CN106000344A - Preparation method of composite membrane absorbing cholesterol - Google Patents
Preparation method of composite membrane absorbing cholesterol Download PDFInfo
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- CN106000344A CN106000344A CN201610479202.8A CN201610479202A CN106000344A CN 106000344 A CN106000344 A CN 106000344A CN 201610479202 A CN201610479202 A CN 201610479202A CN 106000344 A CN106000344 A CN 106000344A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
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Abstract
The invention discloses a preparation method of a composite membrane absorbing cholesterol. According to the preparation method, zein and beta-cyclodextrin (beta-CD) serve as main raw materials, a water solution of ethyl alcohol serves as a solvent, and ethylene glycol diglycidyl ether (EGDE) serves as a crosslinking agent. The beta-cyclodextrin is immobilized on zein molecules through the effect of the crosslinking agent, and a compound is obtained through heating dissolution, pH regulation, purification, freeze drying and other processes; then, the prepared compound is subjected to dissolution, heating, defoaming and other processes to prepare the composite membrane absorbing cholesterol. The composite membrane integrates the advantages of excellent film-forming properties, biocompatibility, biodegradability, good mechanical strength and the like of the zein and the inclusion recognition performance of the beta-cyclodextrin, the prepared composite membrane has stabile properties and a good adsorption effect, the raw materials are rich in source, the preparation method is simple and environmentally friendly, and industrial production is easy to achieve.
Description
[technical field]: the invention belongs to field of material preparation, is specifically related to the system of a kind of composite membrane adsorbing cholesterol
Preparation Method.
[background technology]: cholesterol, also known as cholesterol, is the derivant of a kind of cyclopentanoperhy drophenanthrene, is widely present in animal
Internal, especially with the abundantest in brain and nervous tissue.Cholesterol is the indispensable important substance of animal tissue cell, and it is not
It is only involved in forming cell membrane, and is synthetic bile acid, vitamin D and the raw material of steroid hormone, therefore, gallbladder in blood of human body
Sterin content and human health have close contacting.Blood cholesterol level increases, and cardiovascular disease incidence can be caused several
Rate improves.Cholesterol in blood can pile up formation fritter in blood vessel wall, makes blood vessel wall swell, makes blood vessel thicken, blood
Pipe will become relative narrowness, and the pressure of blood vessel wall can rise, and blood pressure can raise, and can cause atherosclerosis simultaneously.Although
Many medicines reducing cholesterol occur the most, but from the standpoint of nutrient health, it is desirable to can be from diet
Do, reduced by non-drug approach the purpose of cholesterol.
At present, the method for removing Food Cholesterol mainly has: (solvent extraction, supercritical extraction, water steam Physical
Steam distillation method, active carbon adsorption etc.), chemical method (stick with paste by the extracting of succinic anhydrides esterification process, composite electromagnetic method, emulsion, β-ring
Spermatophore buries), bioanalysis (cholesterol oxidase oxidizing process, microorganism directly utilizes, lactic acid bacteria assimilation etc.).Wherein, profit
Most having application prospect by the method for membrance separation absorption cholesterol, its effect and safety are the highest.
Zein (Zein) is the storage protein of a kind of Semen Maydis, and it is similar to Apis cerana Fabricius, and softness, ductility are good, hard
Tough, flexible, there is the advantages such as preferable dissolution characteristics, film property, thermostability, non-oxidizability and biocidal property.Zein is due to tool
There is the feature such as film property, biocompatibility, biological degradability and barrier of excellence, be widely used in packaging for foodstuff and fresh-keeping
Field.Zein is amphipathic protein, has hydrophobic and hydrophilic nmature simultaneously, has helical wheel model, at a protein
In molecule, 9 similar repetitives arrange and pass through hydrogen bond stable existence in antiparallel mode, and little or nothing is the most right
Claim.Owing to its molecular weight, the degree of polymerization are different with chemical constitution, by three-dimensional network, interaction of hydrogen bond, hydrophobic interaction and
Disulfide bond between protein chain stabilizes it existence, and therefore, zein shows good filming performance.
