CN105497908A - Preparation method of temperature-sensitive type gracilaria agar complex gel - Google Patents
Preparation method of temperature-sensitive type gracilaria agar complex gel Download PDFInfo
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- CN105497908A CN105497908A CN201510997355.7A CN201510997355A CN105497908A CN 105497908 A CN105497908 A CN 105497908A CN 201510997355 A CN201510997355 A CN 201510997355A CN 105497908 A CN105497908 A CN 105497908A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/0012—Galenical forms characterised by the site of application
- A61K9/0019—Injectable compositions; Intramuscular, intravenous, arterial, subcutaneous administration; Compositions to be administered through the skin in an invasive manner
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/0012—Galenical forms characterised by the site of application
- A61K9/0048—Eye, e.g. artificial tears
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/06—Ointments; Bases therefor; Other semi-solid forms, e.g. creams, sticks, gels
Abstract
The invention relates to a preparation method of temperature-sensitive type gracilaria agar complex gel, and belongs to the technical field of gel preparation. The method includes the steps of preparing gracilaria agar from fresh gracilaria serving as the raw materials together with thrice sterile water under specific conditions, mixing gracilaria agar with ethyl alcohol and other substances to form a gracilaria agar ethanol solution, making the solution mixed with chloroacetic acid and other substances under specific conditions, and conducting filtering, concentrating and drying to obtain the gel. The method has the advantages that the medicine carrying capacity is strong, the slow-release time is long, and high stability is achieved; the medicine utilization rate is high and is improved by 10-15%, the preparation steps are simple, and cost is low.
Description
Technical field
The present invention relates to a kind of preparation method of temperature sensitive type Gracilaria tenuistipitata agar coordination compound gel, belong to gel preparing technical field.
Background technology
Temperature sensitive hydrogel polymer there is variations in temperature with holding conditions and agents area and autolyze liquid to the characteristic of gel phase transition.Temperature sensitive type medicine-containing gel has good fluidity, easy to use, the holdup time is long, bioavailability is high, have the advantages such as good control Release Performance, be widely used in pharmaceutics, can be made into and bury value type controlled release drug delivery system, through being injected in vivo the misery of exempting implant surgery and bringing to patient, in addition, temperature sensitive hydrogel also can reprint biopharmaceutical macromolecular drug, keeps the activity of biomacromolecule, therefore, temperature sensitive hydrogel drug-loading system has become a bright spot in Pharmaceutical study.
The poloxamer that current most of temperature sensitive hydrogel preparation adopts, it is formed according to the structure of PEO-PPO-PEO by hydrophilic section polyoxyethylene (PEO) and hydrophobic section polyoxypropylene (PPO), has good biocompatibility and lower toxicity.In addition, certain density poloxamer also has reverse temperature-sensitive gelling property, is namely liquid when low temperature, changes semi-solid gel shape when room temperature and body temperature into, after temperature reduces, changes again flowable liquids shape into again.Be widely used at present vein emulsion, the solubilizing agent of insoluble drug, the absorption enhancer of medicine have eased up controlled-release material.But envelop rate and the drug loading of poloxamer are low, and critical micelle concentration is high, and stability is low, thus its application is restricted.
