CN117815108A - Preparation method of gellan gum self-adhesive spray gel based on polyphenol induction - Google Patents
Preparation method of gellan gum self-adhesive spray gel based on polyphenol induction Download PDFInfo
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- 229920002148 Gellan gum Polymers 0.000 title claims abstract description 114
- 235000010492 gellan gum Nutrition 0.000 title claims abstract description 107
- 239000000216 gellan gum Substances 0.000 title claims abstract description 107
- 239000007921 spray Substances 0.000 title claims abstract description 73
- 239000000853 adhesive Substances 0.000 title claims abstract description 64
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 46
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 46
- 230000006698 induction Effects 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 76
- 239000012213 gelatinous substance Substances 0.000 claims abstract description 20
- 238000011065 in-situ storage Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012670 alkaline solution Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005576 amination reaction Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 229920005615 natural polymer Polymers 0.000 claims abstract description 4
- 239000002861 polymer material Substances 0.000 claims abstract description 4
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- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 8
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 8
- QAIPRVGONGVQAS-DUXPYHPUSA-N trans-caffeic acid Chemical compound OC(=O)\C=C\C1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-DUXPYHPUSA-N 0.000 claims description 8
- WMBWREPUVVBILR-WIYYLYMNSA-N (-)-Epigallocatechin-3-o-gallate Chemical compound O([C@@H]1CC2=C(O)C=C(C=C2O[C@@H]1C=1C=C(O)C(O)=C(O)C=1)O)C(=O)C1=CC(O)=C(O)C(O)=C1 WMBWREPUVVBILR-WIYYLYMNSA-N 0.000 claims description 4
- ACEAELOMUCBPJP-UHFFFAOYSA-N (E)-3,4,5-trihydroxycinnamic acid Natural products OC(=O)C=CC1=CC(O)=C(O)C(O)=C1 ACEAELOMUCBPJP-UHFFFAOYSA-N 0.000 claims description 4
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 4
- 239000001263 FEMA 3042 Substances 0.000 claims description 4
- WMBWREPUVVBILR-UHFFFAOYSA-N GCG Natural products C=1C(O)=C(O)C(O)=CC=1C1OC2=CC(O)=CC(O)=C2CC1OC(=O)C1=CC(O)=C(O)C(O)=C1 WMBWREPUVVBILR-UHFFFAOYSA-N 0.000 claims description 4
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 4
- QNVSXXGDAPORNA-UHFFFAOYSA-N Resveratrol Natural products OC1=CC=CC(C=CC=2C=C(O)C(O)=CC=2)=C1 QNVSXXGDAPORNA-UHFFFAOYSA-N 0.000 claims description 4
- LUKBXSAWLPMMSZ-OWOJBTEDSA-N Trans-resveratrol Chemical compound C1=CC(O)=CC=C1\C=C\C1=CC(O)=CC(O)=C1 LUKBXSAWLPMMSZ-OWOJBTEDSA-N 0.000 claims description 4
- 235000010208 anthocyanin Nutrition 0.000 claims description 4
- 229930002877 anthocyanin Natural products 0.000 claims description 4
- 239000004410 anthocyanin Substances 0.000 claims description 4
- 150000004636 anthocyanins Chemical class 0.000 claims description 4
- 229940074360 caffeic acid Drugs 0.000 claims description 4
- 235000004883 caffeic acid Nutrition 0.000 claims description 4
- QAIPRVGONGVQAS-UHFFFAOYSA-N cis-caffeic acid Natural products OC(=O)C=CC1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-UHFFFAOYSA-N 0.000 claims description 4
- 229960003638 dopamine Drugs 0.000 claims description 4
- 229940030275 epigallocatechin gallate Drugs 0.000 claims description 4
- 235000004515 gallic acid Nutrition 0.000 claims description 4
- 229940074391 gallic acid Drugs 0.000 claims description 4
- 235000021283 resveratrol Nutrition 0.000 claims description 4
- 229940016667 resveratrol Drugs 0.000 claims description 4
- 235000015523 tannic acid Nutrition 0.000 claims description 4
- 229920002258 tannic acid Polymers 0.000 claims description 4
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims description 4
- 229940033123 tannic acid Drugs 0.000 claims description 4
- 239000002537 cosmetic Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims 6
- 239000000499 gel Substances 0.000 abstract description 61
- 239000000017 hydrogel Substances 0.000 abstract description 24