Beta-schardinger dextrin-(β-CD) is the cyclic oligosaccharide that a kind of 7 glucose molecules connected by 1-4 α-glycosidic bond form,
It has the cavity of a diameter 60-65nm shape such as conduit, has the special molecular structure of " interior hydrophobic, outer hydrophilic ", can conduct
Different " object " compound of " host " envelope.At present, both at home and abroad in the report about reduction Cholesterol in Foods, Chen Rucai
Successfully removing the cholesterol in egg yolk Deng employing beta-cyclodextrin inclusion compound method, removal efficiency reaches 92.23%;Li Xiangxin etc. are former with Adeps Sus domestica
Material, selects beta-cyclodextrin inclusion compound method, silica gel adsorption and molecularly distilled that Adeps Sus domestica carries out removing cholesterol, and analyzes 3 kinds
Method removing cholesterol effect;Chinese patent CN105504295A discloses the " system of a kind of starch immobilized beta-schardinger dextrin-adsorbent
Preparation Method ", with soluble starch and beta-schardinger dextrin-as raw material, prepare a kind of adsorbing separation effective, stable in properties, favorable reproducibility
Adsorbing material.
Zein is had as macromolecule carrier skeleton the inclusion of the advantages such as good film property and mechanical strength and β-CD
Recognition performance combines, and prepares a kind of stable in properties, adsorbing separation excellent effect, favorable reproducibility, and low cost, and technique is simple
Membrane material have become as reduce cholesterol research field in the urgent need to.
[summary of the invention]: for the deficiencies in the prior art, the present invention provides a kind of and has adsorbing separation cholesterol function
The preparation method of zein/ β-CD composite membrane, prepared composite membrane stable in properties, advantages of good adsorption effect, and abundant raw material source, preparation
Method is simple and environmentally-friendly, it is easy to accomplish industrialized production.
For reaching this purpose, the technology path that the present invention uses is:
1. the synthesis of zein/beta-schardinger dextrin-complex
(1) zein and beta-schardinger dextrin-are joined in 250ml there-necked flask for 20%-60% in mass ratio,
Adding 60% (v/v) ethanol solution, under the condition of water bath heating that temperature is 45 DEG C, the rotating speed machinery with 500rpm/min stirs
Mix and make its rapid solution;
(2) by the NaOH solution of 1mol/L, zein/ β-CD mixed solution pH is adjusted to 8.7;
(3) the zein/ β-CD mixed solution mixing up pH is slowly added to quantitative cross-linking agent Ethylene glycol diglycidyl ether,
With the rotating speed mechanic whirl-nett reaction 4h of 100rpm/min under the condition of water bath heating that temperature is 45 DEG C;
(4) prepare 1.0% (w/w) NaCl solution of certain volume, be placed on 4 DEG C of refrigerators.Obtain for precipitating in (3)
Reactant liquor, and be washed with deionized, purify;
(5) product obtained after purifying after lyophilization 12h, obtains containing β-CD different content at-50 DEG C
Zein complex.
2. the preparation of zein/beta-schardinger dextrin-composite membrane
(1) mould is made.It is 1mm, 5.5cm × 5.5cm's that the adhesive tape thick with 1mm and polytetrafluoroethylene make the degree of depth
Film die, makes 4 equivalently-sized moulds.
(2) zein and the zein/ β-CD complex weighing certain mass respectively joins in 100ml there-necked flask, then depends on
The ethanol solution of secondary addition 95% (v/v), glycerol, with the rotating speed of 100rpm/min under the condition of water bath heating that temperature is 80 DEG C
Mechanical agitation 1h makes its rapid solution, and after boiling, deaeration is stand-by;
(3) solution that will prepare in (2), takes same volume and is slowly injected into respectively in mould.Mould is put into vacuum drying
In case, 25 DEG C of dry 24h;
(4), after film carefully being taken off from mould, put in sealing bag, preserve stand-by.
The present invention, by immobilized for the β-CD composite membrane to adsorbing separation cholesterol prepared on zein, not only remains the bag of β-CD
Knot recognition performance, and have the advantages such as the good stability of macromolecule carrier skeleton, mechanical performance and biocompatibility concurrently, available
In the numerous food such as milk, egg field.And raw material sources of the present invention are wide, low cost, preparation process is simple, to environment friend
Good, it is easy to accomplish industrialized production.
