CN104262540B - A kind of temperature and pH double-response xylan based aquagel and preparation method thereof and application - Google Patents
A kind of temperature and pH double-response xylan based aquagel and preparation method thereof and application Download PDFInfo
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Abstract
The invention belongs to natural polymer functional material preparing technical field, disclose a kind of temperature and pH double-response xylan based aquagel and preparation method and application.The preparation process of described temperature and pH double-response xylan based aquagel is: by xylan with hot water dissolving, obtain xylan solution；N N-isopropylacrylamide and acrylamide is added in xylan solution, add cross-linking agent, logical nitrogen bubble, adds light trigger, after mix homogeneously, it is cooled to room temperature, it is placed in ultraviolet radiation reactor, ultra-vioket radiation under room temperature, then closes placing response at room temperature, reaction is washed with deionized after terminating, and gained solid is described temperature and pH double-response xylan based aquagel.Preparation method technique of the present invention easily operates, and has environment friendly；Gained temperature and pH double-response xylan based aquagel have biocompatibility, have good slow release behavior to medicine, reach 80% in simulation intestinal physiology liquid Chinese medicine burst size.
Description
Technical field
The invention belongs to natural polymer functional material preparing technical field, be specifically related to a kind of temperature and pH is double
Heavily response xylan based aquagel and preparation method and application.
Background technology
The hemicellulose that the plant in the whole world generates every year has 3.5 × 1010More than t.Hemicellulose be on the earth
One of abundant, the most cheap Renewable resource, is inexhaustible, the nexhaustible Renewable resource of nature.
Hemicellulose, because of its wide material sources, has the spies such as biodegradability, biocompatibility, special physiological activity
Point, is the rationality raw material preparing material.Xylan, as the main component of hemicellulose, is primarily present in wealthy
In Ye Mu and grass.Xylan itself has what other natural polymers such as cellulose, starch did not had
Special physicochemical property, has potential using value in pharmaceuticals industry.
Hydrogel is a kind of network-like polymer of three-dimensional hydrophilic, can absorb large quantity of moisture or biofluid, but
Water fast.Hydrogel can keep certain retentiveness and resilience.It is each that this characteristic gives hydrogel
Plant special performance, there is various different respondent behavior, such as pH value, temperature, illumination, magnetic field etc..Water
The characteristic that gel is had, has wide application in sewage disposal, pharmaceutical engineering field.
Especially corresponding with temperature to the pH hydrogel of the hydrogel (intelligent aqueous gel capable) of environmental response becomes for people
Have the focus of research.Temperature sensitive type water gel is the one of intellectual material.Turning mutually at temperature-sensitive hydrogel
Temperature (lower critical solution temperature, LCST) is applied around a little variations in temperature, and the volume of gel is grand
To undergo mutation in sight.The performance of this uniqueness of temperature-sensitive hydrogel makes it in biomaterial and biotechnology side
Face shows wide application prospect, such as drug controlled release, micro-load cell culture material, biomolecule
Identify material, apart material, chemical sensor, temperature-sensitive micro-biochip etc..It addition, pH response
Intelligent aqueous gel capable pH value is had bigger respondent behavior, human body different parts such as stomach, intestinal and blood vessel
PH value is different, and therefore the hydrogel of pH response can also realize medicine targeted controlled-release.Up to the present,
Yet there are no temperature and pH sensitive hydrogel prepared by the hemicellulose about xylan type and be applied to
The report of medicament slow release.
Summary of the invention
In order to overcome the shortcoming of prior art with not enough, the primary and foremost purpose of the present invention be to provide a kind of temperature and
The preparation method of pH double-response xylan based aquagel；
The temperature that another object of the present invention is to provide above-mentioned preparation method to obtain and pH double-response wood gather
Glycosyl hydrogel；
It is still another object of the present invention to provide said temperature and pH double-response xylan based aquagel should
With.
The purpose of the present invention is achieved through the following technical solutions:
A kind of temperature and the preparation method of pH double-response xylan based aquagel, comprise the steps:
(1) by xylan with hot water dissolving, xylan solution is obtained；
(2) in xylan solution, add NIPA and acrylamide, add cross-linking agent,
Logical nitrogen bubble, adds light trigger, after mix homogeneously, is cooled to room temperature, is placed in ultraviolet radiation reactor
In, ultra-vioket radiation under room temperature, then close placing response at room temperature, reaction is washed with deionized after terminating
Removing residual reaction reagent, gained solid is described temperature and pH double-response xylan based aquagel.