- 239000003814 drug Substances 0.000 abstract description 8
- 230000003110 anti-inflammatory effect Effects 0.000 abstract description 2
- 230000003078 antioxidant effect Effects 0.000 abstract description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- 239000000463 material Substances 0.000 description 18
- FPDWHGAQJGAILQ-UHFFFAOYSA-N C(O)(O)=O.[N+](=O)([O-])C1=CC=CC=C1.[N+](=O)([O-])C1=CC=CC=C1 Chemical compound C(O)(O)=O.[N+](=O)([O-])C1=CC=CC=C1.[N+](=O)([O-])C1=CC=CC=C1 FPDWHGAQJGAILQ-UHFFFAOYSA-N 0.000 description 14
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 14
- 238000001338 self-assembly Methods 0.000 description 8
- BWKIBIZZLRPKFY-UHFFFAOYSA-N 1,2,3-benzothiadiazole-5-carbaldehyde Chemical compound O=CC1=CC=C2SN=NC2=C1 BWKIBIZZLRPKFY-UHFFFAOYSA-N 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 238000010494 dissociation reaction Methods 0.000 description 7
- 230000005593 dissociations Effects 0.000 description 7
- 238000004108 freeze drying Methods 0.000 description 7
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- 239000000126 substance Substances 0.000 description 4
- 229940079593 drug Drugs 0.000 description 3
- 210000002850 nasal mucosa Anatomy 0.000 description 3
- 241000282898 Sus scrofa Species 0.000 description 2
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- 241000282887 Suidae Species 0.000 description 1
- 206010052428 Wound Diseases 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 125000003916 ethylene diamine group Chemical group 0.000 description 1
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Landscapes
- Medicinal Preparation (AREA)
Abstract
The invention discloses a preparation method of self-adhesive spray gel based on polyphenol induction gellan gum, which comprises the following steps: amination is carried out on natural polymer material gellan gum by ethylenediamine to prepare aminated gellan gum; heating and dissolving the aminated gellan gum in water, and cooling to room temperature to obtain a gelatinous substance; adding an alkaline solution into the gelatinous substance, and dissociating the gelatinous substance into a uniform aminated gellan gum solution; adding a polyphenol solution into the aminated gellan gum solution, so that the solution self-assembles in situ under the induction of polyphenol to generate self-adhesive spray gel. The self-adhesive spray gel prepared by the invention has the property of shear thinning, so that the self-adhesive spray gel can be applied in a spray form, is simple to prepare and high in biological safety, and can be used as a drug carrier in the field of medicine; meanwhile, the hydrogel has good adhesion and anti-inflammatory and antioxidant properties due to the introduction of polyphenol.
Description
Technical Field
The invention belongs to the field of hydrogel materials and medical preparations, and particularly relates to a preparation method of self-adhesive spray gel based on gellan gum induced by polyphenol.
Background
The hydrogel is a three-dimensional hydrophilic polymer crosslinked network structure, and is gradually developed and applied by industries such as tissue engineering, biological medicine, soft electronics and the like due to the characteristics of good biocompatibility, physical and chemical properties, high water absorbability, high water retention and the like, and particularly in the aspect of biological medicine materials, the hydrogel is widely used as a carrier of slow release medicines due to the abundant crosslinked network structure and good swellability. Spray gels are increasingly used in the biomedical field because of their high mixing efficiency, controllable spray area, and sufficient contact of the atomized droplets with soft tissue. Spray gel facilitates the treatment of open wounds. However, achieving rapid gelation without external stimulus, as well as a combination of functional and biological activity of self-assembled hydrogels, is a challenge.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a preparation method of self-adhesive spray gel based on polyphenol-induced gellan gum.
