CN108926657A - A kind of preparation and application of graphene precious jade medicine nasitis plaster - Google Patents

A kind of preparation and application of graphene precious jade medicine nasitis plaster Download PDF

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CN108926657A
CN108926657A CN201811113230.3A CN201811113230A CN108926657A CN 108926657 A CN108926657 A CN 108926657A CN 201811113230 A CN201811113230 A CN 201811113230A CN 108926657 A CN108926657 A CN 108926657A
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graphene
precious jade
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parts
jade medicine
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赵立春
唐农
宋策
钟余特
王雪
于培良
李俊秀
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Guangxi University of Chinese Medicine
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Abstract

The invention proposes the preparations and application of a kind of graphene precious jade medicine nasitis plaster.The preparation method, comprising the following steps: (1) take Flos Magnoliae Liliflorae, the achene of Siberian cocklebur, Chinese yam, cicada slough, chrysanthemum, the root of Dahurain angelica, crush, distilled water and phosphate buffer is added in mixing, sieving, it stirs evenly, cellulase and pectase is added, stirs, centrifugation, collect supernatant, concentration, it is dry, obtain precious jade medicine enzymatic hydrolyzed extract;(2) Graphene powder is dispersed in precious jade drug metabolizing enzyme solution solution of extract, ultrasound, chitosan solution is added dropwise in stirring, stirs, and stands, obtains graphene-chitosan drug-loading hydrogel;(3) product of step (2) is stirred evenly, is poured into mold, graphene precious jade medicine nasitis plaster is made in solidification sizing.The composition of precious jade medicine treatment rhinitis in conjunction with grapheme material, is prepared hydrogel dosage form, is applied on emplastrum, can play the drug effect of Yao medicinal composition to greatest extent, absorbed convenient for patient, reach good therapeutic effect by the present invention.

Description

A kind of preparation and application of graphene precious jade medicine nasitis plaster
Technical field
The present invention relates to nasitis plaster technical fields, and in particular to a kind of graphene precious jade medicine nasitis plaster.
Background technique
Rhinitis, that is, nasal cavity inflammatory disease is virus, bacterium, allergen, various physical and chemical factors and certain systemic diseases The inflammation of caused bronchia mucosal.The main pathological change of rhinitis is bronchia mucosal hyperemia, swelling, exudation, hyperplasia, atrophy or bad It waits indefinitely.The cause of disease mainly has virus infection, heredity, schneiderian membrane itself easy infection, antigen such as pollen, fungi, acarid, shrimp etc. to cause, The symptom clinically mainly showed be nasal obstruction, more nasal mucus, smell decline, headache, giddy and other.With " just nearby getting rid of evils ", " control It is interior outer to adjust " be characteristic external treatment with Chinese medicine therapy, have significant and lasting curative effect to the disease, commonly use external application emplastrum to treat or subtract Mild shape, but easily make patient contact position that the adverse reactions such as red swelling of the skin, blistering occur.
Hydrogel is a kind of hydrophilic polymer material with three-dimensional structure, in aqueous solution can water absorption and swelling without The highly cross-linked macromolecule network system of dissolution.Since hydrogel has good biocompatibility, biodegradability, nothing The characteristics such as poison, stimulating responsive, thus biologic medical, intellectual material and in terms of have very big application prospect. Hydrogel is a kind of macromolecule network system, and property is soft, is able to maintain certain shape, can absorb a large amount of water.As one kind The high water-keeping material of high water absorption, hydrogel can be widely used for multiple fields, such as: the anti-morning in dry early area, facial mask in cosmetics, Defervescence plaster used, pain easing plaster, agricultural film, the moisture condensation preventing agent in building, conditioning agent, the water blockoff in petrochemical industry are adjusted, crude oil or The dehydration of product oil, the dust suppressant in mining industry, antistaling agent, thickener in food, the pharmaceutical carrier etc. in medical treatment.
