CN101161238A - A lipid nanometer microcapsule based on phospholipids and method for preparing the same - Google Patents
A lipid nanometer microcapsule based on phospholipids and method for preparing the same Download PDFInfo
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- CN101161238A CN101161238A CNA2007101902224A CN200710190222A CN101161238A CN 101161238 A CN101161238 A CN 101161238A CN A2007101902224 A CNA2007101902224 A CN A2007101902224A CN 200710190222 A CN200710190222 A CN 200710190222A CN 101161238 A CN101161238 A CN 101161238A
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Abstract
The present invention relates to a lipid nanometer microcapsule based on phospholipids and preparation method. The lipid nanometer microcapsule is constituted of at least one core material made of oil is liquid under normal temperature and film material composed of phospholipids, the average particle size of the lipid nanometer microcapsule is less than 100 nm, the weight ratio of the core material and film material is 0.5 to 6. Preparing the core material and film material into oil-in-water type microemulsion liquid under 25 to 80 C DEG, and then cooling the O/W microemulsion liquid to obtain lipid nanometer microcapsule, by the present invention preparation method emulsifying and homogenizing preparing to obtain a lipid nanometer microcapsule coating phospholipids, average particle size is less than 100 nm. The lipid nanometer microcapsule has good stability, hydrophilic and biologically compatible, can be widely used in cosmetics, food and medicine filed.
Description
Technical field
The present invention relates to a kind of lipid nanometer microcapsule based on phospholipid and preparation method thereof, be specifically related to a kind of lipid nanometer microcapsule based on phospholipid and preparation method thereof, and the application of this lipid nanometer microcapsule in cosmetics, food and medicine.
Background technology
In recent years, raising along with people's living standard, demand to cosmetics, food and medicine has been tending towards functionalization, problem such as that absorbing in use can appear in wherein employed active function composition is low, poor stability, and the ordinary preparation technology can not satisfy the demand of social development.Based on present situation like this, for can allow active function ingredient stability ground, effectively, fully be transported to the purpose position and discharge, nano-carrier systematic research and development are subjected to the attention of association area researcher, pertinent literature and patent emerge in an endless stream.Microemulsion is that affiliated technical field is known, for the fat-soluble active ingredient of solubilising, needs to use a large amount of surfactants, is extensive use of thereby limited microemulsion; In order to reduce the consumption of surfactant, technology such as millimicro emulsion, lipid nanoparticle are come out one after another.Patent exploitations such as ZL99126428.2, ZL99126145.3 and ZL99126429.0 the nano-carrier system of lipid millimicro emulsion; Patent ZL01807142.2 adopts the core of phospholipid and relatively large hydrophilic surfactant parcel lipid to develop the lipin nanometer capsule carrier system; People such as Wolfgang Mehnert, R.H.Muller have developed solid lipid nanoparticle and nano structured lipid carrier (Wolfgang Mehnert, Karsten Mader, Advanced Drug Delivery Reviews 47 (2001) 165-196; R.H.Muller, M.Radtk, Advanced Drug Delivery Reviews 54 Suppl.1 (2002) S131-S155).But, all adopted relatively large surfactant in these nano-carrier systems, and the surfactant that adopts is all from synthetic class surfactant, because synthetic class surfactant security row is not high, be restricted in actual applications, and, need to add a large amount of synthetic class surfactants in order to reach the effect of solubilising, the parcel amount of liposoluble substance is not high, is unfavorable for actual extensive use.Therefore develop a kind of amount of parcel height, the nano-carrier system that does not contain synthetic class surfactant safe, good stability and have very that important use is worth.
Summary of the invention
Technical problem: the object of the present invention is to provide a kind of lipid nanometer microcapsule based on phospholipid and preparation method thereof, for fat-soluble active matter provides a kind of amount of parcel height, good stability, the safe lipid nanometer microcapsule carrier system based on phospholipid.
