Preparation method of traditional Chinese medicine composition for treating burns and scalds

Abstract

The application discloses a preparation method of a traditional Chinese medicine composition for treating burns and scalds. The traditional Chinese medicine composition is composed of Huangbai, Huzhang and Bingpian. The preparation method comprises the following steps: firstly, Huangbai is subjected to percolation extraction to obtain percolation liquid A, and the obtained percolation liquid A is concentrated; then, the concentrated percolation liquid A and an organic solvent are used to perform countercurrent percolation on Huzhang to obtain a Huzhang-Huangbai composite extraction liquid; and finally, Bingpian is crushed and dissolved in propylene glycol or glycerol, and the Huzhang-Huangbai composite extraction liquid and sterile water are added. The preparation process greatly improves the extraction utilization rate of Huangbai and Huzhang. The preparation method does not rely on a large amount of high-concentration ethanol for extraction and preparation, and the obtained product does not contain high-concentration ethanol, so the product prepared by the application is more suitable for people who are sensitive to alcohol, and the stability of the product is higher.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of traditional Chinese medicine preparation, and relates to a preparation method of a traditional Chinese medicine composition for treating burns and scalds. BACKGROUND

[0002] Shoushangling tincture was included in the 2005 edition of Chinese Pharmacopoeia, and the prescription is rhizoma polygoni codifolii 200g, cortex phellodendri 50g and borneol 10g, which has the functions of clearing heat and drying dampness, detoxifying and detumescence, and astringing and analgesia, and can be used for detoxification, detumescence and analgesia of red and swollen skin, disinfection and treatment of mild trauma, and treatment of I and II degree burns and scalds caused by various reasons. However, the production process of the current Shoushangling tincture mainly relies on ethanol extraction and blending, and the ethanol content in the final drug can reach 70% to 75%, which makes the product unsuitable for alcohol allergy patients and children, and limits the application range of the product.

[0003] However, ethanol is needed for extraction and preparation in the production and formula of such drugs. For example, the Chinese invention patent application No. 202111145889.9, a kind of burn tincture for treating burns and its preparation method, discloses that the components of the burn tincture include cortex phellodendri, rhizoma polygoni codifolii, borneol, ash tree bark, catechu, safflower, rhubarb, cold water stone, incense, purple grass, muscle healing agent, scar removal agent, itching and bacteriostatic agent, wind-preventing, salvia miltiorrhiza and cortex miltiorrhizae, and scar removal agent; the preparation process also needs to rely on ethanol for extraction and preparation. This is because ethanol has better extraction effect on such components. For example, the article Optimization of Extraction Process of Total Alkaloids from Cortex Phellodendri (Journal of Jinggangshan University - Natural Science Edition, May 2010, Fan Jiaoyou and Zhang Songzhu) optimizes the extraction process of total alkaloids from cortex phellodendri, and finds that alcohol extraction is better than water extraction, and the extraction rate can be increased by 32.03% by ethanol extraction.

[0004] Therefore, it is necessary to study the preparation method of tincture products for treating burns and scalds without ethanol. SUMMARY

[0005] The purpose of the present application is to prepare tincture products for treating burns and scalds without ethanol, and to ensure the content and effect of each component.

[0006] The technical scheme adopted by the present application provides a preparation method of a traditional Chinese medicine composition for treating burns and scalds, and the components of the traditional Chinese medicine composition are composed of cortex phellodendri, rhizoma polygoni codifolii and borneol, and the key lies in that the preparation method is as follows:

[0007] First, percolation extraction is performed on Phellodendron chinense to obtain percolation liquid A, and the obtained percolation liquid A is concentrated. Then, the concentrated percolation liquid A and an organic solvent are used to perform countercurrent percolation on Polygonum cuspidatum to obtain a composite extract of Polygonum cuspidatum and Phellodendron chinense. Then, borneol is crushed and dissolved in propylene glycol or glycerol, and the composite extract of Polygonum cuspidatum and Phellodendron chinense and sterile water are added to obtain the product.

[0008] Specifically, the mass ratio of the above-mentioned Phellodendron chinense, Polygonum cuspidatum and borneol is 8:10:1, and the mass ratio of the above-mentioned borneol, propylene glycol or glycerol and sterile water is 1:8-10:180-190.

