CN104893010A - Preparation method of pH-sensitive type hydrogel - Google Patents
Preparation method of pH-sensitive type hydrogel Download PDFInfo
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- CN104893010A CN104893010A CN201510271545.0A CN201510271545A CN104893010A CN 104893010 A CN104893010 A CN 104893010A CN 201510271545 A CN201510271545 A CN 201510271545A CN 104893010 A CN104893010 A CN 104893010A
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Abstract
The invention discloses a preparation method of pH-sensitive type hydrogel. The preparation method comprises the following steps: mixing and dispersing sodium alginate with mass fraction of 1.5% (w/v, similarly hereinafter), 0.9% of gelatin, 0.1% of fish skin collagen and 0.1% of agar into 100mL of distilled water; sufficiently stirring in a 60-DEG C water bath; carrying out 400W ultrasonic treatment until sodium alginate and the gelatin are sufficiently dissolved, wherein the hardness and the elasticity of the hydrogel can be increased by adopting the gelatin, the dissolving of the sodium alginate and the gelatin can be quickened through the ultrasonic treatment, and de-foaming effect is achieved, 0.3% of calcium carbonate is added as a gelling agent, and 0.6% of glucolactone is used as a slow-release preparation of calcium ions; quickly stirring to prepare a turbid liquid, immediately pouring the turbid liquid into a mould and standing and forming gel at 4 DEG C. The shape of the mould can be determined according to the production needs. The pH-sensitive type hydrogel prepared by the method is uniform and stable in texture and good in shape, and has swelling rates of 3.28%, 26.31% and 34.25% 50 minutes after simulating gastric juice, intestinal juice and colon juice.
Description
Technical field
The present invention relates to food processing technology field, be specifically related to a kind of preparation method of pH sensitive hydrogel.
Background technology
The calcium gel of sodium alginate has good bioaffinity, is widely used as control-released agent.For improving its controlled release properties, chemical modification can be carried out to sodium alginate, or carrying out composite with other materials, to slow down the swelling rate of hydrogel.Chemical modification process is loaded down with trivial details, and need add organic reagent, and production cost is higher and be unfavorable for HUMAN HEALTH.By sodium alginate with carry out composite with the superpolymer of opposite charges, the compactness that electrostatic interaction improves hydrogel network structure can be led to, from improving its controlled release properties, as the composite aquogel of sodium alginate and chitosan.And it is at present less about adopting sodium alginate and gelatin to prepare the report of composite aquogel.
The sodium alginate that massfraction is higher and gelatin not soluble, and colloidal sol viscosity is higher, easily residual bubble.Supersound process can play the effect promoting dissolving and froth breaking, is conducive to enhancing productivity, and ensures the homogeneity of hydrogel.
The calcium chloride that adopts as the jelling agent of sodium alginate more at present, but under the effect of free ca, sodium alginate plastic is too fast, easily causes hydrogel quality uneven, and form is difficult to control.Present method adopts calcium carbonate as jelling agent, adopts Gluconolactone as the sustained release dosage of calcium ion, suitably slows down the gelation rate of sodium alginate, extend the operable time of reverse mould.In addition, calcium ion can be evenly distributed in hydrogel, makes the quality stable homogeneous of hydrogel.
Summary of the invention
The invention provides a kind of preparation method of pH sensitive hydrogel, object improves the controlled release properties of sodium alginate calcium gel, and make it have certain form.
For achieving the above object, the present invention is achieved by the following technical solutions:
A preparation method for pH sensitive hydrogel, is made into colloidal sol by sodium alginate, gelatin, adds calcium carbonate, Gluconolactone is made into suspension liquid under ultrasonication, leaves standstill plastic after pouring mould into.
Further improvement to technique scheme: in described colloidal sol, sodium alginate massfraction is 1.5%, and gelatin massfraction is 0.9%, and solvent temperature is 60 DEG C, and ultrasonic power is 400W.
Further improvement to technique scheme: in described suspension liquid, the massfraction of calcium carbonate is 0.3%, the massfraction of Gluconolactone is 0.6%.
