CN103859588A - Preparation method of squalene and astaxanthin composite multivesicular liposome and radical lowering and harm reducing method thereof - Google Patents
Preparation method of squalene and astaxanthin composite multivesicular liposome and radical lowering and harm reducing method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a squalene and astaxanthin composite multivesicular liposome and a radical lowering and harm reducing method thereof. The multivesicular liposome is prepared from 12-18 parts of hydrogenated phospholipid, 10-20 parts of stabilizer, 10-15 parts of surfactant and the balance of squalene and astaxanthin composite. Through microencapsulating the squalene and astaxanthin composite, the defect that the squalene and astaxanthin composite is easily oxidized in the air and loses effectiveness is overcome, and the effect of increasing the stability of a squalene and astaxanthin blending synergy composite is achieved. The multivesicular liposome is built in a cigarette filter tip made of cellulose acetate fiber in the forming process of a cigarette filter tip bar, and 0.5-1.5g of multivesicular liposomes is arranged in each cigarette filter tip, so that a cigarette filter tip capable of lowering the harm of cigarettes is obtained; the surface area of the multivesicular liposome is large, so that anti-oxidant makes full contact with main stream smoke, gas-phase free radical in the main stream smoke can be effectively removed, and powerful technical support is provided for solving the smoking and health problem.
Description
Technical field
The present invention relates to technical field of chemistry, more specifically, relate to a kind of multivesicular liposome containing squalene and astaxanthin composition and preparation method thereof and fall the application aspect base harm reduction at cigarette.
Background technology
The harm that thousands of kinds of compounds that smoking produces and the radical pair human body of high concentration cause causes people's generally attention.And the effect of radical pair health endangers the most by force maximum, it can cause tuberculosis, heart disease and cancer, and these radical pairs smoker produces serious injury.Smoking produces the free radical of high concentration, comprises the phase Free Radicals that the life-span is relatively grown, and generation is reacted in quinones and half quinones, multiring aromatic hydrocarbon free radical and they active oxygen radical with oxygen is as superoxide anion (O
2 -), hydrogen peroxide (H
2o
2), hydroxy radical (OH), singlet oxygen (
1o
2) and the gaseous phase free radical relatively short with life period such as lipid peroxidation free radical (ROO), alkoxy free group (RO), alkyl diradical (R), nitrogen oxide free radical etc.
At present in to flue gas aspect radicals scavenging research and few, mainly reduce the injury of radical pair human body flue gas from additional natural, vitamin, amino acid, protein etc. and biology enzyme free radical scavenger and trace element, natural mineral matter.But these free radical scavengers generally are one or more simple mixing to be added in pipe tobacco.
Squalene is a kind of lipid unsaponifiable matter, for the many unsaturated olefins of one (squalene), to find from the liver oil of shark at first, within 1914, be named as Squalene, its chemical name is 2, 6, 10, 15, 19, 23-hexamethyl-2, 6, 10, 14, 18, 22-tetracosa carbon six alkene, belong to open chain triterpene, claim again Squalene, participate in human body cholesterol biosynthesis and can enhance metabolism, there is superoxide dismutase (SOD) activity in the body of raising, strengthen body immunity, anti-ageing, antifatigue, the different physiological roles such as antitumor, it is a kind of avirulent marine bioactivity material with the effect of preventing and curing diseases.Squalene distributes very wide in plant, but content is not high, and many lower than 5% of unsaponifiable matter in vegetable oil, only minority content is more, and as olive oil contains squalene 150～700mg/100g, in rice bran oil, its content is 332mg/100g.
Astaxanthin is a kind of Red carotenoids of finding from river prawn shell, oyster and salmon, and chemical name is 3,3 '-dihydroxy-4,4 '-diketo-β, and β '-carrotene, can be with protein bound blue or green, blue in vivo.There is anti-oxidant, anti-ageing, antitumor, prevention cardiovascular and cerebrovascular disease effect.Astaxanthin is the one of carotenoid.Also be the highest level product of carotenogenesis, beta carotene, lutein, canthaxanthin, lycopene etc. are only all the intermediate products of carotenogenesis, and therefore at nature, astaxanthin has the strongest non-oxidizability.Effectively the oxygen radical in scavenger-cell, strengthens cytothesis ability, maintains the accumulation of organism balance and minimizing senile cell; Cell protection and DNA health from inside to outside; thereby protection skin health, promotes hair growth, anti-ageing, relieving sports fatigue, invigorate.