Preferably, step (1) is described by the xylan concrete operations of hot water dissolving is: added by xylan
Temperature is in the hot water of 60～80 DEG C, stirring and dissolving 15～40min；
Preferably, step (1) described xylan is spruce wood polysaccharide, and molecular weight is Mw=130000g/mol；
Preferably, the mass concentration of the xylan solution of step (1) gained is 4%～6%；
Preferably, step (2) described cross-linking agent is N, N '-methylene-bisacrylamide；Step (2) is described
Light trigger is dimethoxybenzoin；
Preferably, the consumption of step (2) described cross-linking agent is the 6%～10% of step (1) described xylan quality；
Preferably, step (2) described acrylamide is (8～16) with the mass ratio of step (1) described xylan:
1；
Preferably, the consumption of step (2) described NIPA is step (1) described xylan
The 8%～15% of quality；
Preferably, the consumption of step (2) described light trigger is the 5% of step (1) described xylan quality；
Described light trigger, before adding xylan solution, first dissolves with N-Methyl pyrrolidone (NMP)；
Preferably, the time of the described logical nitrogen bubble of step (2) is 10～30min；
Preferably, the time of step (2) described ultra-vioket radiation is 4～8h, and wavelength is 365nm, and power is
400W；
Preferably, the time of step (2) described closing placing response is 8～20h.
A kind of temperature and pH double-response xylan based aquagel is obtained according to above-mentioned preparation method；
Said temperature and the application in preparing medicinal slow release agent of the pH double-response xylan based aquagel；
Said temperature and the application in preparing medicinal slow release agent of the pH double-response xylan based aquagel, specifically
Comprising the steps: to be dissolved in ethanol medicine, preparation obtains medicine-ethanol solution, by described temperature and pH
Double-response xylan based aquagel impregnated in medicine-ethanol solution, seals, and is placed in dark place and places 20～28h,
Take out, be placed in vacuum drying oven and be dried, obtain the medicine aqueogel with slow release effect；
The medicine aqueogel with slow release effect of gained can delay Slow release in gastrointestinal environment.
In the concrete steps of above-mentioned application:
Preferably, described medicine is aspirin；
Preferably, the mass concentration of described medicine-ethanol solution is 8～15%；
Preferably, described temperature and pH double-response xylan based aquagel before dipping, first uniformly slicing,
Lyophilization；Described lyophilization is lyophilization 24 hours at-50 DEG C；
Preferably, the temperature being dried in described vacuum tank is 40～60 DEG C, and drying time is 20～28h；
The present invention has such advantages as relative to prior art and effect:
(1) raw material that preparation method of the present invention uses is biomass, because of xylan itself has can be biological
Degraded, biocompatibility and special physicochemical property, be to prepare the preferable raw material of medical aquogel, this
The bright commercial Application that can expand xylan type hemicellulose, the higher value application for hemicellulose provides weight
The effective way wanted.
(2) present invention prepare to temperature and pH double-response xylan based aquagel, medicine is had well
Medicament slow release behavior, reach 80% in intestinal Chinese medicine slow release efficiency.
(3) preparation method technique of the present invention easily operates, and easily realizes technology, has environment friendly.
Accompanying drawing explanation
Fig. 1 is the DSC figure of temperature of the present invention and pH double-response xylan based aquagel.
Fig. 2 be the medicine aqueogel with slow release effect of the present invention pH be 7.4 simulated intestinal fluids and
PH is the medicament slow release figure under the gastric juice physiological liquid environment of 2.0 simulations.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to
This.