Technical scheme: the lipid nanometer microcapsule that the present invention is based on phospholipid is made of for the core of liquid line of oils one-tenth with by the film material that phospholipid is formed down at least a room temperature, this lipid nanometer microcapsule mean diameter is less than 100nm, and the ratio value of core weight and film material weight is 0.5～6.
Described phospholipid adopts room temperature to be solid-state phospholipid down.Described room temperature is lecithin or cephalin or lipositol or sphingomyelin for solid-state phospholipid down.Phospholipid is lecithin, and its phosphatidylcholine content is 40%～92%, and total phospholipids content is not less than 97%.The used oil of described core is fatty acid ester or fatty acid or aliphatic alcohol or hydrocarbon ils or above mixtures of material.Contain the fat-soluble active ingredient in cosmetics or food or the medicine in the described core.
The preparation method that the present invention is based on the lipid nanometer microcapsule of phospholipid is that core and film material are prepared into water oil-packaging type micro-emulsion liquid under 25 ℃～80 ℃ temperature, then this o/w microemulsion cooling can be obtained lipid nanometer microcapsule, and concrete preparation method is as follows:
The preparation of A, oil phase: with mass percent 1%～30% oil phase core material component under 25 ℃～80 ℃ temperature conditions stirring and dissolving to the homogeneous system;
The preparation of B, water: the deionized water of mass percent 1%～30% is added in the polyhydric alcohol or sugar of mass percent 30%～80%, be stirred to transparent system under 25 ℃～80 ℃ temperature conditions; In this system, add mass percent 1%～10% film material then, be stirred to the film material under 25 ℃～80 ℃ temperature conditions and be dispersed to the homogeneous system fully;
The preparation of C, O/W emulsion: oil phase is added aqueous phase, be stirred to the homogeneous system under 25 ℃～80 ℃ temperature conditions, then this system high pressure homogenize under 25 ℃ ~ 80 ℃ temperature and 500bar～1500bar pressure condition is circulated 2～8 times, at last cooling under 4 ℃～15 ℃ conditions of the O/W emulsion behind the homogenizing is obtained lipid nanometer microcapsule.
The polyvinyl alcohol or Polyethylene Glycol or polyacrylamide or polyvinylpyrrolidone or the Polyethylene Glycol phospholipid derivative that in deionized water, add mass percent 0.1%～2% when water prepares.A kind of in the glycerol, pentitol, hexitol, fructose, glucose sugar, Xylitol, sucrose, lactose, maltose alcohol, sorbitol of polyhydric alcohol that is adopted or sugar, or above two kinds, or above mixture more than two kinds.
Beneficial effect: the present invention has found that in secular experimentation high employing of a kind of amount of parcel is the lipid nanometer microcapsule carrier system that do not contain synthetic class surfactant of solid-state lecithin as the capsule material under the pure natural room temperature.Advantages such as this lipid nanometer microcapsule has that particle diameter is little, good stability, safe and good biocompatibility, this lipid nanometer microcapsule can wrap up up to 6 times to the fat-soluble core of capsule material in addition, has very wide application prospect in fields such as cosmetics, food and medicines.
The present invention is a kind of lipid nanometer microcapsule based on phospholipid and preparation method thereof, for fat-soluble active matter provides a kind of amount of parcel height, good stability, the safe lipid nanometer microcapsule carrier system based on phospholipid.
The specific embodiment
The said lipid nanometer microcapsule of the present invention based on phospholipid, constitute for the core of liquid line of oils one-tenth with by the film material that phospholipid is formed down by at least a room temperature, this lipid nanometer microcapsule mean diameter is less than 100nm, and the ratio of core weight and film material weight is 0.5～6.This lipid nanometer microcapsule is characterised in that fat-soluble core is wrapped in by monolayer, solid-state lipid immobilized artificial membrane material, has good hydrophilic.
The said lipid nanometer microcapsule mean diameter based on phospholipid of the present invention is less than 50nm.