In order to overcome the shortcoming of common antioxidant, reach the object that can simultaneously remove long-life phase Free Radicals and the relatively short gaseous phase free radical of life period, the applicant is devoted for years in correlative study and has applied for patent, a kind of squalene and tea polyphenol composition and the application in cigarette thereof are disclosed in the patent that is ZL201010529711.X in the patent No., squalene and beta carotene composition and the application in cigarette thereof are disclosed in the application that is ZL201010578167.8 in the patent No., Patents technology is all that squalene and beta carotene synergistic composition or squalene and Tea Polyphenols synergistic composition are directly added in pipe tobacco.But further research is found, squalene and beta carotene and squalene and Tea Polyphenols synergistic composition are easy to oxidation deterioration in air, composition is unstable in the time of application, actual production inconvenience.
Liposome (liposome) is a kind of artificial membrane.In the time that amphiphatic molecule is scattered in water as phosphatide and sphingolipid, the hydrophobic tail of molecule is tended to flock together, and avoids water, and hydrophilic head is exposed to water, form have bilayer structure vesicle, be called liposome.According to textural classification, liposome is divided into unilamelar liposome, multilamelar liposome and multivesicular liposome.Multivesicular liposome is a kind of liposome with slow release effect, is connected and composed by many non-concentric chamber, and particle diameter, at 5～50 μ m, has larger envelope volume than conventional liposome, is particularly useful for sealing of water soluble drug.The application of liposome is mainly aspect medical at present.
The people such as Li Changbao (2011) have applied for the patent of a kind of siraitia grosvenorii seed oil microcapsule powder and preparation method thereof (ZL201110371579.9), what they adopted is that beta-schardinger dextrin-, Arabic gum, monoglyceride are as outer wall materials, main purpose is to avoid the oxidation of Momordica grosvenori seed oil unrighted acid and squalene, can effectively extend the holding time of Momordica grosvenori seed oil.This Microcapsules Size is little, and outer wall is hard, and gas permeability is bad, is unsuitable for being applied in cigarette filter.
These free radical scavengers are processed into multivesicular liposome, insert the research of removing gaseous phase free radical (falling base) in cigarette filter and have no at present report, more have no technology of preparing and the application report of the multivesicular liposome based on squalene and astaxanthin synergistic composition.
Summary of the invention
The object of the invention is to overcome the application deficiency of existing multivesicular liposome technology aspect cigarette, and squalene and astaxanthin synergistic composition are in the technical deficiency of cigarette application aspect, and a kind of multivesicular liposome containing squalene and astaxanthin composition is provided.
Another object of the present invention is to provide the preparation method of described multivesicular liposome.
An also goal of the invention of the present invention is to provide the application of the described multivesicular liposome containing squalene and astaxanthin composition in cigarette.
Object of the present invention is achieved by the following technical programs:
A kind of multivesicular liposome containing squalene and astaxanthin composition is provided, and described multivesicular liposome is to be prepared by each component of following mass fraction:
Hydrogenated phospholipid: 12～18 parts;
Stabilizing agent: 10～20 parts;
Surfactant: 10～15 parts;
Surplus is squalene and astaxanthin composition;
Above-mentioned each constituent mass umber sum is 100 parts.
Preferably, the described multivesicular liposome containing squalene and astaxanthin composition, described multivesicular liposome is to be prepared by each component of following mass fraction:
Hydrogenated phospholipid: 14～16 parts;
Stabilizing agent: 15～18 parts;
Surfactant: 12～14 parts;
Surplus is squalene and astaxanthin composition;
Above-mentioned each constituent mass umber sum is 100 parts.
Can adopt multi-emulsion method to prepare the described multivesicular liposome containing squalene and astaxanthin composition with above-mentioned each component.
Described hydrogenated phospholipid be hydrolecithin, hydrogenated soya phosphatide one or both.Adopt two kinds of phosphatide, the mixed proportion of various phosphatide is not done strict restriction.
The preferred HES of described stabilizing agent, more preferably, adopt the one of low-molecular-weight (40000～70000 dalton) HES, middle molecular weight (130000～200000 dalton) HES and HMW (450000～480000 dalton) HES.