Embodiment 1
A kind of temperature and pH double-response xylan based aquagel, its preparation process is as follows:
Weigh 2.5g xylan (xylan) to be placed in there-necked flask, add 50mL deionized water 80 DEG C of heating
30min stirring make it dissolve；It is cooled to 50 DEG C, is then respectively adding the NIPA of 0.25g
(NIPA), 25g acrylamide (AM) and 0.25g N, N '-methylene-bisacrylamide (MBA), use nitrogen
Gas bell 15min, to remove air in the dissolved oxygen in solution and bottle；It is subsequently adding light trigger Benzoinum two
(being first dissolved in N-Methyl pyrrolidone by dimethoxybenzoin 0.125g, mass concentration is methyl ether 0.125g
2.5%)；After mixed liquor is uniform, it is down to room temperature, pours silica dish into and be placed in ultraviolet radiation reactor, set
Irradiation condition is: wavelength is 365nm, power is 400W, irradiates 6h under room temperature；Reach after the response time
Close under room temperature and place 12h so that it is fully polymerization and crosslinking；After having reacted, the hydrogel of gained is taken out
With excess deionized water wash to remove reaction reagent remaining in hydrogel, obtain described temperature and pH is dual
Response xylan based aquagel.
Temperature and pH double-response xylan based aquagel to gained carry out heat analysis, and gained thermal analysis curue is composed
(DSC figure) as it is shown in figure 1, from Fig. 1 the temperature after flat molten swollen and pH double-response xylan base water-setting
Glue to temperature at the thermal analysis curve of 10～60 DEG C it can be seen that gained temperature and pH double-response xylan Ji Shui
There is a thin and sharp-pointed absworption peak at 35.2 DEG C in gel, illustrates to there occurs phase in version at 35.2 DEG C.
Gained temperature and pH double-response xylan based aquagel are used for drug encapsulation and slow release, concrete steps
For: preparation mass concentration is the aspirin-ethanol solution of 10%；By gained temperature and pH double-response wood
Polysaccharide based aquagel uniformly slicing, lyophilization 24 hours at-50 DEG C, then impregnated in aspirin second
Alcoholic solution, seals, and is placed in dark place and places 24h, take out, is put in 40 DEG C of vacuum drying ovens and is dried 24h,
To the medicine aqueogel with slow release effect.
The medicine aqueogel that gained has slow release effect is placed in simulation human gastric juice (pH is 2.0) and intestinal
In the physiological environment that liquid (pH is 7.4) is different, level concussion (50r/min), took 5ml every 1 hour molten
Liquid, and take same amount of buffer and put back to wherein to maintain total liquor capacity constant.Buffer is now with the current.
The concentration of medium Chinese medicine is measured by ultraviolet spectrophotometer method.
According to following formula calculating pharmaceutical pack carrying capacity and medicament slow release rate:
Pharmaceutical pack carrying capacity (W0)=Bao Zaihou hydrogel quality-Bao Zaiqian hydrogel quality；
Medicament slow release rate (%)=Wt/W0× 100% (WtFor drug quality g, W after t hour0For total drug encapsulation
Amount is g)；
It is calculated analytically, temperature and the pH double-response low Critical Solution of xylan based aquagel in embodiment 1
Temperature (LCST) is 35.2 DEG C；Medicine aspirin is 8h slow release balance in simulated intestinal fluid, and slow release rate reaches
80%, 6 hours slow release balances in simulated gastric fluid, slow release rate is 45%.Gained has the medicine of slow release effect
Aqueogel medicine under pH is 7.4 simulated intestinal fluids and gastric juice physiological liquid environment that pH is 2.0 simulations delays
Release figure as shown in Figure 2.
The DSC figure of example below product and slow release rate figure are the most same as in Example 1, illustrate the most one by one.
Embodiment 2
A kind of temperature and pH double-response xylan based aquagel, its preparation process is as follows:
Weigh 3.0g xylan (xylan) to be placed in there-necked flask, add 50mL deionized water 60 DEG C of heating
40min stirring make it dissolve；It is cooled to 50 DEG C, is then respectively adding the NIPA of 0.45g
(NIPA), 24g acrylamide (AM) and 0.18g N, N '-methylene-bisacrylamide (MBA), use nitrogen
Gas bell 30min, to remove air in the dissolved oxygen in solution and bottle；It is subsequently adding light trigger Benzoinum two
Dimethoxybenzoin 0.15g (is first dissolved in N-Methyl pyrrolidone, mass concentration is 2.5%) by methyl ether 0.15g；
After mixed liquor is uniform, it is down to room temperature, pours silica dish into and be placed in ultraviolet radiation reactor, set and irradiate bar
Part is: wavelength is 365nm, power is 400W, irradiates 8h under room temperature；Reach after the response time at room temperature
Close and place 20h so that it is fully polymerization and crosslinking；After having reacted, by the hydrogel taking-up excess of gained
Deionized water wash, to remove reaction reagent remaining in hydrogel, obtains described temperature and pH double-response wood
Polysaccharide based aquagel.