The invention discloses a preparation method of self-adhesive spray gel based on polyphenol induction gellan gum, which comprises the following steps:
step 1: the natural polymer material gellan gum is aminated by ethylenediamine to prepare aminated gellan gum.
Step 2: the aminated gellan gum is heated in water to dissolve and cooled to room temperature to obtain a gum-like substance.
Step 3: an alkaline solution is added to the gum material, which is dissociated into a homogeneous aminated gellan gum solution.
Step 4: adding a polyphenol solution into the aminated gellan gum solution, so that the solution self-assembles in situ under the induction of polyphenol to generate self-adhesive spray gel.
Further, the aminated gellan gum is ethylenediamine grafted gellan gum.
Further, the heating temperature of the aminated gellan gum is 70-90 ℃; heating for 30-70 min; cooling to 20-30 deg.c.
Further, the polyphenol is one of tannic acid, dopamine, resveratrol, anthocyanin, gallic acid, caffeic acid and epigallocatechin gallate.
The invention relates to a preparation method of self-adhesive spray gel based on polyphenol induction, which comprises the following main components: 0.4 to 1wt.% of amination gellan gum solution, 8 to 12 pH value alkaline solution and 0.5 to 40wt.% of polyphenol solution, wherein the volume ratio of the three is 90 to 96:3 to 6:1 to 4.
The self-adhesive spray gel prepared by the preparation method based on the polyphenol-induced gellan gum base can be used as a drug carrier in the field of medicine or in the field of cosmetics.
The beneficial technical effects of the invention are as follows:
(1) The self-adhesive spray gel prepared by the invention has strong applicability, can be used as a delivery carrier for most medicaments, and can be widely applied to the fields of medicines and cosmetics.
(2) The preparation method of the self-adhesive spray gel based on the gellan gum induced by polyphenol, disclosed by the invention, is capable of inducing the self-assembly of the aminated gellan gum by the polyphenol, forming hydrogel through hydrogen bonding, and is high in biological safety, and an additional cross-linking agent is not needed.
(3) The self-adhesive spray gel prepared by the invention has the shear thinning property, and can generate hydrogel in situ after passing through a nozzle. The introduction of polyphenol endows hydrogel with good adhesiveness, can enhance the retention time of the hydrogel on the surface of the tissue, and prolongs the administration time.
(4) The self-adhesive spray gel prepared by the invention can realize anti-inflammatory and antioxidant effects by utilizing the biological function advantages of polyphenol without adding medicines.
Drawings
FIG. 1 is a physical view of the self-adhesive spray gel prepared in example 1 in a spray bottle.
FIG. 2 is a diagram showing the self-adhesive spray gel prepared in example 1 as sprayed from a spray bottle.
FIG. 3 is a diagram showing the adhered substance of the self-adhesive spray gel prepared in example 1 on pigskin.
Fig. 4 is a graph showing the adhesion of the self-adhesive spray gel prepared in example 2 to the nasal mucosa of swine.
FIG. 5 is an alternate step-strain sweep curve for the self-adhesive spray gel prepared in example 1.
Fig. 6 is a strain sweep curve of the self-adhesive spray gel prepared in example 3.
Fig. 7 is a strain sweep curve of the self-adhesive spray gel prepared in example 4.
Fig. 8 is a strain sweep curve of the self-adhesive spray gel prepared in example 5.
Fig. 9 is a strain sweep curve of the self-adhesive spray gel prepared in example 6.
Fig. 10 is a strain sweep curve of the self-adhesive spray gel prepared in example 7.
Detailed Description
The invention will now be described in further detail with reference to the drawings and to specific examples.