Described surfactant is preferably at least one in PEG400,18 alcohol, glycerine or shitosan (molecular weight does not do strict restriction).Adopt kinds of surface activating agent, the mixed proportion of various surfactants is not done strict restriction.
In described squalene and astaxanthin composition, the mass ratio of squalene and astaxanthin is 1: 10.6～12.6: 1, and its optimized proportion is: 1: 4.8～3.7: 1.
Described squalene can be the extract that extracts from plant, animal or microorganism or purified after sterling, can adopt commercial product.
Described astaxanthin can be that the astaxanthin extract that extracts from shrimp shell, oyster and salmon can be also the sterling after purified, can adopt commercial product.
The present invention provides the preparation method of the described multivesicular liposome containing squalene and astaxanthin composition simultaneously, comprises the following steps:
S1, hydrogenated phospholipid and squalene and astaxanthin composition are dissolved in propane diols, obtain mixed system;
S2, S1 gained mixed system is transferred in the aqueous solution that contains surfactant, high speed homogenizing fully mixes it, obtains the mixed system of homogenizing;
S3, in the mixed system of S2 gained homogenizing, add stabilizing agent to stir, form stable microparticle suspending liquid;
S4, the freeze drying of S3 gained microparticle suspending liquid is obtained to the multivesicular liposome containing squalene and astaxanthin composition.
Wherein, described in S1, the consumption of propane diols is determined according to the dissolubility of material.
Preferably, the aqueous solution that contains surfactant described in S2 is according to (20～30): 100 mass ratio is mixed to get by surfactant and water;
Preferably, the process conditions of high speed homogenizing are :≤2000r/min described in S2, stir 30min;
Preferably, described in S4, cryodesiccated process conditions are :-25 DEG C of freezing 1h, 6 × 10
-4freeze drying 8h under Pa.
The invention provides the multivesicular liposome containing squalene and astaxanthin composition that said method prepares.
Multivesicular liposome containing squalene and astaxanthin composition of the present invention obtains well application in cigarette, preferably application process is: in cigarette filter tip rod forming process, multivesicular liposome of the present invention is made an addition in the cigarette filter of acetate fiber, every built-in 0.5～1.5 gram of multivesicular liposome containing squalene and astaxanthin composition of the present invention of cigarette filter, obtain a kind of new cigarette filter, be applied to cigarette and can effectively reduce the harm of cigarette free radical.
Better addition is every built-in 0.8 gram of multivesicular liposome containing squalene and astaxanthin composition of the present invention of cigarette filter.
Beneficial effect of the present invention:
The present invention is applied to the technology of liposome especially multivesicular liposome in cigarette first, and success is in conjunction with squalene and astaxanthin synergistic composition, sum up suitable compatibility auxiliary agent and proportion compatibility, prepare the multivesicular liposome containing squalene and astaxanthin synergistic composition simplely, envelop rate is higher than general method for preparing lipidosome, for the further developing application of liposome provides strong technical support.
The present invention is successfully embedded in synergistic composition in multivesicular liposome, overcome the shortcoming that squalene and astaxanthin are easy to oxidation deactivation in air, by to squalene and astaxanthin mixture synergistic composition microencapsulation, reach the stability that increases squalene and astaxanthin mixture synergistic composition, acquisition can be applied to the multivesicular liposome of cigarette filter.
The present invention accurately limits material combination and preparation process condition, the multivesicular liposome gas permeability that processing obtains is strong, surface area is large, be applicable to the application demand of cigarette filter, can directly apply to cigarette filter, antioxidant can fully contact with main flume, reaches the object of removing free radical in main flume, provides strong technical support for solving smoking and healthy problem.
Detailed description of the invention
Further describe the present invention below in conjunction with specific embodiment.The test method using in following embodiment if no special instructions, is conventional method; The material, the reagent etc. that use if no special instructions, are reagent and the material that can obtain from conventional commercial sources.