[accompanying drawing explanation]
Fig. 1 is zein/ β-CD complex preparating mechanism
Fig. 2 is the SEM figure of zein/ β-CD composite film surface
Fig. 3 is the SEM figure of zein/ β-CD composite membrane section
[specific embodiments]
Embodiment 1:
1. the synthesis of zein/beta-schardinger dextrin-complex
(1) weigh zein 3g to join in 250ml there-necked flask, add 150ml 60% (v/v) ethanol
Solution, under the condition of water bath heating that temperature is 45 DEG C, the rotating speed mechanical agitation with 500rpm/min makes its rapid solution;
(2) by the NaOH solution of 1mol/L, zein pH value of solution is adjusted to 8.7;
(3) the zein solution mixing up pH is slowly added to 0.75ml Ethylene glycol diglycidyl ether, is 45 DEG C in temperature
With the rotating speed mechanic whirl-nett reaction 4h of 100rpm/min under condition of water bath heating;
(4) preparation 150ml 1.0% (w/w) NaCl solution, is placed on 4 DEG C of refrigerators.For precipitating obtain in (3) anti-
Answer liquid, and be washed with deionized, purify;
(5) product obtained after purifying is at-50 DEG C after lyophilization 12h, and obtaining containing β-CD content is 0%
Zein/ β-CD complex.
2. the preparation of zein/beta-schardinger dextrin-composite membrane
(1) mould is made.It is 1mm, 5.5cm × 5.5cm's that the adhesive tape thick with 1mm and polytetrafluoroethylene make the degree of depth
Film die, makes 4 equivalently-sized moulds.
(2) weigh the zein/ β-CD complex that 1.5g β-CD content is 0% respectively and join in 100ml there-necked flask,
Sequentially add the ethanol solution of 10ml 95% (v/v), 0.3g glycerol, under the condition of water bath heating that temperature is 80 DEG C with
Rotating speed mechanical agitation 1h of 100rpm/min makes its rapid solution, and after boiling, deaeration is stand-by;
(3) solution that will prepare in (2), takes same volume and is slowly injected into respectively in mould.Mould is put into vacuum drying
In case, 25 DEG C of dry 24h;
(4), after film carefully being taken off from mould, put in sealing bag, preserve stand-by.
Embodiment 2:
1. the synthesis of zein/beta-schardinger dextrin-complex
(1) weigh zein 3g and beta-schardinger dextrin-0.6g respectively to join in 250ml there-necked flask, add
150ml60% (v/v) ethanol solution, with the rotating speed mechanical agitation of 500rpm/min under the condition of water bath heating that temperature is 45 DEG C
Make its rapid solution;
(2) by the NaOH solution of 1mol/L, zein/ β-CD mixed solution pH is adjusted to 8.7;
(3) the zein/ β-CD mixed solution mixing up pH is slowly added to 0.75ml Ethylene glycol diglycidyl ether, in temperature
It is the rotating speed mechanic whirl-nett reaction 4h with 100rpm/min under the condition of water bath heating of 45 DEG C;
(4) preparation 150ml 1.0% (w/w) NaCl solution, is placed on 4 DEG C of refrigerators.For precipitating obtain in (3) anti-
Answer liquid, and be washed with deionized, purify;
(5) product obtained after purifying is at-50 DEG C after lyophilization 12h, and obtaining containing β-CD content is 20%
Zein/ β-CD complex.
2. the preparation of zein/beta-schardinger dextrin-composite membrane
(1) mould is made.It is 1mm, 5.5cm × 5.5cm's that the adhesive tape thick with 1mm and polytetrafluoroethylene make the degree of depth
Film die, makes 4 equivalently-sized moulds.
(2) weigh the zein/ β-CD complex that 1.5g β-CD content is 20% respectively and join in 100ml there-necked flask,
Sequentially add the ethanol solution of 10ml 95% (v/v), 0.3g glycerol, under the condition of water bath heating that temperature is 80 DEG C with
Rotating speed mechanical agitation 1h of 100rpm/min makes its rapid solution, and after boiling, deaeration is stand-by;
(3) solution that will prepare in (2), takes same volume and is slowly injected into respectively in mould.Mould is put into vacuum drying
In case, 25 DEG C of dry 24h;
(4), after film carefully being taken off from mould, put in sealing bag, preserve stand-by.