The invention discloses a preparation method of self-adhesive spray gel based on polyphenol induction gellan gum, which comprises the following steps:
step 1: the natural polymer material gellan gum is aminated by ethylenediamine to prepare aminated gellan gum.
Step 2: the aminated gellan gum is heated in water to dissolve and cooled to room temperature to obtain a gum-like substance.
Step 3: an alkaline solution is added to the gum material, which is dissociated into a homogeneous aminated gellan gum solution.
Step 4: adding a polyphenol solution into the aminated gellan gum solution, so that the solution self-assembles in situ under the induction of polyphenol to generate self-adhesive spray gel.
Example 1:
the embodiment provides a preparation method of self-adhesive spray gel based on polyphenol induction gellan gum, which comprises the following specific steps:
step 1: and (3) preparing the aminated gellan gum.
1g of gellan gum was added to 100mL of dimethyl sulfoxide and heated at 60℃with stirring overnight to dissolve. Bis (4-nitrobenzene) carbonate having a molar ratio of 1 to gellan gum repeating units was added to the above solution, reacted at 60℃for 4 hours, then ethylenediamine monohydrate having a molar mass 10 times that of bis (4-nitrobenzene) carbonate was added, and the reaction was continued at 60℃for 3 hours. And (3) precipitating and separating a product by using acetone after the reaction is finished, repeatedly washing the product by using acetone for several times, and freeze-drying the product to obtain the aminated gellan gum.
Step 2: dissociation of the aminated gellan gum-like material.
60mg of aminated gellan gum is weighed and dissolved in 10mL of deionized water at 90 ℃, the solution is fully stirred until the solution is clear and transparent, and then the solution is cooled to be a gelatinous substance at room temperature, so as to obtain the aminated gellan gum gelatinous substance. To the aminated gellan gum material was added 0.4mL of 0.1M sodium hydroxide solution and the hydrogel was dissociated into a homogeneous solution.
Step 3: and preparing the self-adhesive spray gel by using polyphenol to induce gellan gum.
And adding 0.2mL of 6wt.% epigallocatechin gallate solution into the dissociated solution, and performing in-situ self-assembly on the dissociated solution under the induction of the epigallocatechin gallate to form the hydrogel.
The hydrogel in the spray bottle is shown in FIG. 1.
FIG. 2 is a diagram showing the self-adhesive spray gel prepared in this example as sprayed from a spray bottle. As can be seen from the figures, the self-adhesive spray gel prepared by the invention has shear thinning property, can be sprayed out from a nozzle in a spray form and is glued again.
FIG. 3 is a diagram showing the physical adhesion of the self-adhesive spray gel prepared in this example to pigskin. As can be seen from the figure, the self-adhesive spray gel prepared by the invention has adhesive force with pigskin, and can bear the distortion of the pigskin without deformation.
FIG. 5 is an alternate step-strain sweep curve for a self-adhering spray gel prepared in this example. From the figure, it can be seen that the self-adhesive spray gel prepared by the invention has excellent self-healing property.
Example 2:
the embodiment provides a preparation method of self-adhesive spray gel based on polyphenol induction gellan gum, which comprises the following specific steps:
step 1: and (3) preparing the aminated gellan gum.
1g of gellan gum was added to 100mL of dimethyl sulfoxide and heated at 60℃with stirring overnight to dissolve. Bis (4-nitrobenzene) carbonate having a molar ratio of 1 to gellan gum repeating units was added to the above solution, reacted at 60℃for 4 hours, then ethylenediamine monohydrate having a molar mass 10 times that of bis (4-nitrobenzene) carbonate was added, and the reaction was continued at 60℃for 3 hours. And (3) precipitating and separating a product by using acetone after the reaction is finished, repeatedly washing the product by using acetone for several times, and freeze-drying the product to obtain the aminated gellan gum.
Step 2: dissociation of the aminated gellan gum-like material.