The said phospholipid room temperature that lipid nanometer microcapsule adopted based on phospholipid of the present invention is down solid-state, for example lecithin, cephalin, lipositol or sphingomyelin.
The said phospholipid that lipid nanometer microcapsule adopted based on phospholipid of the present invention is lecithin, and its phosphatidylcholine content is 40%～92%, and total phospholipids content is not less than 97%.
The said ratio based on core weight in the lipid nanometer microcapsule of phospholipid and film material weight of the present invention is between 1～4.
The present invention said based on the used oil of core in the lipid nanometer microcapsule of phospholipid be fatty acid ester (for example: myristic acid meat myristin, the dodecyl cetylate, caprylic/capric glyceride, trilaurin, myristin, tripalmitin etc.), fatty acid (for example: stearic acid, Palmic acid, lauric acid, mountain Yu acid, oleic acid, linoleic acid, linolenic acid etc.), aliphatic alcohol (stearyl alcohol for example, spermol, behenyl alcohol etc.), hydrocarbon ils (for example: natural squalane, Fancol ID, 2-Methylpentadecane etc.) and composition thereof (vegetable oil for example, the animal wet goods).
The said lipid nanometer microcapsule of the present invention based on phospholipid, can contain the fat-soluble active ingredient in cosmetics, food or the medicine in the core, for example vitamin A and derivant, vitamin E and derivant, vitamin D and derivant, vitamin K and derivant, essential oil, cholesterol, sitosterol, coenzyme Q10, imiquimod, ceramide etc.
The preparation method of the said lipid nanometer microcapsule based on phospholipid of the present invention is characterized in that core and film material are prepared into the O/W emulsion under 25 ℃～80 ℃ temperature, and this O/W emulsion cooling can be obtained lipid nanometer microcapsule, and concrete preparation method is as follows:
The preparation of A, oil phase: with 1%～30% oil phase core material component under 25 ℃～80 ℃ temperature conditions stirring and dissolving to the homogeneous system;
The preparation of B, water: in the polyhydric alcohol or sugar of deionized water adding 30%～80%, be stirred to transparent system under 25 ℃～80 ℃ temperature conditions with 1%～30%; In this system, add 1%～10% lecithin film material at last, be stirred to lecithin under 25 ℃～80 ℃ temperature conditions and be dispersed to the homogeneous system fully;
The preparation of C, O/W emulsion: oil phase is added aqueous phase, be stirred to the homogeneous system under 25 ℃～80 ℃ temperature conditions, then this system high pressure homogenize under 25 ℃～80 ℃ temperature and 500bar～1500bar pressure condition is circulated 2～8 times, at last cooling under 4 ℃～15 ℃ conditions of the O/W emulsion behind the homogenizing is obtained lipid nanometer microcapsule.
Can in deionized water, add 0.1%～2% high molecular weight water soluble polymer in the preparation method of the said lipid nanometer microcapsule based on phospholipid of the present invention for the viscosity that increases emulsion, for example polyvinyl alcohol, Polyethylene Glycol, polyacrylamide, polyvinylpyrrolidone, Polyethylene Glycol phospholipid derivative.
Polyhydric alcohol that is adopted in the preparation method of the said lipid nanometer microcapsule based on phospholipid of the present invention or sugar are glycerol, pentitol, hexitol, fructose, glucose sugar, Xylitol, sucrose, lactose, maltose alcohol, sorbitol and composition thereof.
