nanoemulsions Indexs measure result such as table 1.
Table 1
From above-described embodiment, use the nanoemulsions that scheme of the present invention prepares, electricity Position absolute value is high, and correspondingly degree of stability is good, and drugloading rate is relatively big, because it has less grain Footpath, can further improve its bioavilability, arbitrarily can dissolve each other with milk, beverage etc., side Just user takes;Wherein with embodiment 4, embodiment 6 more preferably.
Although, the most with a general description of the specific embodiments the present invention is made Detailed description, but on the basis of the present invention, it can be made some modifications or improvements, this Will be apparent to those skilled in the art.Therefore, without departing from present invention spirit On the basis of these modifications or improvements, belong to the scope of protection of present invention.

Claims (10)

1. the nanoemulsions containing vitamin D linseed oil, it is characterised in that by as follows The raw material of mass percent prepares: vitamin D 0.02%-1%, linseed oil 1%-10%, breast Agent 0.5%-3%, antioxidant 0.005%-0.5%, preservative 0.005%-0.5%, surplus is Water.
Nanoemulsions the most according to claim 1, it is characterised in that described containing vitamin The nanoemulsions of D linseed oil, is prepared by the raw material of following mass percent: vitamin D 0.2%-0.8%, linseed oil 2%-6%, emulsifying agent 0.8%-1.5%, antioxidant 0. 01%-0.2%, preservative 0.01%-0.2%, surplus is water.
Nanoemulsions the most according to claim 1 and 2, it is characterised in that described emulsification Agent is selected from soybean lecithin or yolk phospholipid.
Nanoemulsions the most according to claim 1 and 2, it is characterised in that described antioxygen Agent is selected from ascorbyl palmitate, butylated hydroxy anisole, dibutyl hydroxy toluene, no food One or more in sub-propyl propionate, tert-butylhydroquinone or tocopherol.
Nanoemulsions the most according to claim 1 and 2, it is characterised in that described anticorrosion One or more in ethyl-para-hydroxybenzoate, Sodium Benzoate or potassium sorbate of agent.
6. according to the arbitrary described nanoemulsions of claim 1-5, it is characterised in that in Asia Flaxseed oil adds vegetable oil and is configured to miscella.
7. according to the arbitrary described nanoemulsions of claim 1-6, it is characterised in that described contain The nanoemulsions particle diameter of vitamin D linseed oil is 5.5-8.3, Zeta electricity less than 600nm, pH Position is between-36.75V~-13.93mV.
8. a preparation method for the nanoemulsions containing vitamin D linseed oil, its feature exists In, comprise the steps:
1) prepare aqueous phase: added by emulsifying agent in alkaline water, under nitrogen protection, shear to dividing Dissipate uniformly;
2) oil phase is prepared: add in linseed oil by vitamin D, antioxidant, preservative, Add thermal agitation, mixing;
3) oil phase is added in aqueous phase, shear and make colostrum, regulation system pH value to 5.5-8.3;
4) use gradient boost mode to carry out high-pressure homogeneous to colostrum, prepare nanoemulsions.
The preparation method of nanoemulsions the most according to claim 8, it is characterised in that step Rapid 4), in, described gradient boost is: first carry out 200~400bar low pressure recycle process, then 500~ 700bar cycle of higher pressure processes;The temperature that described homogeneous processes controls at 40~60 DEG C.
10. the arbitrary described vitamin D linseed oil nanoemulsions that contains of claim 1-7 is at food Application in product, field of health care products.
CN201610096942.3A 2016-02-22 2016-02-22 Nano-emulsion containing vitamin D and linseed oil as well as preparation method and application of nano-emulsion Pending CN105746730A (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106174555A (en) * 2016-08-31 2016-12-07 济南大东农生物技术有限公司 A kind of dimethylglycine sodium vitamin composite nano-emulsion and preparation method thereof
CN106867866A (en) * 2017-01-26 2017-06-20 广东澳米嘉生物科技有限公司 A kind of nutrition vinegar rich in the unrighted acids of ω 3
CN106867856A (en) * 2017-01-24 2017-06-20 东南大学 A kind of linseed oil health-care vinegar and preparation method thereof
CN107296152A (en) * 2017-08-25 2017-10-27 山东静远药业有限公司 Emulsion compositions containing 25 hydroxycholecalciferols and preparation method thereof
CN107874257A (en) * 2017-11-09 2018-04-06 大连工业大学 The preparation method of high embedding rate small particle antarctic krill oil nanoparticle
CN109430873A (en) * 2018-11-26 2019-03-08 荣海生物科技有限公司 A kind of anti-oxidant linseed oil microcapsules and preparation method thereof
RU2684586C1 (en) * 2018-09-24 2019-04-09 Александр Александрович Кролевец Ice-cream production method with nanostructured vitamin d
CN110623159A (en) * 2019-10-25 2019-12-31 常熟理工学院 Pig feed containing linseed oil and apigenin solid lipid nanoparticles and preparation method thereof
CN114468294A (en) * 2022-01-24 2022-05-13 河南农业大学 Nano-emulsion simultaneously loaded with linseed oil and lutein and preparation method thereof
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
RU2812079C2 (en) * 2018-12-06 2024-01-22 Липикар Лайф Сайенсиз Лтд. Vitamin d microemulsions and their applications

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106174555B (en) * 2016-08-31 2019-10-08 济南大东农生物技术有限公司 A kind of dimethylglycine sodium vitamin composite nano-emulsion and preparation method thereof
CN106174555A (en) * 2016-08-31 2016-12-07 济南大东农生物技术有限公司 A kind of dimethylglycine sodium vitamin composite nano-emulsion and preparation method thereof
CN106867856A (en) * 2017-01-24 2017-06-20 东南大学 A kind of linseed oil health-care vinegar and preparation method thereof
CN106867866A (en) * 2017-01-26 2017-06-20 广东澳米嘉生物科技有限公司 A kind of nutrition vinegar rich in the unrighted acids of ω 3
CN107296152B (en) * 2017-08-25 2021-04-02 山东静远药业有限公司 Emulsion composition containing 25-hydroxy vitamin D3 and preparation method thereof
CN107296152A (en) * 2017-08-25 2017-10-27 山东静远药业有限公司 Emulsion compositions containing 25 hydroxycholecalciferols and preparation method thereof
CN107874257A (en) * 2017-11-09 2018-04-06 大连工业大学 The preparation method of high embedding rate small particle antarctic krill oil nanoparticle
CN107874257B (en) * 2017-11-09 2021-05-07 大连工业大学 Preparation method of euphausia superba oil nanoparticles with high embedding rate and small particle size
RU2684586C1 (en) * 2018-09-24 2019-04-09 Александр Александрович Кролевец Ice-cream production method with nanostructured vitamin d
CN109430873A (en) * 2018-11-26 2019-03-08 荣海生物科技有限公司 A kind of anti-oxidant linseed oil microcapsules and preparation method thereof
RU2812079C2 (en) * 2018-12-06 2024-01-22 Липикар Лайф Сайенсиз Лтд. Vitamin d microemulsions and their applications
CN110623159A (en) * 2019-10-25 2019-12-31 常熟理工学院 Pig feed containing linseed oil and apigenin solid lipid nanoparticles and preparation method thereof
CN114468294A (en) * 2022-01-24 2022-05-13 河南农业大学 Nano-emulsion simultaneously loaded with linseed oil and lutein and preparation method thereof
CN114468294B (en) * 2022-01-24 2024-04-02 河南农业大学 Nanoemulsion simultaneously loaded with linseed oil and lutein and preparation method thereof
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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