Graphene is a kind of honeycomb two-dimensional nanostructure new material that the carbon atom by sp2 hydridization is formed, and is had single former Sub- thickness is most thin material in the world at present.Graphene is highly suitable for developing high performance due to its unique structure Composite material becomes the good filler of nanocomposite.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of graphene precious jade medicine nasitis plaster, and provides its production side Precious jade medicine treatment rhinitis composition in conjunction with grapheme material, is prepared special hydrogel dosage form, is applied to patch by method, this method On cream, physical structure and chemical effective component are combined, and can be played the drug effect of Yao medicinal composition to greatest extent, be inhaled convenient for patient It receives, has good therapeutic effect to a plurality of types of rhinitis.
The present invention provides a kind of preparation method of graphene precious jade medicine nasitis plaster, comprising the following steps:
(1) extraction of medicinal material: 12-17 parts of Flos Magnoliae Liliflorae, 12-17 parts of the achene of Siberian cocklebur, 12-17 parts of Chinese yam, cicada slough are taken by weight 8-12 parts, 12-17 parts of chrysanthemum, 12-17 parts of the root of Dahurain angelica crush, and mix, and distillation is added in sieving, resulting traditional Chinese medicine powder by a certain percentage It in water, stirs evenly, phosphate buffer is added by a certain percentage, a certain amount of cellulase and pectase, 50 DEG C of temperature are added Lower 50-100r/min is stirred to react 2-4h, and reaction is completed, and supernatant is collected in centrifugation, is concentrated, dry, obtains precious jade medicine enzymolysis and extraction Object;
(2) preparation of graphene base load medicinal gel: 200mg Graphene powder is dispersed in 1L precious jade medicament extract aqueous solution, Ultrasonic 1h obtains graphene dispersing solution, and the chitosan solution of 1.5mol/L is added dropwise in strong stirring, continues that 1h is sufficiently stirred, completely It stands after mixing for 24 hours, discharge bubble obtains graphene-chitosan drug-loading hydrogel;
(3) preparation of graphene precious jade medicine nasitis plaster: the graphene of step (2)-chitosan drug-loading hydrogel is stirred evenly, It pours into mold, is put into 0-4 DEG C of solidification sizing 24-48h of refrigerator, graphene precious jade medicine nasitis plaster is made.
Improved as of the invention further, medicinal material take by weight 15 parts of Flos Magnoliae Liliflorae, 15 parts of the achene of Siberian cocklebur, 15 parts of Chinese yam, 10 parts of cicada slough, 15 parts of chrysanthemum, 15 parts of the root of Dahurain angelica.
As further improvement of the invention, the mixed proportion of traditional Chinese medicine powder and distilled water is 1:20.
As further improvement of the invention, the mixed proportion of traditional Chinese medicine powder and phosphate buffer is 1:30.
As further improvement of the invention, the pH of phosphate buffer is 6.5.
Improved as of the invention further, precious jade medicament extract aqueous solution according to precious jade medicament extract and water weight ratio 1:40 It configures.
As further improvement of the invention, the condition that is stirred to react is 100r/min, reacts 3h.
As further improvement of the invention, centrifugal rotational speed 2000r/min, time 20min.
The present invention further protects the application of the graphene precious jade medicine nasitis plaster according to above method preparation.
The invention has the following beneficial effects:
1, graphene-aquagel prepared by the present invention has water absorbing force strong, and drugloading rate is high, and chemical property is stablized etc. Feature, being applied in nasitis plaster has the characteristics that rapid-action, the medicinal time persistently and will not generate skin allergy, redness, discomfort;
2, crude drug source of the present invention is wide, low in cost, and production method is simple, industrialization easy to accomplish.
Detailed description of the invention
Fig. 1 is the preparation technology figure of graphene base load medicinal gel.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the invention is clearly and completely described, Obviously, the embodiment described is the embodiment of part of representative of the invention, rather than whole embodiments, this field are general Other all embodiments obtained belong to protection of the invention to logical technical staff without making creative work Range.