Embodiment 1: the lipid nanometer microcapsule based on phospholipid that does not contain active component
The preparation of A, oil phase: the tripalmitin that takes by weighing 15g caprylic/capric glyceride and 10g is dissolved as the oil phase of homogeneous in the water-bath of 60 degree;
The preparation of B, water: take by weighing the 10g deionized water and become the glycerine water solution of homogeneous in 60 degree stirred in water bath, and then add 5g lecithin (72%PC), be stirred to phospholipid and be distributed to fully in the glycerine water solution, as water with 60g glycerol;
The preparation of C, O/W emulsion: oil phase is added aqueous phase be stirred to the O/W emulsion that forms homogeneous under 60 degree conditions, then this emulsion is circulated 6 times through high pressure homogenizer under the 800bar pressure condition, at last resulting emulsion room temperature cooling is formed translucent thick liquid, can obtain lipid nanometer microcapsule.This lipid nanometer microcapsule is tested its lipid nanometer microcapsule for spherical by the freeze-etching electron microscopy, and mean diameter is between 20～60nm, and electromicroscopic photograph is seen accompanying drawing 1.
In this example, investigated with different formulations and prepared lipid nanometer microcapsule, following table 1 is the different lipid nanometer microcapsules of different formulations preparation.
Table 1
| Mass percent % |
| Caprylic/capric glyceride | 3 | 3 | 3 | 9 | 12 | 20 | 10 |
| Tripalmitin | 1 | 1 | 9.5 | 5 | 8 | 2.5 | 10 |
| Phospholipid | 1 | 1 | 2.5 | 5 | 5 | 7.5 | 10 |
| Glycerol | 80 | 65 | 65 | 80 | 60 | 40 | 60 |
| Deionized water | 15 | 30 | 20 | 1 | 15 | 30 | 10 |
Preparation condition all is consistent (800bar, 6 times) in the above-mentioned prescription, at last the lipid nanometer microcapsule of preparing has been observed its pattern and mean diameter size by the freeze-etching electron microscopy, and particle diameter changes between 20～80nm.
Embodiment 2 is based on the retinoic acid lipid nanometer microcapsule of phospholipid
The preparation of A, oil phase: the retinoic acid that takes by weighing 8g soybean oil and 8g is dissolved as the oil phase of homogeneous in the water-bath of 65 degree;
The preparation of B, water: take by weighing the 15g deionized water and become the glycerine water solution of homogeneous in 65 degree stirred in water bath, and then add 4g lecithin (45%PC), be stirred to phospholipid and be distributed to fully in the glycerine water solution, as water with 65g glycerol;
The preparation of C, O/W emulsion: oil phase is added aqueous phase be stirred to the O/W emulsion that forms homogeneous under 65 degree conditions, then this emulsion is circulated 4 times through high pressure homogenizer under the 1000bar pressure condition, at last resulting emulsion room temperature cooling is formed translucent thick liquid, can obtain the retinoic acid lipid nanometer microcapsule, test its particle diameter greatly between 40～70nm through the freeze-etching electron microscopy.
Embodiment 3 is based on the Vitamin E acetate lipid nanometer microcapsule of phospholipid
The preparation of A, oil phase: the Vitamin E acetate that takes by weighing natural squalane of 2g and 15g is dissolved as the oil phase of homogeneous in the water-bath of 40 degree;
The preparation of B, water: take by weighing the 20g deionized water and become the glycerine water solution of homogeneous in 40 degree stirred in water bath, and then add 6g lecithin (72%PC), be stirred to phospholipid and be distributed to fully in the fructose water solution, as water with 57g fructose;
The preparation of C, O/W emulsion: oil phase is added aqueous phase be stirred to the O/W emulsion that forms homogeneous under 45 degree conditions, then this emulsion is circulated 4 times through high pressure homogenizer under the 1500bar pressure condition, at last resulting emulsion room temperature cooling is formed transparent thick liquid, can obtain the Vitamin E acetate lipid nanometer microcapsule, test its particle diameter between 30～50nm through the freeze-etching electron microscopy.