60mg of aminated gellan gum is weighed and dissolved in 10mL of deionized water at 90 ℃, the solution is fully stirred until the solution is clear and transparent, and then the solution is cooled to be a gelatinous substance at room temperature, so as to obtain the aminated gellan gum gelatinous substance. To the aminated gellan gum material was added 0.4mL of 0.1M sodium hydroxide solution and the hydrogel was dissociated into a homogeneous solution.
Step 3: and preparing the self-adhesive spray gel by using polyphenol to induce gellan gum.
And adding 0.1mL of 30wt.% tannic acid solution into the dissociated solution, and performing in-situ self-assembly on the dissociated solution under the induction of tannic acid to generate the hydrogel.
Fig. 4 is a diagram showing the adhesion of the self-adhesive spray gel prepared in this example to the nasal mucosa of swine. From the figure, the self-adhesive spray gel prepared by the invention can be adhered on the nasal mucosa of pigs and does not slide off.
Example 3:
the embodiment provides a preparation method of self-adhesive spray gel based on polyphenol induction gellan gum, which comprises the following specific steps:
step 1: and (3) preparing the aminated gellan gum.
1g of gellan gum was added to 100mL of dimethyl sulfoxide and heated at 60℃with stirring overnight to dissolve. Bis (4-nitrobenzene) carbonate having a molar ratio of 1 to gellan gum repeating units was added to the above solution, reacted at 60℃for 4 hours, then ethylenediamine monohydrate having a molar mass 10 times that of bis (4-nitrobenzene) carbonate was added, and the reaction was continued at 60℃for 3 hours. And (3) precipitating and separating a product by using acetone after the reaction is finished, repeatedly washing the product by using acetone for several times, and freeze-drying the product to obtain the aminated gellan gum.
Step 2: dissociation of the aminated gellan gum-like material.
60mg of aminated gellan gum is weighed and dissolved in 10mL of deionized water at 90 ℃, the solution is fully stirred until the solution is clear and transparent, and then the solution is cooled to be a gelatinous substance at room temperature, so as to obtain the aminated gellan gum gelatinous substance. To the aminated gellan gum material was added 0.4mL of 0.1M sodium hydroxide solution and the hydrogel was dissociated into a homogeneous solution.
Step 3: and preparing the self-adhesive spray gel by using polyphenol to induce gellan gum.
And adding 0.2mL of 10wt.% dopamine solution into the dissociated solution, and performing in-situ self-assembly on the dissociated solution under the induction of dopamine to form the hydrogel.
FIG. 6 is a graph showing strain sweep of the self-adhesive spray gel prepared in this example, showing gel properties with storage modulus greater than loss modulus over the strain range of 0.1-39%.
Example 4:
the embodiment provides a preparation method of self-adhesive spray gel based on polyphenol induction gellan gum, which comprises the following specific steps:
step 1: and (3) preparing the aminated gellan gum.
1g of gellan gum was added to 100mL of dimethyl sulfoxide and heated at 60℃with stirring overnight to dissolve. Bis (4-nitrobenzene) carbonate having a molar ratio of 1 to gellan gum repeating units was added to the above solution, reacted at 60℃for 4 hours, then ethylenediamine monohydrate having a molar mass 10 times that of bis (4-nitrobenzene) carbonate was added, and the reaction was continued at 60℃for 3 hours. And (3) precipitating and separating a product by using acetone after the reaction is finished, repeatedly washing the product by using acetone for several times, and freeze-drying the product to obtain the aminated gellan gum.
Step 2: dissociation of the aminated gellan gum-like material.
60mg of aminated gellan gum is weighed and dissolved in 10mL of deionized water at 90 ℃, the solution is fully stirred until the solution is clear and transparent, and then the solution is cooled to be a gelatinous substance at room temperature, so as to obtain the aminated gellan gum gelatinous substance. To the aminated gellan gum material was added 0.4mL of 0.1M sodium hydroxide solution and the hydrogel was dissociated into a homogeneous solution.
Step 3: and preparing the self-adhesive spray gel by using polyphenol to induce gellan gum.
