CN113318162A - Preparation method of Li medicine Callicarpa nudiflora scald ointment - Google Patents

Preparation method of Li medicine Callicarpa nudiflora scald ointment Download PDF

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CN113318162A
CN113318162A CN202110640642.8A CN202110640642A CN113318162A CN 113318162 A CN113318162 A CN 113318162A CN 202110640642 A CN202110640642 A CN 202110640642A CN 113318162 A CN113318162 A CN 113318162A
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callicarpa nudiflora
scald ointment
ointment
medicine
scald
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谭银丰
李海龙
张仲
秦贞苗
张俊清
周金娜
邱梦婕
周小芳
黄明浩
罗贤强
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Hainan Medical College
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    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
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    • A61K2236/30Extraction of the material
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    • A61K2236/50Methods involving additional extraction steps
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Abstract

The invention discloses a Li medicine Callicarpa nudiflora scald ointment preparation method, which comprises the steps of taking Callicarpa nudiflora medicinal materials, respectively adding water with the weight of 12, 10 and 10 times of the medicinal materials, soaking for 2h, then carrying out reflux extraction for 1h each time, filtering, combining 3 times of water extract, and concentrating to obtain Callicarpa nudiflora medicinal material extract; preparing w/o callicarpa nudiflora scald ointment by adopting an emulsification method, heating oil-phase raw materials of polysorbate-80, glyceryl monostearate and glycerin to 70-80 ℃, slowly adding the heated oil-phase raw materials of liquid paraffin, sorbitan oleate, solid paraffin and vaseline which are heated to 70-80 ℃, adding callicarpa nudiflora medicinal material fluid extract under stirring, emulsifying and coagulating for 20-30 minutes to obtain the Li medicine callicarpa nudiflora scald ointment. The Li medicine callicarpa nudiflora scald ointment prepared by optimizing raw materials through a large number of experiments is scientific and reasonable in component proportion, stable in performance, reliable in curative effect and good in safety, and can promote wound healing well.