Embodiment 1
Prepare each component according to following mass fraction: 18 grams of hydrolecithins (g); Squalene (the true Bioisystech Co., Ltd in Shanghai, content is greater than 96.0%, and following embodiment is same.But therefore do not limit the present invention, those skilled in the art can adopt the squalene in other sources) 5 grams (g); Astaxanthin (natural astaxanthin Co., Ltd of Jingzhou City, content is greater than 2.0%, and following embodiment is same.But therefore do not limit the present invention, those skilled in the art can adopt the astaxanthin in other sources) 42 grams (g); 15 grams of PEG400s (g); Middle molecular weight (130000～200000 dalton) 20 grams of HESs (g).
Preparation process is:
S1. hydrogenated phospholipid and squalene and astaxanthin are dissolved in 100mL propane diols, obtain mixed system;
S2. S1 gained mixed system is transferred in the 50mL water that contains 15g PEG400, high speed homogenizing (2000r/min, 30min) fully mixes it, obtains the mixed system of homogenizing;
S3. in the mixed system of S2 gained homogenizing, add HES to stir, form stable microparticle suspending liquid;
S4. by the freeze drying of S3 gained microparticle suspending liquid (25 DEG C of freezing 1h, 6 × 10
-4freeze drying 8h under Pa), obtain the multivesicular liposome containing squalene and astaxanthin composition.
In the preparation process of described multivesicular liposome, make water and propane diols, but propane diols and water finally all removes through freeze drying, do not count the component of composition, lower with.
Embodiment 2
Prepare each component according to following mass fraction: 18 grams of hydrogenated soya phosphatides; 10 grams of squalenes; 37 grams of astaxanthins; 18 15 grams of alcohol; 20 grams of HMW (450000～480000 dalton) HESs.
Preparation process is:
S1. hydrogenated soya phosphatide and squalene and astaxanthin are dissolved in 100 milliliters of (mL) propane diols, obtain mixed system;
S2. S1 gained mixed system is transferred in the 50mL water that contains 15g 18 alcohol, high speed homogenizing fully mixes it, obtains the mixed system of homogenizing;
S3. in the mixed system of S2 gained homogenizing, add HES to stir, form stable microparticle suspending liquid;
S4. the freeze drying of S3 gained microparticle suspending liquid is obtained to the multivesicular liposome containing squalene and astaxanthin composition.
Embodiment 3
Prepare each component according to following mass fraction: totally 18 grams of hydrolecithin and hydrogenated soya phosphatides; 20 grams of squalenes; 27 grams of astaxanthins; 15 grams of glycerine; 20 grams of low-molecular-weight (40000～70000 dalton) HESs.
Preparation process is:
S1. hydrogenated soya phosphatide and squalene and astaxanthin are dissolved in 100 milliliters of (mL) propane diols, obtain mixed system;
S2. S1 gained mixed system is transferred in the 50mL water that contains 15g glycerine, high speed homogenizing fully mixes it, obtains the mixed system of homogenizing;
S3. in the mixed system of S2 gained homogenizing, add HES to stir, form stable microparticle suspending liquid;
S4. the freeze drying of S3 gained microparticle suspending liquid is obtained to the multivesicular liposome containing squalene and astaxanthin composition.
Embodiment 4
Preparation process is with embodiment 1,2 or 3.Taking 18 grams of hydrogenated soya phosphatides, 27 grams of squalenes and 20 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 15 grams of shitosans and PEG400, high speed homogenizing fully mixes it, add 20 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 5
Preparation process is with embodiment 1,2 or 3.Taking 16 grams of hydrolecithins, 37 grams of squalenes and 10 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 15 grams of PEG400s and 18 alcohol, high speed homogenizing fully mixes it, add 20 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 6
Preparation process is with embodiment 1,2 or 3.Taking 16 grams of hydrolecithins, 42 grams of squalenes and 10 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 14 grams of glycerine, high speed homogenizing fully mixes it, add 18 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 7
Preparation process is with embodiment 1,2 or 3.Taking 15 grams of hydrolecithins, 5 grams of squalenes and 53 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 12 grams of glycerine, high speed homogenizing fully mixes it, add 15 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 8
Preparation process is with embodiment 1,2 or 3.Taking 15 grams of hydrogenated soya phosphatides, 10 grams of squalenes and 48 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 12 gram of 18 alcohol, high speed homogenizing fully mixes it, add 15 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 9
Taking 14 grams of hydrolecithins, 20 grams of squalenes and 38 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 12 grams of glycerine, high speed homogenizing fully mixes it, add 16 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 10