Gained temperature and pH double-response xylan based aquagel are used for drug encapsulation and slow release, concrete steps
For: preparation mass concentration is the aspirin-ethanol solution of 8%；Gained temperature and pH double-response wood are gathered
Glycosyl hydrogel uniformly slicing, lyophilization 24 hours at-50 DEG C, then impregnated in aspirin ethanol
Solution, seals, and is placed in dark place and places 20h, take out, is put in 60 DEG C of vacuum drying ovens and is dried 20h, obtain
There is the medicine aqueogel of slow release effect.
The medicine aqueogel that gained has slow release effect is placed in simulation human gastric juice (pH is 2.0) and intestinal
In the physiological environment that liquid (pH is 7.4) is different, level concussion (50r/min), took 5ml every 1 hour molten
Liquid, and take same amount of buffer and put back to wherein to maintain total liquor capacity constant.Buffer is now with the current.
The concentration of medium Chinese medicine is measured by ultraviolet spectrophotometer method.
It is calculated analytically, temperature and the pH double-response low Critical Solution of xylan based aquagel in embodiment 2
Temperature (LCST) is 34.3 DEG C；Medicine aspirin 6h medicament slow release rate in simulated intestinal fluid reaches 68%,
In simulated gastric fluid, 4h slow release rate is 35%.
Embodiment 3
A kind of temperature and pH double-response xylan based aquagel, its preparation process is as follows:
Weigh 3.0g xylan (xylan) to be placed in there-necked flask, add 75mL deionized water 70 DEG C of heating
15min stirring make it dissolve；It is cooled to 50 DEG C, is then respectively adding the NIPA of 0.24g
(NIPA), 45g acrylamide (AM) and 0.24g N, N '-methylene-bisacrylamide (MBA), use nitrogen
Gas bell 10min, to remove air in the dissolved oxygen in solution and bottle；It is subsequently adding light trigger Benzoinum two
Dimethoxybenzoin 0.15g (is first dissolved in N-Methyl pyrrolidone, mass concentration is 2.5%) by methyl ether 0.15g；
After mixed liquor is uniform, it is down to room temperature, pours silica dish into and be placed in ultraviolet radiation reactor, set and irradiate bar
Part is: wavelength is 365nm, power is 400W, irradiates 4h under room temperature；Reach after the response time at room temperature
Close and place 8h so that it is fully polymerization and crosslinking；After having reacted, by the hydrogel taking-up excess of gained
Deionized water wash, to remove reaction reagent remaining in hydrogel, obtains described temperature and pH double-response wood
Polysaccharide based aquagel.
Gained temperature and pH double-response xylan based aquagel are used for drug encapsulation and slow release, concrete steps
For: preparation mass concentration is the aspirin-ethanol solution of 15%；By gained temperature and pH double-response wood
Polysaccharide based aquagel uniformly slicing, lyophilization 24 hours at-50 DEG C, then impregnated in aspirin second
Alcoholic solution, seals, and is placed in dark place and places 28h, take out, is put in 50 DEG C of vacuum drying ovens and is dried 28h,
To the medicine aqueogel with slow release effect.
The medicine aqueogel that gained has slow release effect is placed in simulation human gastric juice (pH is 2.0) and intestinal
In the physiological environment that liquid (pH is 7.4) is different, level concussion (50r/min), took 5ml every 1 hour molten
Liquid, and take same amount of buffer and put back to wherein to maintain total liquor capacity constant.Buffer is now with the current.
The concentration of medium Chinese medicine is measured by ultraviolet spectrophotometer method.
It is calculated analytically, temperature and the pH double-response low Critical Solution of xylan based aquagel in embodiment 2
Temperature (LCST) is 35.0 DEG C；Medicine aspirin 7h medicament slow release rate in simulated intestinal fluid reaches 76%,
In simulated gastric fluid, 5h slow release rate is 40%.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-mentioned enforcement
The restriction of example, the change made, modifies, replaces under other any spirit without departing from the present invention and principle
In generation, combine, simplify, all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (10)
1. a temperature and the preparation method of pH double-response xylan based aquagel, it is characterised in that: bag
Include following steps:
(1) by xylan with hot water dissolving, xylan solution is obtained；
(2) in xylan solution, add NIPA and acrylamide, add cross-linking agent,
Logical nitrogen bubble, adds light trigger, after mix homogeneously, is cooled to room temperature, is placed in ultraviolet radiation reactor
In, ultra-vioket radiation under room temperature, then close placing response at room temperature, reaction is washed with deionized after terminating
Removing residual reaction reagent, gained solid is described temperature and pH double-response xylan based aquagel.