Summary of the invention
The technical problem that the present invention mainly solves: poor for the gel stability utilizing poloxamer to prepare at present, the effective rate of utilization of medicine is low, the problem that envelop rate is low, provide a kind of main with fresh Gracilaria tenuistipitata for raw material, respectively through with three sterilized water under given conditions, be prepared into gracilaria verrucosa agar gel, and the materials such as itself and ethanol are mixed into Gracilaria tenuistipitata agar alcoholic solution, more under given conditions, mix with materials such as monoxones, and after filtration, concentrated, dry obtained gel.It is strong that temperature sensitive type Gracilaria tenuistipitata agar coordination compound gel prepared by the present invention has Drug loading capacity, and slow-release time is long, has the feature of stronger stability.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention:
(1) fresh Gracilaria tenuistipitata is chosen, clean with clear water and dry under being placed in sunlight, be placed on dry 2 ~ 3h in 55 ~ 60 DEG C of baking ovens subsequently, be prepared into dry Gracilaria tenuistipitata, press solid-liquid mass ratio 1:10 subsequently, dry Gracilaria tenuistipitata and sterilized water are stirred swelling, is sealed subsequently and be placed in 20 ~ 30 DEG C of bottom fermentation process 2 ~ 3 days;
(2) after fermentation completes, it is filtered and collects filtering residue, with sterilized water washing 3 ~ 5 times, by solid-liquid mass ratio 1:10, itself and sterilized water are uniformly mixed again, press sterilized water and sodium hydroxide solution mass ratio 1:1 subsequently, by mass concentration be 20% sodium hydroxide solution be added in above-mentioned solution, after being uniformly mixed 10 ~ 15min, at 65 ~ 70 DEG C water bath with thermostatic control heating 2 ~ 3h;
(3) after heating in water bath completes, filter cake is collected to its decompress filter, and with distilled water wash 3 ~ 5 times, after washing completes, rinse with the hydrochloric acid solution of 0.1mol/L again and make its pH to 6.5, after using deionized water wash 3 ~ 5 times subsequently, be placed in beaker, by solid-liquid mass ratio 1:50, sterilized water is added in beaker;
(4) to be added complete after, sealed and be placed in 120 ~ 125 DEG C of oil bath heating 2 ~ 3h, after it has heated, making it naturally cool to 20 ~ 30 DEG C, and to its sucking filtration again, collect filtrate and filtering residue, by solid-liquid mass ratio 1:25, filtering residue and sterilized water are uniformly mixed and are placed in beaker, oil bath heating 1 ~ 2h is continued at 120 ~ 130 DEG C, filter after its natural cooling and collect filtrate, merge twice filtrate and to its vacuum lyophilization 6 ~ 8h, be prepared into gracilaria verrucosa agar gel;
(5) by the gracilaria verrucosa agar gel of above-mentioned preparation and sodium hydroxide solution 1:10 in mass ratio, the sodium hydroxide solution being 40% by gracilaria verrucosa agar gel and mass fraction is uniformly mixed, alkalize 12 ~ 14h subsequently at 20 ~ 25 DEG C, after alkalization completes, continue the dehydrated alcohol added and sodium hydroxide solution is identical in quality, be uniformly mixed 5 ~ 8h, be prepared into Gracilaria tenuistipitata agar alcoholic solution;
(6) by solid-liquid mass ratio 1:1.5, monoxone and absolute ethyl alcohol and stirring are mixed and makes it dissolve completely, 1:4 in mass ratio again, above-mentioned mixed liquor is dropped in the Gracilaria tenuistipitata agar alcoholic solution of above-mentioned preparation by the speed of 2mL/min, react 2 ~ 4h at 20 ~ 30 DEG C after, intensification is heated to 66 ~ 70 DEG C of reaction 2 ~ 3h, after question response completes, leave standstill cooling and dilute pH to 7.0 with deionized water, filtration under diminished pressure subsequently, after absolute ethanol washing 3 ~ 5 times, vacuum lyophilization 6 ~ 8h at being placed on 40 ~ 45 DEG C, is prepared into modification Gracilaria tenuistipitata agar;
(7) 10 ~ 15g modification Gracilaria tenuistipitata agar of above-mentioned preparation is got, be added in the hydrochloric acid solution of the 0.1mol/L of 450 ~ 500mL, be uniformly mixed and make it dissolve completely, filter with G3 funnel subsequently, collect agar filtrate, 1:10 in mass ratio subsequently, the modification Gracilaria tenuistipitata agar of above-mentioned preparation is dissolved in distilled water, be prepared into modification agar solution, 1:10 is compared again by modification agar solution and agar filtrate quality, modification agar solution is slowly dropped in filtrate, slowly stir subsequently and rotary evaporation to 1/5 of original volume, dry 2 ~ 3h at being placed on 50 ~ 70 DEG C again, a kind of temperature sensitive type Gracilaria tenuistipitata agar coordination compound gel can be prepared into.
application of the present invention: the temperature sensitive type Gracilaria tenuistipitata agar coordination compound gel of above-mentioned preparation is used for local injection administration, can forms gel under body temperature, can slow releasing medicine, and the release medicine time can extend 10 ~ 12h; Or using the temperature sensitive type Gracilaria tenuistipitata agar coordination compound gel of above-mentioned preparation as dosing eyes, effectively eye strain can be extenuated.