1 graphene precious jade medicine nasitis plaster of embodiment
It follows the steps below:
(1) extraction of medicinal material: 17 parts of Flos Magnoliae Liliflorae, 17 parts of the achene of Siberian cocklebur, 17 parts of Chinese yam, 12 parts of cicada slough, chrysanthemum are taken by weight 17 parts, 17 parts of the root of Dahurain angelica crush, and mix, and sieving, resulting traditional Chinese medicine powder is mixed by 1:50 with distilled water, stir evenly, by traditional Chinese medicine powder Phosphate buffer is added with phosphate buffer 1:50, the cellulase of 300U/g, the fruit of 300U/g is added in pH of buffer=7.5 Glue enzyme, 80r/min is stirred to react 4h at a temperature of 50 DEG C, and reaction is completed, and supernatant is collected in centrifugation, is concentrated, dry, obtains precious jade medicine Enzymatic hydrolyzed extract, yield 75%;
(2) preparation of graphene base load medicinal gel: 200mg Graphene powder is dispersed in 1L precious jade medicament extract aqueous solution, Graphene dispersing solution is obtained into ultrasound 1h according to the weight ratio 1:100 of precious jade medicament extract and water configuration, strong stirring is added dropwise The chitosan solution of 1.5mol/L continues that 1h is sufficiently stirred, and stands after being mixed thoroughly for 24 hours, and discharge bubble obtains graphene- Chitosan drug-loading hydrogel;
(3) preparation of graphene precious jade medicine nasitis plaster: the graphene of step (2)-chitosan drug-loading hydrogel is stirred evenly, It pours into mold, is put into 4 DEG C of solidification sizing 36h of refrigerator, graphene precious jade medicine nasitis plaster is made.
2 graphene precious jade medicine nasitis plaster of embodiment
It follows the steps below:
(1) extraction of medicinal material: 15 parts of Flos Magnoliae Liliflorae, 15 parts of the achene of Siberian cocklebur, 15 parts of Chinese yam, 10 parts of cicada slough, chrysanthemum are taken by weight 15 parts, 15 parts of the root of Dahurain angelica crush, and mix, and sieving, resulting traditional Chinese medicine powder is mixed by 1:20 with distilled water, stir evenly, by traditional Chinese medicine powder Phosphate buffer is added with phosphate buffer 1:30, the cellulase of 200U/g, the fruit of 200U/g is added in pH of buffer=6.5 Glue enzyme, 100r/min is stirred to react 3h at a temperature of 50 DEG C, and reaction is completed, and supernatant is collected in centrifugation, is concentrated, dry, obtains precious jade medicine Enzymatic hydrolyzed extract, yield 94%;
(2) preparation of graphene base load medicinal gel: 200mg Graphene powder is dispersed in 1L precious jade medicament extract aqueous solution, It is configured according to the weight ratio 1:40 of precious jade medicament extract and water, ultrasonic 1h obtains graphene dispersing solution, and strong stirring is added dropwise The chitosan solution of 1.5mol/L continues that 1h is sufficiently stirred, and stands after being mixed thoroughly for 24 hours, and discharge bubble obtains graphene- Chitosan drug-loading hydrogel;
(3) preparation of graphene precious jade medicine nasitis plaster: the graphene of step (2)-chitosan drug-loading hydrogel is stirred evenly, It pours into mold, is put into 4 DEG C of solidification sizings of refrigerator for 24 hours, graphene precious jade medicine nasitis plaster is made.
3 graphene precious jade medicine nasitis plaster of embodiment
It follows the steps below:
(1) extraction of medicinal material: 12 parts of Flos Magnoliae Liliflorae, 12 parts of the achene of Siberian cocklebur, 12 parts of Chinese yam, 8 parts of cicada slough, chrysanthemum 12 are taken by weight Part, 12 parts of the root of Dahurain angelica, crush, mix, sieving, resulting traditional Chinese medicine powder is mixed with distilled water by 1:10, stir evenly, by traditional Chinese medicine powder and Phosphate buffer is added in phosphate buffer 1:20, and the cellulase of 100U/g, the pectin of 100U/g is added in pH of buffer=5.5 Enzyme, 50r/min is stirred to react 2h at a temperature of 50 DEG C, and reaction is completed, and supernatant is collected in centrifugation, is concentrated, dry, obtains precious jade drug metabolizing enzyme Solve extract, yield 54%;
(2) preparation of graphene base load medicinal gel: 200mg Graphene powder is dispersed in 1L precious jade medicament extract aqueous solution, It is configured according to the weight ratio 1:20 of precious jade medicament extract and water, ultrasonic 1h obtains graphene dispersing solution, and strong stirring is added dropwise The chitosan solution of 1.5mol/L continues that 1h is sufficiently stirred, and stands after being mixed thoroughly for 24 hours, and discharge bubble obtains graphene- Chitosan drug-loading hydrogel;
(3) preparation of graphene precious jade medicine nasitis plaster: the graphene of step (2)-chitosan drug-loading hydrogel is stirred evenly, It pours into mold, is put into 4 DEG C of solidification sizing 48h of refrigerator, graphene precious jade medicine nasitis plaster is made.