Embodiment 4 is based on the imiquimod lipid nanometer microcapsule of phospholipid
The preparation of A, oil phase: the imiquimod that takes by weighing the natural squalane of 2g, 5g capric acid and 5g is dissolved as the oil phase of homogeneous in the water-bath of 70 degree;
The preparation of B, water: take by weighing 2g cetomacrogol 1000 adding 15g deionized water and dissolve fully, and then adding 69g glycerol becomes the glycerine water solution of homogeneous in 70 degree stirred in water bath, and then adding 2g lecithin (72%PC), being stirred to phospholipid is distributed in the glycerine water solution, as water fully;
The preparation of C, O/W emulsion: oil phase is added aqueous phase be stirred to the O/W emulsion that forms homogeneous under 70 degree conditions, then this emulsion is circulated 8 times through high pressure homogenizer under the 800bar pressure condition, at last resulting emulsion room temperature cooling is formed translucent thick liquid, can obtain the imiquimod lipid nanometer microcapsule, test its particle diameter between 50～80nm through the freeze-etching electron microscopy.
Embodiment 5 is based on the coenzyme Q10 lipid nanometer microcapsule of phospholipid
The preparation of A, oil phase: the coenzyme Q10 that takes by weighing 5g caprylic/capric glyceride and 5g is dissolved as the oil phase of homogeneous in the water-bath of 60 degree;
The preparation of B, water: take by weighing the 23g deionized water and become the D/W of homogeneous in 60 degree stirred in water bath, and then add 5g lecithin (72%PC), be stirred to phospholipid and be distributed to fully in the D/W, as water with the 62g glucose;
The preparation of C, O/W emulsion: oil phase is added aqueous phase be stirred to the O/W emulsion that forms homogeneous under 60 degree conditions, then this emulsion is circulated 4 times through high pressure homogenizer under 1 000bar pressure condition, at last resulting emulsion room temperature cooling is formed transparent thick liquid, can obtain the coenzyme Q10 lipid nanometer microcapsule, test its particle diameter between 40～60nm through the freeze-etching electron microscopy.
Claims (9)
1. lipid nanometer microcapsule based on phospholipid, it is characterized in that this lipid nanometer microcapsule is made of for the core of liquid line of oils one-tenth with by the film material that phospholipid is formed down at least a room temperature, this lipid nanometer microcapsule mean diameter is less than 100nm, and the ratio value of core weight and film material weight is 0.5～6.
2. the lipid nanometer microcapsule based on phospholipid as claimed in claim 1 is characterized in that described phospholipid adopts room temperature to be solid-state phospholipid down.
3. the lipid nanometer microcapsule based on phospholipid as claimed in claim 2 is characterized in that under the described room temperature being that solid-state phospholipid is lecithin or cephalin or lipositol or sphingomyelin.
4. the lipid nanometer microcapsule based on phospholipid as claimed in claim 1 or 2 is characterized in that phospholipid is lecithin, and its phosphatidylcholine content is 40%～92%, and total phospholipids content is not less than 97%.
5. the lipid nanometer microcapsule based on phospholipid as claimed in claim 1 is characterized in that the used oil of described core is fatty acid ester or fatty acid or aliphatic alcohol or hydrocarbon ils or above mixtures of material.
6. the lipid nanometer microcapsule based on phospholipid as claimed in claim 1 is characterized in that containing in the described core fat-soluble active ingredient in cosmetics or food or the medicine.
7. the preparation method of the lipid nanometer microcapsule based on phospholipid as claimed in claim 1, it is characterized in that core and film material are prepared into water oil-packaging type micro-emulsion liquid under 25 ℃～80 ℃ temperature, then this o/w microemulsion cooling can be obtained lipid nanometer microcapsule, concrete preparation method is as follows:
The preparation of A, oil phase: with mass percent 1%～30% oil phase core material component under 25 ℃～80 ℃ temperature conditions stirring and dissolving to the homogeneous system;
The preparation of B, water: the deionized water of mass percent 1%～30% is added in the polyhydric alcohol or sugar of mass percent 30%～80%, be stirred to transparent system under 25 ℃～80 ℃ temperature conditions; In this system, add mass percent 1%～10% film material then, be stirred to the film material under 25 ℃～80 ℃ temperature conditions and be dispersed to the homogeneous system fully;
The preparation of C, O/W emulsion: oil phase is added aqueous phase, be stirred to the homogeneous system under 25 ℃～80 ℃ temperature conditions, then this system high pressure homogenize under 25 ℃ ~ 80 ℃ temperature and 500bar～1500bar pressure condition is circulated 2～8 times, at last cooling under 4 ℃～15 ℃ conditions of the O/W emulsion behind the homogenizing is obtained lipid nanometer microcapsule.