Preparation process is with embodiment 1,2 or 3.Taking 15 grams of hydrogenated soya phosphatides, 30 grams of squalenes and 28 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 12 grams of shitosans and glycerine, high speed homogenizing fully mixes it, add 15 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 11
Preparation process is with embodiment 1,2 or 3.Taking 15 grams of hydrogenated soya phosphatides, 40 grams of squalenes and 18 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 12 gram of 18 alcohol, high speed homogenizing fully mixes it, add 15 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 12
Preparation process is with embodiment 1,2 or 3.Taking 15 grams of hydrolecithins, 50 grams of squalenes and 8 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 12 grams of PEG400s, high speed homogenizing fully mixes it, add 15 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 13
Preparation process is with embodiment 1,2 or 3.Taking 12 grams of hydrolecithins, 8 grams of squalenes and 60 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 10 grams of PEG400s, high speed homogenizing fully mixes it, add 10 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 14
Preparation process is with embodiment 1,2 or 3.Taking 12 grams of hydrogenated soya phosphatides, 18 grams of squalenes and 50 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 10 gram of 18 alcohol, high speed homogenizing fully mixes it, add 10 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 15
Preparation process is with embodiment 1,2 or 3.Taking 12 grams of hydrogenated soya phosphatides, 28 grams of squalenes and 40 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 10 grams of glycerine, high speed homogenizing fully mixes it, add 10 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 16
Preparation process is with embodiment 1,2 or 3.Taking 12 grams of hydrolecithins, 38 grams of squalenes and 30 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 10 grams of shitosans, high speed homogenizing fully mixes it, add 10 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 17
Preparation process is with embodiment 1,2 or 3.Taking 12 grams of hydrolecithins, 48 grams of squalenes and 20 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 10 gram of 18 alcohol, high speed homogenizing fully mixes it, add 10 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 18
Preparation process is with embodiment 1,2 or 3.Taking 12 grams of hydrolecithins, 58 grams of squalenes and 10 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 10 grams of glycerine, high speed homogenizing fully mixes it, add 10 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
Embodiment 19
Preparation process is with embodiment 1,2 or 3.Taking 12 grams of hydrogenated soya phosphatides, 63 grams of squalenes and 5 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 10 grams of shitosans, high speed homogenizing fully mixes it, add 10 grams of HESs to stir, then freeze drying obtains the multivesicular liposome of squalene and astaxanthin composition again.
The multivesicular liposome testing result that above-described embodiment 1～19 is prepared is as follows: adopt ESEM or laser scattering method to detect, the multivesicular liposome particle diameter that embodiment 1～19 prepares is 900～1300nm, is evenly distributed, and is normality, and span is little.
Adopt sephadex separation method that squalene free in solution is separated with liposome with astaxanthin, respectively mensuration, computational envelope rate.According to (in liposome in squalene and astaxanthin composition quality/liposome squalene and astaxanthin composition gross mass) × 100% computational envelope rate.The multivesicular liposome envelop rate that the embodiment of the present invention 1～19 prepares is more than 79%.
Comparative example 1
Preparation process is with embodiment 1,2 or 3.Taking 6 grams of hydrogenated soya phosphatides, 39 grams of squalenes and 10 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 20 grams of glycerine, high speed homogenizing fully mixes it, add again 25 grams of HESs to stir, then the dry multivesicular liposome obtaining containing squalene and astaxanthin composition of freeze-drying.The multivesicular liposome particle diameter preparing is 1500～2500nm, skewness.Envelop rate is 36%.
Comparative example 2
Preparation process is with embodiment 1,2 or 3.Taking 10 Borneo camphor phosphatide, 50 grams of squalenes and 22 grams of astaxanthins is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 8 grams of gelatin, high speed homogenizing fully mixes it, add again 10 grams of hydroxypropyl methylcelluloses to stir, then the dry multivesicular liposome that obtains squalene and astaxanthin composition of freeze-drying.The multivesicular liposome particle diameter preparing is 1600～2700nm, skewness.Envelop rate is 30%.