The extract of 1 Yao medicinal composition conventional method of reference examples preparation
It follows the steps below:
(1) 15 parts of Flos Magnoliae Liliflorae, 15 parts of the achene of Siberian cocklebur, 15 parts of Chinese yam, 10 parts of cicada slough, 15 parts of chrysanthemum, the root of Dahurain angelica 15 are taken by weight Part mixes after crushing, and 10 times of volume of water are added, and impregnates 1h, decocts 3h, is filtered under diminished pressure, filtrate is spare;
(2) 5 times of volume of water are added in the dregs of a decoction obtained by step (1), decoct 2h, is filtered under diminished pressure, filtrate is spare;
(3) filtrate obtained by step (1) and step (2) is merged, crosses 400 meshes, concentration filtrate to relative density 1.0- 1.5, to get Yao medicinal composition water extract, add auxiliary material, are prepared into transdermal patch.
The extract of 2 Yao medicinal composition enzymatic isolation method of reference examples preparation
It follows the steps below:
(1) 15 parts of Flos Magnoliae Liliflorae, 15 parts of the achene of Siberian cocklebur, 15 parts of Chinese yam, 10 parts of cicada slough, 15 parts of chrysanthemum, the root of Dahurain angelica 15 are taken by weight Part, it crushes, mixes, sieving;
(2) resulting traditional Chinese medicine powder is mixed by 1:20 with distilled water, is stirred evenly, is added by traditional Chinese medicine powder and phosphate buffer 1:30 Enter phosphate buffer, pH of buffer=6.5 are added the cellulase of 200U/g, the pectase of 200U/g, at a temperature of 50 DEG C 100r/min is stirred to react 3h;
(3) after the reaction was completed, it is centrifuged, centrifugal rotational speed 2000r/min, time 20min, collects supernatant, be concentrated, do It is dry, precious jade medicine enzymatic hydrolyzed extract is obtained, auxiliary material is added, is prepared into transdermal patch.
3 Yao medicinal composition ordinary gel agent of comparative example
It follows the steps below:
(1) 15 parts of Flos Magnoliae Liliflorae, 15 parts of the achene of Siberian cocklebur, 15 parts of Chinese yam, 10 parts of cicada slough, 15 parts of chrysanthemum, the root of Dahurain angelica 15 are taken by weight Part, it crushes, mixes, sieving;
(2) resulting traditional Chinese medicine powder is mixed by 1:20 with distilled water, is stirred evenly, is added by traditional Chinese medicine powder and phosphate buffer 1:30 Enter phosphate buffer, pH of buffer=6.5 are added the cellulase of 200U/g, the pectase of 200U/g, at a temperature of 50 DEG C 100r/min is stirred to react 3h;
(3) after the reaction was completed, it is centrifuged, centrifugal rotational speed 2000r/min, time 20min, collects supernatant, be concentrated, do It is dry, obtain precious jade medicine enzymatic hydrolyzed extract;
(4) precious jade medicine enzymatic hydrolyzed extract prepared by step (3) is dissolved in water, strong stirring, the chitosan that 1mol/L is added dropwise is molten Liquid continues that 1h is sufficiently stirred, and stands after being mixed thoroughly for 24 hours, and discharge bubble obtains Yao medicinal composition hydrogel, adds auxiliary Material, is prepared into transdermal patch.