Description

Preparation method of Li medicine Callicarpa nudiflora scald ointment
The application is a divisional application with application date of 2016, month 07, application number of 201610971201.5 and invention name of preparation method of a Li yao nudiflower beautyberry scald ointment.
Technical Field
The invention belongs to the technical field of medicines, and particularly relates to a preparation method of a Li medicine Callicarpa nudiflora scald ointment.
Background
Callicarpa nudiflora (Callicarpa pandifora hook. exArn.) is a perennial small tree of Callicarpa of Verbenaceae, namely a large fan blade, which is distributed above 300m above the altitude in the central and south of Hainan, and grows well in mountain sides, valley, stream sides or bush forest of a vast mountain area with the annual rainfall of 1000-1800 mm at a relatively high temperature of 15-25 ℃ per year, so that the Callicarpa nudiflora is a major genuine medicinal material in Hainan and is one of common medicinal materials for doctors in Hainan. Modern pharmacological research shows that active ingredients of the Li medicine callicarpa nudiflora comprise terpenes, flavones and volatile oil, and the Li medicine callicarpa nudiflora has good effects of resisting inflammation, stopping bleeding and the like.
At present, no reports of preparing the Li medicine callicarpa nudiflora into scald ointment exist.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the defects of the prior art and provides the preparation method of the Li medicine callicarpa nudiflora scald ointment, which has scientific and reasonable component proportion, stable performance, good effect of promoting wound healing, reliable curative effect and safety.
The technical scheme is as follows: in order to achieve the above purpose, the invention adopts the technical scheme that:
a preparation method of Li's medicine Callicarpa nudiflora scald ointment is prepared from the following raw materials in percentage by weight:
(1) extracting callicarpa nudiflora:
taking a callicarpa nudiflora medicinal material, respectively adding water with the weight of 12, 10 and 10 times of the medicinal material, soaking for 2 hours, then performing reflux extraction for 1 hour each time, filtering, combining 3 times of water extract, and concentrating to obtain callicarpa nudiflora medicinal material extract;
(2) preparation of scald ointment
Preparing w/o callicarpa nudiflora scald ointment by adopting an emulsification method, heating oil-phase raw materials of polysorbate-80, glyceryl monostearate and glycerin to 70-80 ℃, slowly adding the heated oil-phase raw materials of liquid paraffin, sorbitan oleate, solid paraffin and vaseline to 70-80 ℃, adding callicarpa nudiflora medicinal material fluid extract, ethylparaben and dimethyl sulfoxide under stirring, and carrying out co-directional stirring, emulsification and condensation for 20-40 minutes to obtain the Li medicine callicarpa nudiflora scald ointment.
The preparation method of the Li medicine Callicarpa nudiflora scald ointment comprises the following components in parts by weight: the oil phase raw materials comprise 800.8-1.4 g of polysorbate-0, 4.2-5.5 g of glycerin monostearate and 0.6-1.2 g of glycerol; the water phase raw materials comprise 9-12 g of liquid paraffin, 0.6-1.8 g of sorbitan oleate, 0.6-1.8 g of solid paraffin and 0.7-1.3 g of vaseline; the dosage of the callicarpa nudiflora medicinal material extract is 2-5 g; 0.037-0.15 g of ethylparaben and 0.0187-0.03 g of dimethyl sulfoxide;
as a preferred scheme, the preparation method of the liyao nudiflower beautyberry scald ointment comprises the following components in parts by weight: the oil phase raw materials comprise polysorbate-801.2 g, glycerin monostearate 4.7g and glycerin 0.9 g; the water phase raw materials comprise 10.8g of liquid paraffin, 1.4g of sorbitan oleate, 1.4g of solid paraffin and 0.9g of vaseline; the dosage of the callicarpa nudiflora medicinal material extract is 3 g; 0.0729g of ethylparaben and 0.0243g of dimethyl sulfoxide;
preferably, in the preparation method of the Li YAO ZIZHU scald ointment, the emulsification temperature in the step (2) is 70 ℃, and the emulsification time is 25 minutes.
Process screening experiments:
first, optimization experiment of water extraction process of Callicarpa nudiflora
1. Purpose of experiment
Optimized process for extracting callicarpa nudiflora water preferably
2. Experimental methods
Reflux extraction with distilled water, selecting four factors of medicinal material soaking time, water consumption, extraction time and extraction frequency, selecting three levels for each factor, and arranging experiments according to orthogonal table as shown in table 1 and table 2.
TABLE 1 water extraction level factor table of Callicarpa nudiflora
Figure BDA0003107473980000021
TABLE 2 orthogonal experimental table for water extraction of callicarpa nudiflora
Figure BDA0003107473980000031
3. Results of the experiment
In summary, the best extraction process of beautyberry is A2B3C2D3Soaking for 2h, adding 12, 10 and 10 times of water, extracting for 3 times, wherein each extraction time is 1 h; the factor influences the primary and secondary>C>B>A, the extraction frequency has the largest influence on the extract yield, the extraction time is next, the amount of water is then the same, the influence is the soaking time, and according to the optimal process, the rate of extracting the callicarpa nudiflora medicinal material extract through a repeatability experiment is 19.9%.
Second, preparation of Callicarpa nudiflora ointment
1. Purpose of experiment
Screening the prescription of callicarpa nudiflora paste.
2. Procedure of experiment
Preparing w/o Callicarpa nudiflora ointment by emulsification method, heating oil phase, slowly adding water phase heated to the same temperature, slowly adding concentrated Callicarpa nudiflora extract, and stirring in the same direction while adding until emulsification and coagulation.
3. Results of the experiment
Firstly, an orthogonal experiment method is adopted, the emulsification effect (score of visual analysis, full score of 40 points) is taken as an index, and the optimal formula, emulsification temperature and emulsification time are selected preferably. The first prescription experiment orthogonal table is shown in tables 3 and 4; the orthogonal tables of the second prescription experiment are shown in tables 5 and 6.
TABLE 3 formula of Callicarpa nudiflora ointment-level factor table
Figure BDA0003107473980000041
TABLE 4 formulation-orthogonal analysis table for Callicarpa nudiflora ointment
Figure BDA0003107473980000042
Figure BDA0003107473980000051
Formula one-orthogonal table results for Callicarpa nudiflora ointment show: screening formula I of Callicarpa nudiflora ointment, wherein the optimal effect is A1B1C2D2
TABLE 5 formula two-level factor table of Callicarpa nudiflora ointment
Figure BDA0003107473980000052
TABLE 6 Diorthogonal analysis Table for prescription of Callicarpa nudiflora ointment
Figure BDA0003107473980000053
Figure BDA0003107473980000061
The results of the two-orthogonal analysis of the formula of the callicarpa nudiflora ointment show that: the best effect of the screened formula II of the callicarpa nudiflora ointment is A3B3C2D1
3. Results of the experiment