Embodiment 20 application experiments
In cigarette filter tip rod forming process, multivesicular liposome described in above-described embodiment 1～19 is placed in to the cigarette filter of acetate fiber, multivesicular liposome described in every built-in 0.5,0.8 and 1.5 gram of embodiment 1～19 of cigarette filter, obtains reducing the cigarette filter that cigarette gaseous phase free radical endangers.Not contain the blank multivesicular liposome of squalene or astaxanthin, (taking 65 grams of hydrogenated soya phosphatides is dissolved in 100 milliliters of propane diols, be transferred in 50 ml waters that contain 15 gram of 18 alcohol, high speed homogenizing fully mixes it, add 20 grams of high molecular weight hydroxyethyl starch to stir, then freeze-drying is dry obtains blank multivesicular liposome again.The blank multivesicular liposome particle diameter preparing is 900～1100nm) be contrast.
Radicals scavenging effect detection in cigarette smoke: smoke gaseous phase free radical adopts spin catching agent PBN(2-benzene tert-butylnitrone) the rear detection of trapping.
Adopt conventional gaseous phase free radical detection method: adopt glassware to collect flue gas free radical.Add the carbon tetrachloride solution of certain density free radical scavenger PBN in collector, collector is linked on smoking machine, taking suction capacity as 35.0mL, suction time is 2s, and suction is spaced apart the standard suction speed smoking cigarette of 60s.After smoking, constant volume is collected flue gas free-atom aqueous solution, then puts into liquid nitrogen freezing.Detecting volume is 200 μ L.
The filter-tip cigarette that adds the natural synergistic composition multivesicular liposome of different content and different proportionings by detection produces the content of free radical, compared with the control, and the removing effect of calculation composition to gaseous phase free radical in cigarette smoke.Experimental result is in table 1～3:
Every cigarette filter of table 1:(adds 0.5 gram of multivesicular liposome)
| Sample | Gaseous phase free radical clearance rate (%) |
| Embodiment 1 | 4.39 |
| Embodiment 2 | 7.02 |
| Embodiment 3 | 8.94 |
| Embodiment 4 | 10.27 |
| Embodiment 5 | 9.39 |
| Embodiment 6 | 5.52 |
| Embodiment 7 | 8.39 |
| Embodiment 8 | 12.74 |
| Embodiment 9 | 13.82 |
| Embodiment 10 | 13.99 |
| Embodiment 11 | 14.62 |
| Embodiment 12 | 9.03 |
| Embodiment 13 | 9.71 |
| Embodiment 14 | 14.05 |
| Embodiment 15 | 17.83 |
| Embodiment 16 | 18.95 |
| Embodiment 17 | 20.73 |
| Embodiment 18 | 10.57 |
| Embodiment 19 | 6.39 |
| Blank | 0.23 |
Every cigarette filter of table 2:(adds 0.8 gram of multivesicular liposome)
| Sample | Gaseous phase free radical clearance rate (%) |
| Embodiment 1 | 5.38 |
| Embodiment 2 | 9.95 |
| Embodiment 3 | 10.74 |
| Embodiment 4 | 12.37 |
| Embodiment 5 | 13.97 |
| Embodiment 6 | 7.03 |
| Embodiment 7 | 9.38 |
| Embodiment 8 | 13.62 |
| Embodiment 9 | 19.37 |
| Embodiment 10 | 26.48 |
| Embodiment 11 | 24.35 |
| Embodiment 12 | 10.73 |
| Embodiment 13 | 10.25 |
| Embodiment 14 | 17.38 |
| Embodiment 15 | 20.65 |
| Embodiment 16 | 29.38 |
| Embodiment 17 | 28.47 |
| Embodiment 18 | 13.26 |
| Embodiment 19 | 8.38 |
| Blank | 0.23 |
Every cigarette filter of table 3:(adds 1.5 grams of multivesicular liposomes)
| Sample | Gaseous phase free radical clearance rate (%) |
| Embodiment 1 | 5.94 |
| Embodiment 2 | 10.17 |
| Embodiment 3 | 10.95 |
| Embodiment 4 | 13.04 |
| Embodiment 5 | 12.76 |
| Embodiment 6 | 8.38 |
| Embodiment 7 | 9.66 |
| Embodiment 8 | 12.94 |
| Embodiment 9 | 20.56 |
| Embodiment 10 | 24.83 |
| Embodiment 11 | 25.18 |
| Embodiment 12 | 11.93 |
| Embodiment 13 | 9.17 |
| Embodiment 14 | 18.90 |
| Embodiment 15 | 19.37 |
| Embodiment 16 | 27.49 |
| Embodiment 17 | 28.03 |
| Embodiment 18 | 14.95 |
| Embodiment 19 | 9.01 |
| Blank | 0.23 |
Experiment conclusion: from above-described embodiment, cigarette gaseous phase free radical being removed to effect can find out, when in multivesicular liposome containing the amount of natural during in 47～68% left and right, it freely has certain removing effect to gas phase, the proportioning of particularly working as squalene and astaxanthin is between 1: 10.6～12.6: 1, especially between 1: 4.8～3.7: 1 time, composition is removed effect to gaseous phase free radical and is had obvious synergistic effect, and its ability of removing free radical strengthens along with the increase of the amount of antioxidant.Actual according to producing, the present invention is for containing squalene and astaxanthin in 58% left and right in the multivesicular liposome of the natural composition of cigarette filter, its the removing ability synergistic effect to gaseous phase free radical between 1: 4.8～3.7: 1 of the proportioning of squalene and astaxanthin is obvious, and in every cigarette filter, to add multivesicular liposome amount be 0.8 gram of the best.