The invention has the beneficial effects as follows:
(1) have Drug loading capacity strong, slow-release time is long, has the feature of stronger stability;
(2) utilization ratio of drug is high, improves 10 ~ 15%;
(3) preparation process is simple, and cost is low.
Detailed description of the invention
First fresh Gracilaria tenuistipitata is chosen, clean with clear water and dry under being placed in sunlight, be placed on dry 2 ~ 3h in 55 ~ 60 DEG C of baking ovens subsequently, be prepared into dry Gracilaria tenuistipitata, press solid-liquid mass ratio 1:10 subsequently, dry Gracilaria tenuistipitata and sterilized water are stirred swelling, is sealed subsequently and be placed in 20 ~ 30 DEG C of bottom fermentation process 2 ~ 3 days, after fermentation completes, it is filtered and collects filtering residue, with sterilized water washing 3 ~ 5 times, by solid-liquid mass ratio 1:10, itself and sterilized water are uniformly mixed again, press sterilized water and sodium hydroxide solution mass ratio 1:1 subsequently, by mass concentration be 20% sodium hydroxide solution be added in above-mentioned solution, after being uniformly mixed 10 ~ 15min, at 65 ~ 70 DEG C water bath with thermostatic control heating 2 ~ 3h, after heating in water bath completes, filter cake is collected to its decompress filter, and with distilled water wash 3 ~ 5 times, after washing completes, rinse with the hydrochloric acid solution of 0.1mol/L again and make its pH to 6.5, after using deionized water wash 3 ~ 5 times subsequently, be placed in beaker, by solid-liquid mass ratio 1:50, sterilized water is added in beaker, to be added complete after, sealed and be placed in 120 ~ 125 DEG C of oil bath heating 2 ~ 3h, after it has heated, making it naturally cool to 20 ~ 30 DEG C, and to its sucking filtration again, collect filtrate and filtering residue, by solid-liquid mass ratio 1:25, filtering residue and sterilized water are uniformly mixed and are placed in beaker, oil bath heating 1 ~ 2h is continued at 120 ~ 130 DEG C, filter after its natural cooling and collect filtrate, merge twice filtrate and to its vacuum lyophilization 6 ~ 8h, be prepared into gracilaria verrucosa agar gel, again by the gracilaria verrucosa agar gel of above-mentioned preparation and sodium hydroxide solution 1:10 in mass ratio, the sodium hydroxide solution being 40% by gracilaria verrucosa agar gel and mass fraction is uniformly mixed, alkalize 12 ~ 14h subsequently at 20 ~ 25 DEG C, after alkalization completes, continue the dehydrated alcohol added and sodium hydroxide solution is identical in quality, be uniformly mixed 5 ~ 8h, be prepared into Gracilaria tenuistipitata agar alcoholic solution, by solid-liquid mass ratio 1:1.5, monoxone and absolute ethyl alcohol and stirring are mixed and makes it dissolve completely, 1:4 in mass ratio again, above-mentioned mixed liquor is dropped in the Gracilaria tenuistipitata agar alcoholic solution of above-mentioned preparation by the speed of 2mL/min, react 2 ~ 4h at 20 ~ 30 DEG C after, intensification is heated to 66 ~ 70 DEG C of reaction 2 ~ 3h, after question response completes, leave standstill cooling and dilute pH to 7.0 with deionized water, filtration under diminished pressure subsequently, after absolute ethanol washing 3 ~ 5 times, vacuum lyophilization 6 ~ 8h at being placed on 40 ~ 45 DEG C, is prepared into modification Gracilaria tenuistipitata agar, get 10 ~ 15g modification Gracilaria tenuistipitata agar of above-mentioned preparation, be added in the hydrochloric acid solution of the 0.1mol/L of 450 ~ 500mL, be uniformly mixed and make it dissolve completely, filter with G3 funnel subsequently, collect agar filtrate, 1:10 in mass ratio subsequently, the modification Gracilaria tenuistipitata agar of above-mentioned preparation is dissolved in distilled water, be prepared into modification agar solution, 1:10 is compared again by modification agar solution and agar filtrate quality, modification agar solution is slowly dropped in filtrate, slowly stir subsequently and rotary evaporation to 1/5 of original volume, dry 2 ~ 3h at being placed on 50 ~ 70 DEG C again, a kind of temperature sensitive type Gracilaria tenuistipitata agar coordination compound gel can be prepared into.