And adding 0.2mL of 3wt.% resveratrol solution into the dissociated solution, and performing in-situ self-assembly on the dissociated solution under the induction of resveratrol to generate hydrogel.
Fig. 7 is a strain sweep curve of the self-adhesive spray gel prepared in this example, and it can be seen from the figure that the storage modulus is greater than the loss modulus in the strain range of 0.1 to 175%, showing the gel properties.
Example 5:
the embodiment provides a preparation method of self-adhesive spray gel based on polyphenol induction gellan gum, which comprises the following specific steps:
step 1: and (3) preparing the aminated gellan gum.
1g of gellan gum was added to 100mL of dimethyl sulfoxide and heated at 60℃with stirring overnight to dissolve. Bis (4-nitrobenzene) carbonate having a molar ratio of 1 to gellan gum repeating units was added to the above solution, reacted at 60℃for 4 hours, then ethylenediamine monohydrate having a molar mass 10 times that of bis (4-nitrobenzene) carbonate was added, and the reaction was continued at 60℃for 3 hours. And (3) precipitating and separating a product by using acetone after the reaction is finished, repeatedly washing the product by using acetone for several times, and freeze-drying the product to obtain the aminated gellan gum.
Step 2: dissociation of the aminated gellan gum-like material.
60mg of aminated gellan gum is weighed and dissolved in 10mL of deionized water at 90 ℃, the solution is fully stirred until the solution is clear and transparent, and then the solution is cooled to be a gelatinous substance at room temperature, so as to obtain the aminated gellan gum gelatinous substance. To the aminated gellan gum material was added 0.4mL of 0.1M sodium hydroxide solution and the hydrogel was dissociated into a homogeneous solution.
Step 3: and preparing the self-adhesive spray gel by using polyphenol to induce gellan gum.
And adding 0.2mL of 6wt.% anthocyanin solution into the dissociated solution, and performing in-situ self-assembly on the dissociated solution under the induction of anthocyanin to generate the hydrogel.
Fig. 8 is a strain sweep curve of the self-adhesive spray gel prepared in this example, and it can be seen from the figure that the storage modulus is greater than the loss modulus in the strain range of 0.1 to 369%, showing the gel properties.
Example 6:
the embodiment provides a preparation method of self-adhesive spray gel based on polyphenol induction gellan gum, which comprises the following specific steps:
step 1: and (3) preparing the aminated gellan gum.
1g of gellan gum was added to 100mL of dimethyl sulfoxide and heated at 60℃with stirring overnight to dissolve. Bis (4-nitrobenzene) carbonate having a molar ratio of 1 to gellan gum repeating units was added to the above solution, reacted at 60℃for 4 hours, then ethylenediamine monohydrate having a molar mass 10 times that of bis (4-nitrobenzene) carbonate was added, and the reaction was continued at 60℃for 3 hours. And (3) precipitating and separating a product by using acetone after the reaction is finished, repeatedly washing the product by using acetone for several times, and freeze-drying the product to obtain the aminated gellan gum.
Step 2: dissociation of the aminated gellan gum-like material.
60mg of aminated gellan gum is weighed and dissolved in 10mL of deionized water at 90 ℃, the solution is fully stirred until the solution is clear and transparent, and then the solution is cooled to be a gelatinous substance at room temperature, so as to obtain the aminated gellan gum gelatinous substance. To the aminated gellan gum material was added 0.4mL of 0.1M sodium hydroxide solution and the hydrogel was dissociated into a homogeneous solution.
Step 3: and preparing the self-adhesive spray gel by using polyphenol to induce gellan gum.
And adding 0.2mL of 1wt.% caffeic acid solution into the dissociated solution, and performing in-situ self-assembly on the dissociated solution under the induction of caffeic acid to generate hydrogel.
Fig. 9 is a strain sweep curve of the self-adhesive spray gel prepared in this example, and it can be seen from the figure that the storage modulus is greater than the loss modulus in the strain range of 0.1 to 82%, showing the gel properties.