Claims (13)
1. containing a multivesicular liposome for squalene and astaxanthin composition, it is characterized in that, described multivesicular liposome is to be prepared by each component of following mass fraction:
Hydrogenated phospholipid: 12～18 parts;
Stabilizing agent: 10～20 parts;
Surfactant: 10～15 parts;
Surplus is squalene and astaxanthin composition;
Above-mentioned each constituent mass umber sum is 100 parts;
Described hydrogenated phospholipid is one or both in hydrolecithin, hydrogenated soya phosphatide;
Described stabilizing agent is HES;
Described surfactant is at least one in PEG400,18 alcohol, glycerine or shitosan.
2. according to claim 1 containing the multivesicular liposome of squalene and astaxanthin composition, it is characterized in that, is to be prepared by each component of following mass fraction:
Hydrogenated phospholipid: 14～16 parts;
Stabilizing agent: 15～18 parts;
Surfactant: 12～14 parts;
Surplus is squalene and astaxanthin composition;
Above-mentioned each constituent mass umber sum is 100 parts.
3. according to the multivesicular liposome that contains squalene and astaxanthin composition described in claim 1 or 2, it is characterized in that, described HES is the one of low-molecular-weight HES, middle molecular weight hydroxyethyl starch or high molecular weight hydroxyethyl starch.
4. according to the multivesicular liposome that contains squalene and astaxanthin composition described in claim 1 or 2, it is characterized in that, in described squalene and astaxanthin composition, the mass ratio of squalene and astaxanthin is 1: 10.6～12.6: 1.
5. according to claim 4 containing the multivesicular liposome of squalene and astaxanthin composition, it is characterized in that, in described squalene and astaxanthin composition, the mass ratio of squalene and astaxanthin is 1: 4.8～3.7: 1.
6. the preparation method who contains the multivesicular liposome of squalene and astaxanthin composition described in claim 1～5 any one, is characterized in that, comprises the following steps:
S1, hydrogenated phospholipid and squalene and astaxanthin composition are dissolved in propane diols, obtain mixed system;
S2, S1 gained mixed system is transferred in the aqueous solution that contains surfactant, high speed homogenizing fully mixes it, obtains the mixed system of homogenizing;
S3, in the mixed system of S2 gained homogenizing, add stabilizing agent to stir, form stable microparticle suspending liquid;
S4, the freeze drying of S3 gained microparticle suspending liquid is obtained to the multivesicular liposome containing squalene and astaxanthin composition.
7. according to claim 6 containing the preparation method of the multivesicular liposome of squalene and astaxanthin composition, it is characterized in that, the aqueous solution that contains surfactant described in S2 be by surfactant and water according to (20～30): 100 mass ratio is mixed to get.
8. according to claim 6 containing the preparation method of the multivesicular liposome of squalene and astaxanthin composition, it is characterized in that, the process conditions of high speed homogenizing are :≤2000r/min described in S2, stirring 30min.