First example 1 chooses fresh Gracilaria tenuistipitata, cleans and dries under being placed in sunlight, be placed on dry 3h in 60 DEG C of baking ovens subsequently with clear water, be prepared into dry Gracilaria tenuistipitata, press solid-liquid mass ratio 1:10 subsequently, dry Gracilaria tenuistipitata and sterilized water are stirred swelling, sealed subsequently and be placed in 30 DEG C of bottom fermentation process 3 days, after fermentation completes, it is filtered and collects filtering residue, 5 times are washed with sterilized water, by solid-liquid mass ratio 1:10, itself and sterilized water are uniformly mixed again, press sterilized water and sodium hydroxide solution mass ratio 1:1 subsequently, by mass concentration be 20% sodium hydroxide solution be added in above-mentioned solution, after being uniformly mixed 15min, at 70 DEG C water bath with thermostatic control heating 3h, after heating in water bath completes, filter cake is collected to its decompress filter, and with distilled water wash 5 times, after washing completes, rinse with the hydrochloric acid solution of 0.1mol/L again and make its pH to 6.5, after using deionized water wash 5 times subsequently, be placed in beaker, by solid-liquid mass ratio 1:50, sterilized water is added in beaker, to be added complete after, sealed and be placed in 125 DEG C of oil bath heating 3h, after it has heated, making it naturally cool to 30 DEG C, and to its sucking filtration again, collect filtrate and filtering residue, by solid-liquid mass ratio 1:25, filtering residue and sterilized water are uniformly mixed and are placed in beaker, oil bath heating 2h is continued at 130 DEG C, filter after its natural cooling and collect filtrate, merge twice filtrate and to its vacuum lyophilization 8h, be prepared into gracilaria verrucosa agar gel, again by the gracilaria verrucosa agar gel of above-mentioned preparation and sodium hydroxide solution 1:10 in mass ratio, the sodium hydroxide solution being 40% by gracilaria verrucosa agar gel and mass fraction is uniformly mixed, alkalize 14h subsequently at 25 DEG C, after alkalization completes, continue the dehydrated alcohol added and sodium hydroxide solution is identical in quality, be uniformly mixed 8h, be prepared into Gracilaria tenuistipitata agar alcoholic solution, by solid-liquid mass ratio 1:1.5, monoxone and absolute ethyl alcohol and stirring are mixed and makes it dissolve completely, 1:4 in mass ratio again, above-mentioned mixed liquor is dropped in the Gracilaria tenuistipitata agar alcoholic solution of above-mentioned preparation by the speed of 2mL/min, react 4h at 30 DEG C after, intensification is heated to 70 DEG C of reaction 3h, after question response completes, leave standstill cooling and dilute pH to 7.0 with deionized water, filtration under diminished pressure subsequently, after absolute ethanol washing 5 times, vacuum lyophilization 8h at being placed on 45 DEG C, is prepared into modification Gracilaria tenuistipitata agar, get the 15g modification Gracilaria tenuistipitata agar of above-mentioned preparation, be added in the hydrochloric acid solution of the 0.1mol/L of 500mL, be uniformly mixed and make it dissolve completely, filter with G3 funnel subsequently, collect agar filtrate, 1:10 in mass ratio subsequently, the modification Gracilaria tenuistipitata agar of above-mentioned preparation is dissolved in distilled water, be prepared into modification agar solution, 1:10 is compared again by modification agar solution and agar filtrate quality, modification agar solution is slowly dropped in filtrate, slowly stir subsequently and rotary evaporation to 1/5 of original volume, dry 3h at being placed on 70 DEG C again, a kind of temperature sensitive type Gracilaria tenuistipitata agar coordination compound gel can be prepared into.The temperature sensitive type Gracilaria tenuistipitata agar coordination compound gel of above-mentioned preparation is used for local injection administration, gel can be formed under body temperature, can slow releasing medicine, the release medicine time can extend 10h.