1 human trial of test example
1, group is tested.It is divided into 5 groups, Yao medicinal composition water prepared by reference examples 1 proposes patch group (1 group of control), reference examples 2 are made Standby Yao medicinal composition enzyme proposes patch group (control 2 groups), prepared by reference examples 3 Yao medicinal composition ordinary gel patch group (3 groups of control), Graphene precious jade medicine nasitis plaster (experimental group) prepared by eucalyptus quintessence oil patch group (4 groups of control) and the embodiment of the present invention 2.
2, experimental method.
(1) case selection.That chooses that my downtown hospital accepts for medical treatment for 2 months -2017 years 2 months 2015 is diagnosed as through ear-nose-throat department Patient is divided into 5 groups with way of drawing lots by the patient of rhinitis 200, and every group 40,1 group of patient of control is 26 male, and female 14, year It is age 16-65 years old, 39.5 years old average, course of disease 1-15.It is 17 male to compare 2 groups of patients, female 23, the age l5-66 years old, average 38.2 Year, course of disease 1-l4.3 groups of patient male 20 are compareed, female 20, the age 16-62 years old, 37.9 years old average, course of disease 1-13.Control 4 groups of patient male 21, female 19, the age 15-64 years old, 36.5 years old average, course of disease 1-15.Experimental group patient male 23, female 17 Example, the age 15-65 years old, 38.1 years old average, course of disease 1-12.
(2) diagnostic method.According to Otolaryngology branches of Chinese Medical Association in 1997 and Chinese hals,Nasen und Ohrenheilkunde magazine The diagnostic criteria that editorial board formulates, which is ridiculed, is included in study group for the patient for being diagnosed as rhinitis.
(3) exclusion criteria.1. the vitals such as the heart, lung, kidney function is obviously abnormal;2. consciousness is abnormal, no independence;3. anxious Property infection of the upper respiratory tract person, pregnant woman, skin injury ulcer, severe allergy person etc.: 4. merge other Cavity in Critical Patients.
(4) treatment method.It compares 1 group and patch is mentioned using Yao medicinal composition water prepared by reference examples 1, half an hour patch before sleeping at night On, the next morning removes;It compares 2 groups and patch is mentioned using Yao medicinal composition enzyme prepared by reference examples 2, half an hour patch before sleeping at night On, the next morning removes;3 groups of Yao medicinal composition ordinary gel patches prepared using reference examples 3 are compareed, sleep preceding half an hour at night It sticks, the next morning removes;It compares 4 groups to paste using eucalyptus quintessence oil, half an hour sticks before sleeping at night, and the next morning takes Under;The graphene precious jade medicine nasitis plaster that experimental group uses the embodiment of the present invention 2 to prepare, half an hour sticks before sleeping at night, and second day early On remove.Continuous treatment one month.
(5) observation index and curative effect determinate standard.
Clinical efficacy: curative effect is evaluated according to the diagnostic criteria of rhinitis and efficacy assessment standard.Observe sneeze, the stream of patient Tears, nasal obstruction, rhiocnesmus etc. are scored before and after treatment patient (table 1).
1 patient stratification's standards of grading of table
Clinical efficacy is evaluated according to the formula of deduction rate: total before scoring rate=(total score after total score-treatment before treating)/treatment Divide × 100%.Total score=symptom score+sign scoring, calculated value >=51% are effective.50%-21% be it is effective ,≤20% is In vain.It is total effective=effective+effective.
Experimental result is shown in Table 2.
The comparison of clinical efficacy after 25 groups of patient's treatments of table
As seen from the above table, compare by five groups of patient's curative effects after treating, illustrate graphene precious jade medicine nose prepared by the present invention Inflammation posts the effect of apparent treatment rhinitis, can be relieved the symptoms such as nasal obstruction caused by rhinitis, rhiocnesmus, sneeze and runny nose, effect The gel drug paste and on the market outstanding that fruit is superior to the drug paste that conventional method is extracted, enzymatic isolation method extracts, enzymatic isolation method extracts preparation Sharp essential oil is added to paste.It can be seen that Yao medicinal composition of the present invention can effectively treat rhinitis, the gel adhesive prepared after graphene is added Drug effect can be played to the greatest extent, be absorbed convenient for patient, there is wide medical prospect.