9. according to claim 6 containing the preparation method of the multivesicular liposome of squalene and astaxanthin composition, it is characterized in that, cryodesiccated process conditions are described in S4 :-25 DEG C of freezing 1h, 6 × 10
-4freeze drying 8h under Pa.
10. the multivesicular liposome containing squalene and astaxanthin composition that the arbitrary described method of claim 6-9 prepares.
Described in 11. claims 1～5 or 10 any one, contain the application of the multivesicular liposome of squalene and astaxanthin composition, it is characterized in that, in cigarette filter tip rod forming process, described multivesicular liposome is made an addition in the cigarette filter of acetate fiber.
12. according to described in claim 11 containing the multivesicular liposome of squalene and astaxanthin composition application, it is characterized in that, contain the multivesicular liposome of squalene and astaxanthin composition described in built-in 0.5～1.5 gram of every cigarette filter.
13. according to described in claim 12 containing the multivesicular liposome of squalene and astaxanthin composition application, it is characterized in that, contain the multivesicular liposome of squalene and astaxanthin composition described in built-in 0.8 gram of every cigarette filter.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105686079A (en) * | 2016-03-07 | 2016-06-22 | 云南瑞升烟草技术（集团）有限公司 | Preparation method of paper filter material capable of reducing gas-phase free radicals in smoke |
| CN105725270A (en) * | 2016-03-07 | 2016-07-06 | 云南瑞升烟草技术（集团）有限公司 | Preparation method of astaxanthin particles and application thereof in cigarette filter sticks |
| CN106666824A (en) * | 2016-12-28 | 2017-05-17 | 云南中烟工业有限责任公司 | Grape polyphenols nano liposome cigarette filter tip material and application thereof |
| CN106723349A (en) * | 2016-12-28 | 2017-05-31 | 云南中烟工业有限责任公司 | A kind of olive polyphenol nano liposomes composite membrane and its application in cigarette |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1449746A (en) * | 2003-05-07 | 2003-10-22 | 蒋家驹 | Soft capsule containing trace element |
| WO2006014035A1 (en) * | 2004-08-06 | 2006-02-09 | Biospectrum, Inc. | Multiple layered liposome and preparation method thereof |
| US20080113031A1 (en) * | 2004-09-27 | 2008-05-15 | Joey Moodley | Minicapsule Formulations |
| CN102061174A (en) * | 2010-10-29 | 2011-05-18 | 华南农业大学 | Squalene and tea polyphenol composition and application thereof in cigarettes |
| CN102079979A (en) * | 2010-12-08 | 2011-06-01 | 华南农业大学 | Composition of squalene and beta-carotene and application thereof in cigarettes |
-
2014
- 2014-03-20 CN CN201410104907.2A patent/CN103859588B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1449746A (en) * | 2003-05-07 | 2003-10-22 | 蒋家驹 | Soft capsule containing trace element |
| WO2006014035A1 (en) * | 2004-08-06 | 2006-02-09 | Biospectrum, Inc. | Multiple layered liposome and preparation method thereof |
| US20080113031A1 (en) * | 2004-09-27 | 2008-05-15 | Joey Moodley | Minicapsule Formulations |
| CN102061174A (en) * | 2010-10-29 | 2011-05-18 | 华南农业大学 | Squalene and tea polyphenol composition and application thereof in cigarettes |
| CN102079979A (en) * | 2010-12-08 | 2011-06-01 | 华南农业大学 | Composition of squalene and beta-carotene and application thereof in cigarettes |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105686079A (en) * | 2016-03-07 | 2016-06-22 | 云南瑞升烟草技术（集团）有限公司 | Preparation method of paper filter material capable of reducing gas-phase free radicals in smoke |
| CN105725270A (en) * | 2016-03-07 | 2016-07-06 | 云南瑞升烟草技术（集团）有限公司 | Preparation method of astaxanthin particles and application thereof in cigarette filter sticks |
| CN106666824A (en) * | 2016-12-28 | 2017-05-17 | 云南中烟工业有限责任公司 | Grape polyphenols nano liposome cigarette filter tip material and application thereof |
| CN106723349A (en) * | 2016-12-28 | 2017-05-31 | 云南中烟工业有限责任公司 | A kind of olive polyphenol nano liposomes composite membrane and its application in cigarette |
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| CN103859588B (en) | 2016-04-13 |
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