example 2
First choose fresh Gracilaria tenuistipitata, clean with clear water and dry under being placed in sunlight, being placed on dry 2h in 55 DEG C of baking ovens subsequently, be prepared into dry Gracilaria tenuistipitata, press solid-liquid mass ratio 1:10 subsequently, dry Gracilaria tenuistipitata and sterilized water are stirred swelling, sealed subsequently and be placed in 20 DEG C of bottom fermentation process 2 days, after fermentation completes, it is filtered and collects filtering residue, 3 times are washed with sterilized water, by solid-liquid mass ratio 1:10, itself and sterilized water are uniformly mixed again, press sterilized water and sodium hydroxide solution mass ratio 1:1 subsequently, by mass concentration be 20% sodium hydroxide solution be added in above-mentioned solution, after being uniformly mixed 10min, at 65 DEG C water bath with thermostatic control heating 2h, after heating in water bath completes, filter cake is collected to its decompress filter, and with distilled water wash 3 times, after washing completes, rinse with the hydrochloric acid solution of 0.1mol/L again and make its pH to 6.5, after using deionized water wash 3 times subsequently, be placed in beaker, by solid-liquid mass ratio 1:50, sterilized water is added in beaker, to be added complete after, sealed and be placed in 120 DEG C of oil bath heating 2h, after it has heated, making it naturally cool to 20 DEG C, and to its sucking filtration again, collect filtrate and filtering residue, by solid-liquid mass ratio 1:25, filtering residue and sterilized water are uniformly mixed and are placed in beaker, oil bath heating 1h is continued at 120 DEG C, filter after its natural cooling and collect filtrate, merge twice filtrate and to its vacuum lyophilization 6h, be prepared into gracilaria verrucosa agar gel, again by the gracilaria verrucosa agar gel of above-mentioned preparation and sodium hydroxide solution 1:10 in mass ratio, the sodium hydroxide solution being 40% by gracilaria verrucosa agar gel and mass fraction is uniformly mixed, alkalize 12h subsequently at 20 DEG C, after alkalization completes, continue the dehydrated alcohol added and sodium hydroxide solution is identical in quality, be uniformly mixed 5h, be prepared into Gracilaria tenuistipitata agar alcoholic solution, by solid-liquid mass ratio 1:1.5, monoxone and absolute ethyl alcohol and stirring are mixed and makes it dissolve completely, 1:4 in mass ratio again, above-mentioned mixed liquor is dropped in the Gracilaria tenuistipitata agar alcoholic solution of above-mentioned preparation by the speed of 2mL/min, react 2h at 20 DEG C after, intensification is heated to 66 DEG C of reaction 2h, after question response completes, leave standstill cooling and dilute pH to 7.0 with deionized water, filtration under diminished pressure subsequently, after absolute ethanol washing 3 times, vacuum lyophilization 6h at being placed on 40 DEG C, is prepared into modification Gracilaria tenuistipitata agar, get the 10g modification Gracilaria tenuistipitata agar of above-mentioned preparation, be added in the hydrochloric acid solution of the 0.1mol/L of 450mL, be uniformly mixed and make it dissolve completely, filter with G3 funnel subsequently, collect agar filtrate, 1:10 in mass ratio subsequently, the modification Gracilaria tenuistipitata agar of above-mentioned preparation is dissolved in distilled water, be prepared into modification agar solution, 1:10 is compared again by modification agar solution and agar filtrate quality, modification agar solution is slowly dropped in filtrate, slowly stir subsequently and rotary evaporation to 1/5 of original volume, dry 2h at being placed on 50 DEG C again, a kind of temperature sensitive type Gracilaria tenuistipitata agar coordination compound gel can be prepared into.The temperature sensitive type Gracilaria tenuistipitata agar coordination compound gel of above-mentioned preparation is used for local injection administration, gel can be formed under body temperature, can slow releasing medicine, the release medicine time can extend 12h.