Those skilled in the art is not under conditions of departing from the spirit and scope of the present invention that claims determine, also Various modifications can be carried out to the above content.Therefore the scope of the present invention is not limited in above explanation, but by The range of claims determines.

Claims (10)

1. a kind of preparation method of graphene precious jade medicine nasitis plaster, which comprises the following steps:
(1) extraction of medicinal material: 12-17 parts of Flos Magnoliae Liliflorae, 12-17 parts of the achene of Siberian cocklebur, 12-17 parts of Chinese yam, cicada slough 8-12 are taken by weight Part, 12-17 parts of chrysanthemum, 12-17 parts of the root of Dahurain angelica crush, and mix, and sieving, resulting traditional Chinese medicine powder is added in distilled water by a certain percentage, It stirs evenly, phosphate buffer is added by a certain percentage, a certain amount of cellulase and pectase, 50- at a temperature of 50 DEG C is added 100r/min is stirred to react 2-4h, and reaction is completed, and supernatant is collected in centrifugation, is concentrated, dry, obtains precious jade medicine enzymatic hydrolyzed extract;
(2) preparation of graphene base load medicinal gel: 200mg Graphene powder is dispersed in 1L precious jade medicament extract aqueous solution, ultrasound 1h obtains graphene dispersing solution, and the chitosan solution of 1.5mol/L is added dropwise in strong stirring, continues that 1h is sufficiently stirred, is thoroughly mixed It is stood after uniformly for 24 hours, discharge bubble obtains graphene-chitosan drug-loading hydrogel;
(3) preparation of graphene precious jade medicine nasitis plaster: the graphene of step (2)-chitosan drug-loading hydrogel is stirred evenly, is poured into In mold, it is put into 0-4 DEG C of solidification sizing 24-48h of refrigerator, graphene precious jade medicine nasitis plaster is made.
2. a kind of preparation method of graphene precious jade medicine nasitis plaster according to claim 1, which is characterized in that the medicinal material is by weight Amount part takes 15 parts of Flos Magnoliae Liliflorae, 15 parts of the achene of Siberian cocklebur, 15 parts of Chinese yam, 10 parts of cicada slough, 15 parts of chrysanthemum, 15 parts of the root of Dahurain angelica.
3. a kind of preparation method of graphene precious jade medicine nasitis plaster according to claim 1, which is characterized in that the traditional Chinese medicine powder with The mixed proportion of distilled water is 1:20.
4. a kind of preparation method of graphene precious jade medicine nasitis plaster according to claim 1, which is characterized in that the traditional Chinese medicine powder with The mixed proportion of phosphate buffer is 1:30.
5. a kind of preparation method of graphene precious jade medicine nasitis plaster according to claim 1, which is characterized in that the phosphoric acid buffer The pH of liquid is 6.5.
6. a kind of preparation method of graphene precious jade medicine nasitis plaster according to claim 1, which is characterized in that the cellulase Dosage be 200U/g, the dosage of pectase is 200U/g.
7. a kind of preparation method of graphene precious jade medicine nasitis plaster according to claim 1, which is characterized in that the precious jade medicine extracts Object aqueous solution is configured according to the weight ratio 1:40 of precious jade medicament extract and water.
8. a kind of preparation method of graphene precious jade medicine nasitis plaster according to claim 1, which is characterized in that described to be stirred to react Condition is 100r/min, reacts 3h.
9. a kind of preparation method of graphene precious jade medicine nasitis plaster according to claim 1, which is characterized in that the centrifugal rotational speed For 2000r/min, time 20min.
10. a kind of application of the graphene precious jade medicine nasitis plaster of the preparation of the preparation method according to any of the above claim.
CN201811113230.3A 2018-09-25 2018-09-25 A kind of preparation and application of graphene precious jade medicine nasitis plaster Pending CN108926657A (en)

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Application publication date: 20181204