1. The comparative analysis of the experimental results shows that: prescription two A3B3C2D1Better than prescription one results in appearance and after trial, for A3B3C2D1Repeating the experiment for many times to meet the requirement, so that A of the second prescription is selected3B3C2D1The oil phase raw materials comprise polysorbate-801.2 g, glycerin monostearate 4.7g and glycerin 0.9 g; the water phase raw materials comprise 10.8g of liquid paraffin, 1.4g of sorbitan oleate, 1.4g of solid paraffin and 0.9g of vaseline; the emulsification was 70 ℃ and the emulsification time was 25 minutes.
2. And (3) inspecting the stability of the scald ointment: 10ml of callicarpa nudiflora scald ointment is put into a centrifuge tube, cooled to room temperature and then centrifuged for 1h at 4000r/min in a centrifuge. The stability inspection result shows that the scald ointment has stable property after centrifugation and is not layered, and the stability of the callicarpa nudiflora scald ointment is proved to meet the requirement.
Has the advantages that: compared with the prior art, the preparation method of the Li medicine Callicarpa nudiflora scald ointment provided by the invention has the following advantages:
the Li-medicine callicarpa nudiflora scald ointment prepared by optimizing raw materials through a large number of experiments, particularly optimizing a water extraction process of callicarpa nudiflora and a formula composition of callicarpa nudiflora ointment through a large number of experiments has the advantages of scientific and reasonable component proportion, stable performance, good promotion of wound healing, reliable curative effect and good safety. The preparation method of the Li medicine Callicarpa nudiflora scald ointment provided by the invention has the advantages of reasonable industrial design, strong operability, contribution to popularization and low production cost.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, as various equivalent modifications of the invention will occur to those skilled in the art upon reading the present disclosure and fall within the scope of the appended claims.
Example 1
A preparation method of Li's medicine Callicarpa nudiflora scald ointment is characterized by comprising the following steps:
(1) extracting callicarpa nudiflora:
taking a callicarpa nudiflora medicinal material, respectively adding water with the weight of 12, 10 and 10 times of the medicinal material, soaking for 2 hours, then performing reflux extraction for 1 hour each time, filtering, combining 3 times of water extract, and concentrating to obtain callicarpa nudiflora medicinal material extract;
(2) preparation of scald ointment
Preparing w/o callicarpa nudiflora scald ointment by adopting an emulsification method, heating oil phase raw material components of polysorbate-801.2 g, glyceryl monostearate 4.7g and glycerol 0.9g to 70 ℃, then slowly adding into water phase raw material liquid paraffin 10.8g, sorbitan oleate 1.4g, solid paraffin 1.4g and vaseline 0.9g which are heated to 70 ℃, then adding callicarpa nudiflora medicinal material fluid extract 3g, ethylparaben 0.12g and dimethyl sulfoxide 0.022g under stirring, and stirring, emulsifying and coagulating for 30 minutes in the same direction to obtain the Li medicine callicarpa nudiflora scald ointment.
Example 2 pharmacodynamic experiment of Callicarpa nudiflora ointment
1. Principle of experiment
Firstly, the degree or speed of wound healing can be changed under the action of medicaments on the scald wound, and macroscopic changes (such as the size of the wound area, the color, the hardness degree, the scabbing condition and the like) can be generated in the healing process.
② in the healing process of the scald wound, the content of some cell factors (TNF, IL, TGF, VEGF, etc.) in the body will change. The action mechanism of the medicine is explored according to the content change condition.
2. Experimental methods
Scalding SD rat and making mold: 30 SD rats (240 +/-10 g) were taken,randomly divided into 3 groups of 10 each, i.e. deep II0Scald experiment group (Callicarpa nudiflora scald ointment group prepared in example 1) and Shenqi II0Scald blank control group (matrix group without Callicarpa nudiflora extract), and deep II0Scald negative control group (blank). The rats were coated with sodium sulfide depilatory on their backs and gently scraped off after a few minutes. 24h after depilation, rats were anesthetized with an intraperitoneal injection of 20% urethane 1000 mg/kg. The rat is fixed on the molding board in a supine position (the size of the molding hole is about 6 cm)2) Exposing the back skin of the rat in the holes of the template, and placing the template in an electric heating constant-temperature water bath pan to scald for 12s at 80 ℃ to form a skin II0Scald.
(II) SD rat administration treatment: after the model is scalded and the model is made for 24 hours, a proper amount (0.3 mL/rat) of callicarpa nudiflora scalding ointment (prepared in example 1, the content of callicarpa nudiflora fluid extract is 19.9%) is smeared on the scalded part of the rat in the experimental group every day to form a uniform layer; uniformly smearing matrix (0.3 mL/rat) on the scalded part every day for empty control group rats; the negative control group was not administered. Each rat was housed in a single cage with adequate food and water.
Taking data and samples: after scald, the wound changes were recorded every 3 sun phases. Blood was collected from each mouse after orbital surgery every 5 days, and the blood sample was stood still for 30min, centrifuged (8000r/40min), and the supernatant was collected and stored at-70 ℃.
Fourthly, pathological section treatment: 21 days after scald, a large amount of sweat glands are generated in the dermis, a large amount of collagen fibers are simultaneously generated, the number of formed fibroblasts and capillaries is small, the epithelialization of the scald ointment group is basically finished, the healing is basically finished, the epithelialization of the matrix group and the blank group is incomplete, the generation of skin accessories is not obvious, and a large amount of fibroblasts and capillaries are simultaneously in the large proliferation period of granulation tissues.
Analyzing macroscopic area of the wound: the area of the photograph was calculated using Image J software, and the size of the wound area was the initial size of the wound.
The calculation formula is as follows: the percent wound area on day i.e. wound size on day i.e. initial wound size 100%, was averaged for each group and the data was analyzed using SPSS. The analytical results are shown in tables 7 and 8.
TABLE 7 macroscopic area of Callicarpa nudiflora ointment wound (area unit cm)2) Change table
Figure BDA0003107473980000081
TABLE 8 multiple comparisons of pharmacodynamic experiments with Callicarpa nudiflora ointment
Figure BDA0003107473980000082
Figure BDA0003107473980000091
4. Results of the experiment
The above experimental results show that: the wound area of the callicarpa nudiflora scald ointment group prepared by the invention is obviously smaller than that of the other two groups (P is less than 0.05), and it is worth mentioning that the wound size of the callicarpa nudiflora scald ointment group is the smallest from 8 th day, which shows that the callicarpa nudiflora scald ointment prepared by the invention has obvious treatment effect on scalds.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (1)