Further improvement to technique scheme: the shape of described mould can be determined according to Production requirement, described gelling temperature is 4 DEG C.
Further improvement to technique scheme: described pH responsive type type hydrogel quality stable homogeneous, form are good, and the swelling ratio in simulated gastric fluid, intestinal fluid and colonic fluid after 50min is respectively 3.28%, 26.31% and 34.25%.
Compared with prior art, advantage of the present invention and technique effect are: the present invention is compared to ordinary method, and prepared pH sensitive hydrogel quality stable homogeneous, have certain form, controlled release properties is good.
Add appropriate amounts of gelatin, increase the consistency and elasticity of hydrogel.
In sol-process, carry out supersound process, play the effect promoting dissolving and froth breaking, can raise the efficiency, ensure the homogeneity of hydrogel.
Adopt calcium carbonate as jelling agent, adopt Gluconolactone as the sustained release dosage of calcium ion.Suitably slow down the gelation rate of sodium alginate, extend the operable time of reverse mould.In addition, calcium ion can be evenly distributed in hydrogel, makes the quality stable homogeneous of hydrogel.
The present invention contributes to the exploitation deepening hydrogel.PH sensitive hydrogel quality stable homogeneous of the present invention, form are good, and the swelling ratio in simulated gastric fluid, intestinal fluid and colonic fluid after 50min is respectively 3.28%, 26.31% and 34.25%.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described in detail:
The present invention can select for the preparation of the sodium alginate of pH sensitive hydrogel, gelatin, Gluconolactone the commercially available prod that on market, company produces.Such as: sodium alginate is optional purchased from Qingdao Mingyue Marine Alga Group Corp., Ltd., gelatin is optional purchased from Tian Xin Food Co., Ltd of Qingdao City, and Gluconolactone is optional purchased from Anhui Xingzhou Medicine Food Co., Ltd..
Embodiment 1
Calcium carbonate adds test---and calcium carbonate massfraction affects pH sensitive hydrogel hardness.Solvent temperature is 60 DEG C, and ultrasonic power is 400W, and Gluconolactone massfraction is 0.6%, gelling temperature 4 DEG C.
Table 1 calcium carbonate massfraction is on the impact of pH sensitive hydrogel hardness
As shown in Table 1, when calcium carbonate massfraction lower than 0.3% time, pH sensitive hydrogel hardness raises with the increase of calcium carbonate massfraction.Calcium carbonate massfraction higher than 0.3% time, gel hardness change is little.This illustrates that the calcium carbonate of certain mass mark is conducive to improving the hardness of pH sensitive hydrogel.
Embodiment 2
Gluconolactone adds test---and Gluconolactone massfraction affects the release rate of calcium ion, thus affects the hardness of pH sensitive hydrogel.Solvent temperature is 60 DEG C, and ultrasonic power is 400W, and calcium carbonate massfraction is 0.3%, gelling temperature 4 DEG C.
Table 2 Gluconolactone massfraction is on the impact of pH sensitive hydrogel hardness
As shown in Table 2, when Gluconolactone massfraction lower than 0.6% time, pH sensitive hydrogel hardness raises with the increase of calcium carbonate massfraction.Gluconolactone massfraction higher than 0.6% time, gel hardness change is little.This illustrates that the Gluconolactone massfraction of certain mass mark is conducive to improving the hardness of pH sensitive hydrogel.
Embodiment 3
Gelatin adds test---and gelatin massfraction affects elasticity and the hardness of pH sensitive hydrogel.By measuring the storage modulus (G ') of pH sensitive hydrogel, out-of-phase modulus (G "), dissipation factor (tan δ), evaluate its structural stability.Solvent temperature is 60 DEG C, and ultrasonic power is 400W, and calcium carbonate addition is 0.3%, and Gluconolactone massfraction is 0.6%, gelling temperature 4 DEG C, and oscillation frequency is 0.1Hz.