Example 3
First choose fresh Gracilaria tenuistipitata, clean with clear water and dry under being placed in sunlight, being placed on dry 2.5h in 57 DEG C of baking ovens subsequently, be prepared into dry Gracilaria tenuistipitata, press solid-liquid mass ratio 1:10 subsequently, dry Gracilaria tenuistipitata and sterilized water are stirred swelling, sealed subsequently and be placed in 25 DEG C of bottom fermentation process 3 days, after fermentation completes, it is filtered and collects filtering residue, 4 times are washed with sterilized water, by solid-liquid mass ratio 1:10, itself and sterilized water are uniformly mixed again, press sterilized water and sodium hydroxide solution mass ratio 1:1 subsequently, by mass concentration be 20% sodium hydroxide solution be added in above-mentioned solution, after being uniformly mixed 12min, at 66 DEG C water bath with thermostatic control heating 2h, after heating in water bath completes, filter cake is collected to its decompress filter, and with distilled water wash 4 times, after washing completes, rinse with the hydrochloric acid solution of 0.1mol/L again and make its pH to 6.5, after using deionized water wash 4 times subsequently, be placed in beaker, by solid-liquid mass ratio 1:50, sterilized water is added in beaker, to be added complete after, sealed and be placed in 122 DEG C of oil bath heating 2h, after it has heated, making it naturally cool to 25 DEG C, and to its sucking filtration again, collect filtrate and filtering residue, by solid-liquid mass ratio 1:25, filtering residue and sterilized water are uniformly mixed and are placed in beaker, oil bath heating 1h is continued at 125 DEG C, filter after its natural cooling and collect filtrate, merge twice filtrate and to its vacuum lyophilization 7h, be prepared into gracilaria verrucosa agar gel, again by the gracilaria verrucosa agar gel of above-mentioned preparation and sodium hydroxide solution 1:10 in mass ratio, the sodium hydroxide solution being 40% by gracilaria verrucosa agar gel and mass fraction is uniformly mixed, alkalize 13h subsequently at 22 DEG C, after alkalization completes, continue the dehydrated alcohol added and sodium hydroxide solution is identical in quality, be uniformly mixed 7h, be prepared into Gracilaria tenuistipitata agar alcoholic solution, by solid-liquid mass ratio 1:1.5, monoxone and absolute ethyl alcohol and stirring are mixed and makes it dissolve completely, 1:4 in mass ratio again, above-mentioned mixed liquor is dropped in the Gracilaria tenuistipitata agar alcoholic solution of above-mentioned preparation by the speed of 2mL/min, react 3h at 25 DEG C after, intensification is heated to 67 DEG C of reaction 2h, after question response completes, leave standstill cooling and dilute pH to 7.0 with deionized water, filtration under diminished pressure subsequently, after absolute ethanol washing 3 ~ 5 times, vacuum lyophilization 7h at being placed on 42 DEG C, is prepared into modification Gracilaria tenuistipitata agar, get the 12g modification Gracilaria tenuistipitata agar of above-mentioned preparation, be added in the hydrochloric acid solution of the 0.1mol/L of 470mL, be uniformly mixed and make it dissolve completely, filter with G3 funnel subsequently, collect agar filtrate, 1:10 in mass ratio subsequently, the modification Gracilaria tenuistipitata agar of above-mentioned preparation is dissolved in distilled water, be prepared into modification agar solution, 1:10 is compared again by modification agar solution and agar filtrate quality, modification agar solution is slowly dropped in filtrate, slowly stir subsequently and rotary evaporation to 1/5 of original volume, dry 2.5h at being placed on 60 DEG C again, a kind of temperature sensitive type Gracilaria tenuistipitata agar coordination compound gel can be prepared into.Using the temperature sensitive type Gracilaria tenuistipitata agar coordination compound gel of above-mentioned preparation as dosing eyes, effectively eye strain can be extenuated.