1. A preparation method of Li's medicine Callicarpa nudiflora scald ointment is characterized by comprising the following steps:
(1) extracting callicarpa nudiflora:
taking Callicarpa nudiflora, adding water with volume of 12, 10 and 10 times of the weight of the medicinal material respectively, soaking for 2h, then reflux-extracting for 1h each time, filtering, combining 3 times of water extract, and concentrating to obtain Callicarpa nudiflora medicinal material extract;
(2) preparation of scald ointment
Preparing w/o callicarpa nudiflora scald ointment by adopting an emulsification method, heating oil-phase raw materials of polysorbate-80, glyceryl monostearate and glycerin to 70-80 ℃, slowly adding the oil-phase raw materials into water-phase raw materials of liquid paraffin, sorbitan oleate, solid paraffin and vaseline which are heated to 70-80 ℃, then adding ethylparaben and dimethyl sulfoxide into the mixture under stirring, and the callicarpa nudiflora medicinal material fluid extract prepared in the step (1), and stirring, emulsifying and coagulating the mixture in the same direction for 20-40 minutes to obtain the Li medicine callicarpa nudiflora scald ointment;
the proportions of the components are as follows: polysorbate-801.2 g, glyceryl monostearate 4.7g, glycerol 0.9g, liquid paraffin 10.8g, sorbitan oleate 1.4g, solid paraffin 1.4g and vaseline 0.9g, callicarpa nudiflora medicinal material fluid extract 3g, ethylparaben 0.0729g and dimethyl sulfoxide 0.0243 g;
the emulsifying temperature in the step (2) is 70 ℃, and the emulsifying time is 25 minutes.
CN202110640642.8A 2016-11-07 2016-11-07 Preparation method of Li medicine Callicarpa nudiflora scald ointment Pending CN113318162A (en)

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Application publication date: 20210831