As described in the claim 7 based on the preparation method of the lipid nanometer microcapsule of phospholipid, it is characterized in that in deionized water, adding when water prepares polyvinyl alcohol or Polyethylene Glycol or polyacrylamide or the polyvinylpyrrolidone or the Polyethylene Glycol phospholipid derivative of mass percent 0.1%～2%.
As described in the claim 8 based on the preparation method of the lipid nanometer microcapsule of phospholipid, it is characterized in that a kind of in glycerol, pentitol, hexitol, fructose, glucose sugar, Xylitol, sucrose, lactose, maltose alcohol, the sorbitol of the polyhydric alcohol that adopted or sugar, or above two kinds, or above mixture more than two kinds.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102429828A (en) * | 2011-12-08 | 2012-05-02 | 海南海之润生物工程有限公司 | Coenzyme Q10 microcapsule and preparation method and application thereof |
| CN102939077A (en) * | 2010-06-03 | 2013-02-20 | 莱迪杜德制药公司 | Nanoemulsion composition containing vitamin k |
| CN104013955A (en) * | 2014-06-18 | 2014-09-03 | 中国科学院过程工程研究所 | Oil-in-water emulsion free of surfactant and use thereof |
| CN107173458A (en) * | 2017-05-23 | 2017-09-19 | 三河汇福生物科技有限公司 | A kind of edible oil and fat microencapsulation composite antioxidant and preparation method thereof |
| CN112168737A (en) * | 2019-07-04 | 2021-01-05 | 伽蓝（集团）股份有限公司 | Nano emulsion and preparation method thereof |
| CN116058479A (en) * | 2023-03-06 | 2023-05-05 | 山东凯欣绿色农业发展股份有限公司 | Formula and processing technology of canned pear with health-care effect |
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2007
- 2007-11-20 CN CNA2007101902224A patent/CN101161238A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102939077A (en) * | 2010-06-03 | 2013-02-20 | 莱迪杜德制药公司 | Nanoemulsion composition containing vitamin k |
| CN102939077B (en) * | 2010-06-03 | 2016-04-06 | 莱迪杜德制药公司 | Nano-emulsion composition containing vitamin K |
| CN102429828A (en) * | 2011-12-08 | 2012-05-02 | 海南海之润生物工程有限公司 | Coenzyme Q10 microcapsule and preparation method and application thereof |
| CN104013955A (en) * | 2014-06-18 | 2014-09-03 | 中国科学院过程工程研究所 | Oil-in-water emulsion free of surfactant and use thereof |
| CN104013955B (en) * | 2014-06-18 | 2016-02-24 | 中国科学院过程工程研究所 | A kind of not containing O/w emulsion and uses thereof of surfactant |
| CN107173458A (en) * | 2017-05-23 | 2017-09-19 | 三河汇福生物科技有限公司 | A kind of edible oil and fat microencapsulation composite antioxidant and preparation method thereof |
| CN107173458B (en) * | 2017-05-23 | 2021-04-27 | 三河汇福生物科技有限公司 | Microencapsulated composite antioxidant for edible oil and fat and preparation method thereof |
| CN112168737A (en) * | 2019-07-04 | 2021-01-05 | 伽蓝（集团）股份有限公司 | Nano emulsion and preparation method thereof |
| CN116058479A (en) * | 2023-03-06 | 2023-05-05 | 山东凯欣绿色农业发展股份有限公司 | Formula and processing technology of canned pear with health-care effect |
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