A kind of temperature the most according to claim 1 and the preparation of pH double-response xylan based aquagel
Method, it is characterised in that: step (1) is described by the xylan concrete operations of hot water dissolving is: gathered by wood
Sugar adds in the hot water that temperature is 60～80 DEG C, stirring and dissolving 15～40min.
A kind of temperature the most according to claim 1 and the preparation of pH double-response xylan based aquagel
Method, it is characterised in that: the mass concentration of the xylan solution of step (1) gained is 4%～6%.
A kind of temperature the most according to claim 1 and the preparation of pH double-response xylan based aquagel
Method, it is characterised in that: step (2) described cross-linking agent is N, N '-methylene-bisacrylamide；Step (2)
Described light trigger is dimethoxybenzoin.
A kind of temperature the most according to claim 1 and the preparation of pH double-response xylan based aquagel
Method, it is characterised in that: the consumption of step (2) described cross-linking agent is step (1) described xylan quality
6%～10%；Step (2) described acrylamide is (8～16) with the mass ratio of step (1) described xylan:
1；The consumption of step (2) described NIPA is step (1) described xylan quality
8%～15%；The consumption of step (2) described light trigger is the 5% of step (1) described xylan quality.
A kind of temperature the most according to claim 1 and the preparation of pH double-response xylan based aquagel
Method, it is characterised in that: the time of the described logical nitrogen bubble of step (2) is 10～30min；Step (2)
The time of described closing placing response is 8～20h.
7. one kind according to the temperature described in any one of claim 1～6 and pH double-response xylan base water-setting
The preparation method of glue obtains temperature and pH double-response xylan based aquagel.
Temperature the most according to claim 7 and pH double-response xylan based aquagel are preparing medicine
Application in slow releasing agent.
Application the most according to claim 8, it is characterised in that: specifically include following steps: by medicine
Being dissolved in ethanol, preparation obtains medicine-ethanol solution, by described temperature and pH double-response xylan Ji Shui
Immersing hydrogels, in medicine-ethanol solution, seals, and is placed in dark place and places 20～28h, takes out, and is placed in vacuum and does
Dry case is dried, obtains the medicine aqueogel with slow release effect.
Application the most according to claim 9, it is characterised in that: described medicine is aspirin；
The mass concentration of described medicine-ethanol solution is 8～15%；Described temperature and pH double-response xylan Ji Shui
Gel before dipping, first uniformly slicing, lyophilization；The temperature being dried in described vacuum tank is 40～60 DEG C,
Drying time is 20～28h.
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| CN105596289A (en) * | 2015-12-29 | 2016-05-25 | 华南理工大学 | Drug sustained release hydrogel carrier and preparing method and application thereof |
| CN106279541B (en) * | 2016-08-17 | 2019-01-18 | 华南理工大学 | A kind of magnetic coupling hydrogel and the preparation method and application thereof for magnetic control fixed point heating source |
| CN106279542B (en) * | 2016-08-22 | 2018-11-02 | 华南理工大学 | A kind of dual network Nanometer composite hydrogel and its preparation and application based on xylan |
| CN107298736A (en) * | 2017-05-16 | 2017-10-27 | 河南工业大学 | A kind of preparation method of pawpaw seeds matrix pH value sensitive type hydrogel |
| CN111961230A (en) * | 2020-08-31 | 2020-11-20 | 江南大学 | Arabinoxylan hydrogel with pH responsiveness and preparation method thereof |
| CN113398273B (en) * | 2021-05-14 | 2022-07-19 | 广西壮族自治区中国科学院广西植物研究所 | Application of xylan derivative as hydrophilic sustained-release material in preparation of drug sustained-release tablets |
| CN114702693A (en) * | 2022-04-12 | 2022-07-05 | 武汉纺织大学 | Synthesis method and application of trehalose-modified PNIPAm temperature-sensitive intelligent hydrogel |
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