Claims (1)
1. a preparation method for temperature sensitive type Gracilaria tenuistipitata agar coordination compound gel, is characterized in that concrete preparation process is:
(1) fresh Gracilaria tenuistipitata is chosen, clean with clear water and dry under being placed in sunlight, be placed on dry 2 ~ 3h in 55 ~ 60 DEG C of baking ovens subsequently, be prepared into dry Gracilaria tenuistipitata, press solid-liquid mass ratio 1:10 subsequently, dry Gracilaria tenuistipitata and sterilized water are stirred swelling, is sealed subsequently and be placed in 20 ~ 30 DEG C of bottom fermentation process 2 ~ 3 days;
(2) after fermentation completes, it is filtered and collects filtering residue, with sterilized water washing 3 ~ 5 times, by solid-liquid mass ratio 1:10, itself and sterilized water are uniformly mixed again, press sterilized water and sodium hydroxide solution mass ratio 1:1 subsequently, by mass concentration be 20% sodium hydroxide solution be added in above-mentioned solution, after being uniformly mixed 10 ~ 15min, at 65 ~ 70 DEG C water bath with thermostatic control heating 2 ~ 3h;
(3) after heating in water bath completes, filter cake is collected to its decompress filter, and with distilled water wash 3 ~ 5 times, after washing completes, rinse with the hydrochloric acid solution of 0.1mol/L again and make its pH to 6.5, after using deionized water wash 3 ~ 5 times subsequently, be placed in beaker, by solid-liquid mass ratio 1:50, sterilized water is added in beaker;
(4) to be added complete after, sealed and be placed in 120 ~ 125 DEG C of oil bath heating 2 ~ 3h, after it has heated, making it naturally cool to 20 ~ 30 DEG C, and to its sucking filtration again, collect filtrate and filtering residue, by solid-liquid mass ratio 1:25, filtering residue and sterilized water are uniformly mixed and are placed in beaker, oil bath heating 1 ~ 2h is continued at 120 ~ 130 DEG C, filter after its natural cooling and collect filtrate, merge twice filtrate and to its vacuum lyophilization 6 ~ 8h, be prepared into gracilaria verrucosa agar gel;
(5) by the gracilaria verrucosa agar gel of above-mentioned preparation and sodium hydroxide solution 1:10 in mass ratio, the sodium hydroxide solution being 40% by gracilaria verrucosa agar gel and mass fraction is uniformly mixed, alkalize 12 ~ 14h subsequently at 20 ~ 25 DEG C, after alkalization completes, continue the dehydrated alcohol added and sodium hydroxide solution is identical in quality, be uniformly mixed 5 ~ 8h, be prepared into Gracilaria tenuistipitata agar alcoholic solution;
(6) by solid-liquid mass ratio 1:1.5, monoxone and absolute ethyl alcohol and stirring are mixed and makes it dissolve completely, 1:4 in mass ratio again, above-mentioned mixed liquor is dropped in the Gracilaria tenuistipitata agar alcoholic solution of above-mentioned preparation by the speed of 2mL/min, react 2 ~ 4h at 20 ~ 30 DEG C after, intensification is heated to 66 ~ 70 DEG C of reaction 2 ~ 3h, after question response completes, leave standstill cooling and dilute pH to 7.0 with deionized water, filtration under diminished pressure subsequently, after absolute ethanol washing 3 ~ 5 times, vacuum lyophilization 6 ~ 8h at being placed on 40 ~ 45 DEG C, is prepared into modification Gracilaria tenuistipitata agar;
(7) 10 ~ 15g modification Gracilaria tenuistipitata agar of above-mentioned preparation is got, be added in the hydrochloric acid solution of the 0.1mol/L of 450 ~ 500mL, be uniformly mixed and make it dissolve completely, filter with G3 funnel subsequently, collect agar filtrate, 1:10 in mass ratio subsequently, the modification Gracilaria tenuistipitata agar of above-mentioned preparation is dissolved in distilled water, be prepared into modification agar solution, 1:10 is compared again by modification agar solution and agar filtrate quality, modification agar solution is slowly dropped in filtrate, slowly stir subsequently and rotary evaporation to 1/5 of original volume, dry 2 ~ 3h at being placed on 50 ~ 70 DEG C again, a kind of temperature sensitive type Gracilaria tenuistipitata agar coordination compound gel can be prepared into.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800935A (en) * | 2016-12-25 | 2017-06-06 | 常州梦泰照明科技有限公司 | A kind of preparation method of the degradable sand-consolidating agent of consolidation force high |
| CN110003362A (en) * | 2019-04-23 | 2019-07-12 | 福建省绿麒食品胶体有限公司 | A kind of preparation method of the modified agar of high grade of transparency high-gel strength |
| USD918654S1 (en) | 2019-06-06 | 2021-05-11 | Sharkninja Operating Llc | Grill plate |
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2015
- 2015-12-28 CN CN201510997355.7A patent/CN105497908A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800935A (en) * | 2016-12-25 | 2017-06-06 | 常州梦泰照明科技有限公司 | A kind of preparation method of the degradable sand-consolidating agent of consolidation force high |
| CN110003362A (en) * | 2019-04-23 | 2019-07-12 | 福建省绿麒食品胶体有限公司 | A kind of preparation method of the modified agar of high grade of transparency high-gel strength |
| USD918654S1 (en) | 2019-06-06 | 2021-05-11 | Sharkninja Operating Llc | Grill plate |
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Application publication date: 20160420 |