Embodiment 3:
1. the synthesis of zein/beta-schardinger dextrin-complex
(1) weigh zein 3g and beta-schardinger dextrin-1.2g respectively to join in 250ml there-necked flask, add
150ml 60% (v/v) ethanol solution, under the condition of water bath heating that temperature is 45 DEG C, the rotating speed machinery with 500rpm/min stirs
Mix and make its rapid solution;
(2) by the NaOH solution of 1mol/L, zein/ β-CD mixed solution pH is adjusted to 8.7;
(3) the zein/ β-CD mixed solution mixing up pH is slowly added to 0.75ml Ethylene glycol diglycidyl ether, in temperature
It is the rotating speed mechanic whirl-nett reaction 4h with 100rpm/min under the condition of water bath heating of 45 DEG C;
(4) preparation 150ml 1.0% (w/w) NaCl solution, is placed on 4 DEG C of refrigerators.For precipitating obtain in (3) anti-
Answer liquid, and be washed with deionized, purify;
(5) product obtained after purifying is at-50 DEG C after lyophilization 12h, and obtaining containing β-CD content is 40%
Zein/ β-CD complex.
2. the preparation of zein/beta-schardinger dextrin-composite membrane
(1) mould is made.It is 1mm, 5.5cm × 5.5cm's that the adhesive tape thick with 1mm and polytetrafluoroethylene make the degree of depth
Film die, makes 4 equivalently-sized moulds.
(2) weigh the zein/ β-CD complex that 1.5g β-CD content is 40% respectively and join in 100ml there-necked flask,
Sequentially add the ethanol solution of 10ml 95% (v/v), 0.3g glycerol, under the condition of water bath heating that temperature is 80 DEG C with
Rotating speed mechanical agitation 1h of 100rpm/min makes its rapid solution, and after boiling, deaeration is stand-by;
(3) solution that will prepare in (2), takes same volume and is slowly injected into respectively in mould.Mould is put into vacuum drying
In case, 25 DEG C of dry 24h;
(4), after film carefully being taken off from mould, put in sealing bag, preserve stand-by.
Embodiment 4:
1. the synthesis of zein/beta-schardinger dextrin-complex
(1) weigh zein 3g and beta-schardinger dextrin-1.8g respectively to join in 250ml there-necked flask, add
150ml 60% (v/v) ethanol solution, under the condition of water bath heating that temperature is 45 DEG C, the rotating speed machinery with 500rpm/min stirs
Mix and make its rapid solution;
(2) by the NaOH solution of 1mol/L, zein/ β-CD mixed solution pH is adjusted to 8.7;
(3) the zein/ β-CD mixed solution mixing up pH is slowly added to 0.75ml Ethylene glycol diglycidyl ether, in temperature
It is the rotating speed mechanic whirl-nett reaction 4h with 100rpm/min under the condition of water bath heating of 45 DEG C;
(4) preparation 150ml 1.0% (w/w) NaCl solution, is placed on 4 DEG C of refrigerators.For precipitating obtain in (3) anti-
Answer liquid, and be washed with deionized, purify;
(5) product obtained after purifying is at-50 DEG C after lyophilization 12h, and obtaining containing β-CD content is 60%
Zein/ β-CD complex.
2. the preparation of zein/beta-schardinger dextrin-composite membrane
(1) mould is made.It is 1mm, 5.5cm × 5.5cm's that the adhesive tape thick with 1mm and polytetrafluoroethylene make the degree of depth
Film die, makes 4 equivalently-sized moulds.
(2) weigh the zein/ β-CD complex that 1.5g β-CD content is 60% respectively and join in 100ml there-necked flask,
Sequentially add the ethanol solution of 10ml 95% (v/v), 0.3g glycerol, under the condition of water bath heating that temperature is 80 DEG C with
Rotating speed mechanical agitation 1h of 100rpm/min makes its rapid solution, and after boiling, deaeration is stand-by;
(3) solution that will prepare in (2), takes same volume and is slowly injected into respectively in mould.Mould is put into vacuum drying
In case, 25 DEG C of dry 24h;
(4), after film carefully being taken off from mould, put in sealing bag, preserve stand-by.
Claims (6)
1. adsorb a preparation method for the composite membrane of cholesterol, comprise the steps:
1) synthesis of zein/beta-schardinger dextrin-complex
1. zein and beta-schardinger dextrin-are joined in 250ml there-necked flask for 20%-60% in mass ratio, add
60% (v/v) ethanol solution, under the condition of water bath heating that temperature is 45 DEG C, the rotating speed mechanical agitation with 500rpm/min makes it
Rapid solution;
2. by the NaOH solution of 1mol/L, zein/ β-CD mixed solution pH is adjusted to 8.7;
3. the zein/ β-CD mixed solution mixing up pH is slowly added to quantitative cross-linking agent Ethylene glycol diglycidyl ether, in temperature
Degree is the rotating speed mechanic whirl-nett reaction 4h under the condition of water bath heating of 45 DEG C with 100rpm/min;
4. prepare 1.0% (w/w) NaCl solution of certain volume, be placed on 4 DEG C of refrigerators.The reaction obtained in precipitating 3.