The elasticity of table 3 gelatin massfraction on pH sensitive hydrogel and the impact of hardness
As shown in Table 3, along with the increase of gelatin massfraction, gel elastomer is in rising trend, gel hardness, G', G ", tan δ first increases rear reduction.When gelatin addition is 0.9%, gel elastomer reaches 0.955, and gel hardness reaches 905g, G', G, and " reach maximum value respectively, tan δ is minimum value.This illustrates that the gelatin of certain mass mark is conducive to improving the consistency and elasticity of pH sensitive type gel, increases the stability of gel structure.
Embodiment 4
Controlled release properties is tested---and gelatin massfraction affects the controlled release properties of pH sensitive hydrogel.Simulated gastric fluid is the HCl solution of pH 1.2, and simulated intestinal fluid is pH 6.8, the phosphoric acid buffer of simulation colonic fluid pH 7.4.
The controlled release properties of table 4 pH sensitive hydrogel
The controlled release properties of table 4 pH sensitive hydrogel
As shown in Table 4, along with the increase of gelatin massfraction, under the fluid environment of different pH, swelling the taking the lead in of hydrogel increases rear reduction.When gelatin massfraction is 0.9%, the swelling ratio of hydrogel in simulated gastric fluid is lower, and the swelling ratio in simulated intestinal fluid, simulated intestinal fluid reaches maximum value respectively.This illustrates that the gelatin of certain mass mark is conducive to the controlled release properties improving hydrogel.
Above embodiment only in order to technical scheme of the present invention to be described, but not is limited; Although with reference to previous embodiment to invention has been detailed description, for the person of ordinary skill of the art, still can modify to the technical scheme described in previous embodiment, or equivalent replacement is carried out to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of the present invention's technical scheme required for protection.
Claims (5)
1. a preparation method for pH sensitive hydrogel, is characterized in that: sodium alginate, gelatin, collagen of fish skin and agar are made into colloidal sol under ultrasonication, add calcium carbonate, Gluconolactone is made into suspension liquid, leaves standstill plastic after pouring mould into.
2. the preparation method of pH sensitive hydrogel according to claim 1, it is characterized in that: in described colloidal sol, sodium alginate massfraction is 1.5%, gelatin massfraction is 0.9%, collagen of fish skin massfraction is 0.1%, agar massfraction is 0.1%, and solvent temperature is 60 DEG C, and ultrasonic power is 400W.
3. the preparation method of a kind of pH sensitive hydrogel according to claim 1 and 2, is characterized in that: in described suspension liquid, the massfraction of calcium carbonate is 0.3%, the massfraction of Gluconolactone is 0.6%.
4. the preparation method of a kind of pH sensitive hydrogel according to claim 1 or 3, is characterized in that: the shape of described mould can be determined according to Production requirement, and described gelling temperature is 4 DEG C.
5. the preparation method of a kind of pH sensitive hydrogel according to claim 1, it is characterized in that: described Compositional type hydrogel quality stable homogeneous, form are good, and the swelling ratio in simulated gastric fluid, intestinal fluid and colonic fluid after 50min is respectively 3.28%, 26.31% and 34.25%.
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| CN108685791A (en) * | 2018-07-26 | 2018-10-23 | 上海沃必盛生物科技有限公司 | A kind of carrier-free mixed-forming moisturizing gel mask and preparation method thereof |
| CN109589885A (en) * | 2018-12-18 | 2019-04-09 | 西南石油大学 | A kind of preparation method of monodispersity oil-containing sodium alginate microcapsule |
| CN110823882A (en) * | 2019-12-05 | 2020-02-21 | 吉林农业大学 | Antifreezing gel state indicating material, application and preparation method thereof |
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| CN113652386B (en) * | 2021-07-08 | 2023-04-25 | 重庆理工大学 | Rigidity-controllable three-dimensional porous gel scaffold material and preparation method and application thereof |
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| CN109589885A (en) * | 2018-12-18 | 2019-04-09 | 西南石油大学 | A kind of preparation method of monodispersity oil-containing sodium alginate microcapsule |
| CN110823882A (en) * | 2019-12-05 | 2020-02-21 | 吉林农业大学 | Antifreezing gel state indicating material, application and preparation method thereof |
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