Example 7:
the embodiment provides a preparation method of self-adhesive spray gel based on polyphenol induction gellan gum, which comprises the following specific steps:
step 1: and (3) preparing the aminated gellan gum.
1g of gellan gum was added to 100mL of dimethyl sulfoxide and heated at 60℃with stirring overnight to dissolve. Bis (4-nitrobenzene) carbonate having a molar ratio of 1 to gellan gum repeating units was added to the above solution, reacted at 60℃for 4 hours, then ethylenediamine monohydrate having a molar mass 10 times that of bis (4-nitrobenzene) carbonate was added, and the reaction was continued at 60℃for 3 hours. And (3) precipitating and separating a product by using acetone after the reaction is finished, repeatedly washing the product by using acetone for several times, and freeze-drying the product to obtain the aminated gellan gum.
Step 2: dissociation of the aminated gellan gum-like material.
60mg of aminated gellan gum is weighed and dissolved in 10mL of deionized water at 90 ℃, the solution is fully stirred until the solution is clear and transparent, and then the solution is cooled to be a gelatinous substance at room temperature, so as to obtain the aminated gellan gum gelatinous substance. To the aminated gellan gum material was added 0.4mL of 0.1M sodium hydroxide solution and the hydrogel was dissociated into a homogeneous solution.
Step 3: and preparing the self-adhesive spray gel by using polyphenol to induce gellan gum.
And adding 0.2mL of 1wt.% gallic acid solution into the dissociated solution, and performing in-situ self-assembly on the dissociated solution under the induction of gallic acid to generate hydrogel.
Fig. 10 is a strain sweep of the self-adhesive spray gel prepared in this example, showing gel properties with storage modulus greater than loss modulus over the 0.1-175% strain range.
The present invention is not limited to the above-described embodiments, which are merely illustrative and not restrictive, and many modifications may be made thereto by those of ordinary skill in the art without departing from the spirit of the invention and the scope of the appended claims.
Claims (6)
1. A method for preparing a self-adhesive spray gel based on polyphenol-induced gellan gum, comprising the steps of:
step 1: amination is carried out on natural polymer material gellan gum by ethylenediamine to prepare aminated gellan gum;
step 2: heating and dissolving the aminated gellan gum in water, and cooling to room temperature to obtain a gelatinous substance;
step 3: adding an alkaline solution into the gelatinous substance, and dissociating the gelatinous substance into a uniform aminated gellan gum solution;
step 4: adding a polyphenol solution into the aminated gellan gum solution, so that the solution self-assembles in situ under the induction of polyphenol to generate self-adhesive spray gel.
2. The method for preparing self-adhesive spray gel based on gellan gum induced by polyphenol according to claim 1, wherein the prepared self-adhesive spray gel mainly comprises the following components: 0.4 to 1wt.% of amination gellan gum solution, 8 to 12 pH value alkaline solution and 0.5 to 40wt.% of polyphenol solution, wherein the volume ratio of the three is 90 to 96:3 to 6:1 to 4.
3. The method for preparing a self-adhesive spray gel based on a polyphenol-induced gellan gum of claim 1, wherein the aminated gellan gum is an ethylenediamine grafted gellan gum.
4. The method for preparing the self-adhesive spray gel based on the gellan gum induced by polyphenol according to claim 1, wherein the heating temperature of the aminated gellan gum is 70-90 ℃; heating for 30-70 min; cooling to 20-30 deg.c.
5. The method for preparing the gellan gum self-adhesive spray gel based on polyphenol induction according to claim 1, wherein the polyphenol is one of tannic acid, dopamine, resveratrol, anthocyanin, gallic acid, caffeic acid and epigallocatechin gallate.
6. The method for preparing self-adhesive spray gel based on gellan gum induced by polyphenol according to claim 1, wherein the prepared self-adhesive spray gel is used as a drug carrier in the medical field or in the cosmetic field.
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