Liquid, and be washed with deionized, purify;
5. the product obtained after purifying after lyophilization 12h, obtains the zein containing β-CD different content and is combined at-50 DEG C
Thing.
2) preparation of zein/beta-schardinger dextrin-composite membrane
1. mould is made.The adhesive tape thick with 1mm and polytetrafluoroethylene make the film forming that the degree of depth is 1mm, 5.5cm × 5.5cm
Mould, makes 4 equivalently-sized moulds.
Zein and the zein/ β-CD complex weighing certain mass the most respectively joins in 100ml there-necked flask, sequentially adds
The ethanol solution of 95% (v/v), glycerol, under the condition of water bath heating that temperature is 80 DEG C, the rotating speed machinery with 100rpm/min stirs
Mixing 1h and make its rapid solution, after boiling, deaeration is stand-by;
3. the solution that will prepare in 2., takes same volume and is slowly injected into respectively in mould.Mould is put into vacuum drying oven, 25
DEG C dry 24h;
4., after film carefully being taken off from mould, put in sealing bag, preserve stand-by.
The preparation method of a kind of composite membrane adsorbing cholesterol the most according to claim 1, it is characterised in that: with zein and
β-CD is raw material, with ethanol solution as solvent, is prepared immobilized for β-CD by cross-linking agent diglycidyl ether of ethylene glycol on zein
Composite membrane.
The preparation method of a kind of composite membrane adsorbing cholesterol the most according to claim 1, it is characterised in that: described β-
It is 20%-60% that CD accounts for the mass percent of zein, and cross-linking agent diglycidyl ether of ethylene glycol consumption is 0.75ml.
The preparation method of a kind of composite membrane adsorbing cholesterol the most according to claim 1, its characteristic is: used
Cross-linking agent is diglycidyl ether of ethylene glycol, is the functional cross-links agent with epoxide group of a kind of end, can be used for crosslinking protein
Matter.
The preparation method of a kind of composite membrane adsorbing cholesterol the most according to claim 1, its characteristic is: glycerol is for increasing
Mould agent, for increasing the toughness of composite membrane.
The preparation method of a kind of composite membrane adsorbing cholesterol the most according to claim 1, it is characterised in that: zein/ β-
The reaction temperature of CD complex is 45 DEG C, and the response time is 4h;When preparing composite membrane, reaction temperature is 80 DEG C, and the response time is
1h。
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1302550A (en) * | 2000-01-01 | 2001-07-11 | 天津商学院 | Process for preparing alcohol-soluble corn protein membrane from corn gluten |
CN1411904A (en) * | 2001-10-08 | 2003-04-23 | 吴文腾 | Immobilized beta-cyclodextrin and method for removing cholesterol and triglyceride |
CN1490349A (en) * | 2002-10-15 | 2004-04-21 | 浙江大学 | Preparation of chitin-beta-cyclodextrin resin |
CN105504295A (en) * | 2015-12-21 | 2016-04-20 | 广西大学 | Preparation method of starch immobilized beta-cyclodextrin adsorbing agent |
-
2016
- 2016-06-27 CN CN201610479202.8A patent/CN106000344A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1302550A (en) * | 2000-01-01 | 2001-07-11 | 天津商学院 | Process for preparing alcohol-soluble corn protein membrane from corn gluten |
CN1411904A (en) * | 2001-10-08 | 2003-04-23 | 吴文腾 | Immobilized beta-cyclodextrin and method for removing cholesterol and triglyceride |
CN1490349A (en) * | 2002-10-15 | 2004-04-21 | 浙江大学 | Preparation of chitin-beta-cyclodextrin resin |
CN105504295A (en) * | 2015-12-21 | 2016-04-20 | 广西大学 | Preparation method of starch immobilized beta-cyclodextrin adsorbing agent |
Non-Patent Citations (3)
Title |
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徐晖等: "油酸与甘油对玉米醇溶蛋白膜机械性能的影响及机理探讨", 《包装与机械》 * |
戴荣继等: "生物活性环糊精衍生化蛋白质的合成", 《北京理工大学学报》 * |
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