[0009] Furthermore, the specific operating steps of the percolation extraction of Phellodendron chinense are as follows:

[0010] Phellodendron chinense is crushed, soaked in ethanol for 2-4 hours, and then percolated with ethanol to collect percolation liquid A; the collected percolation liquid A is concentrated under reduced pressure to obtain concentrated percolation liquid A, which is concentrated to 1 / 3-1 / 4 of the original volume and the ethanol is evaporated.

[0011] Furthermore, the specific operating steps of countercurrent percolation of Japanese knotweed using concentrated percolate A and an organic solvent are as follows:

[0012] The polygonum cuspidatum was crushed, and the concentrated percolation solution A was soaked for 2-4 hours, and then an organic solvent was added for countercurrent percolation to obtain percolation solution B, which was concentrated under reduced pressure and the solvent was evaporated to obtain a composite extract of polygonum cuspidatum and phellodendron.

[0013] Preferably, the concentration of the ethanol is 60% to 80%, and the mass of the ethanol is 3 to 4 times the mass of Phellodendron chinense.

[0014] It should also be noted that before soaking Phellodendron amurense in ethanol, it needs to be soaked in dilute hydrochloric acid at a temperature of 40°C to 50°C for 1 hour to 2 hours.

[0015] Preferably, the above-mentioned organic solvent refers to any one of ethyl acetate or methyl acetate, and the mass of the organic solvent used is 1.5 to 2 times the mass of knotweed.

[0016] Preferably, the above-mentioned pulverization is pulverizing to a particle size of 20 mesh to 60 mesh.

[0017] Preferably, the percolation rate is 2 mL / kg to 3 mL / kg.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] The present invention reduces the proportion of Phellodendron chinense and Polygonum cuspidatum components in the process, but the content of the main components related to the above two medicinal materials in the product does not decrease, but increases. This shows that the preparation method of the present invention greatly improves the extraction utilization rate of Phellodendron chinense and Polygonum cuspidatum;

[0020] The present invention does not rely on a large amount of ethanol for extraction and preparation, and the resulting product does not contain high concentrations of ethanol. It is not only suitable for people who are sensitive to alcohol and children, but also avoids the phenomenon of rapid reduction in skin surface moisture caused by the use of alcohol products, thereby improving the comfort of use.

[0021] The product prepared by the present invention has higher stability. After being sealed and placed in a high-temperature and high-humidity environment for 6 months, the content of the main component, emodin, is reduced by 28.3%, which is 0.57 times the reduction rate of the commercially available product. If the process of the present invention is applied to the production of the product, the shelf life of the product can be extended. Moreover, after being placed for 6 months, the product prepared by the present invention meets the requirements of the identification test, indicating that under the condition that the process is well controlled and the equipment is not contaminated, even if high-concentration ethanol with an antibacterial effect is not used and only sterile water is used for preparation, it can be ensured that the product will not deteriorate. DETAILED DESCRIPTION

[0022] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of them. All other embodiments derived by persons of ordinary skill in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0023] If the specific conditions are not specified in the examples, the experiments can be carried out under conventional conditions; if the manufacturers of the reagents or instruments are not specified, they are all conventional products that can be purchased from the market.

[0024] For the convenience of description, the following description is based on parts by mass.

[0025] Example 1

[0026] S1. Grind 40 parts of Phellodendron amurense into 40 mesh size, soak the Phellodendron amurense powder in 45 parts of dilute hydrochloric acid at 45°C for 1.5 hours, filter and dry to remove the hydrochloric acid;

[0027] S2. Soak the Phellodendron chinense soaked in hydrochloric acid in 140 parts of 75% ethanol for 3 hours, then place the percolator for percolation at a rate of 2.5 mL / kg, collect the percolate A, and concentrate the collected percolate A under reduced pressure to 1 / 3 of its original volume. Then, remove the ethanol by evaporation to obtain a concentrated percolate A. The ethanol content of the concentrated percolate A is less than 0.5%.

[0028] S3, take 50 parts of polygonum cuspidatum, crush to 40 mesh, soak in concentrated percolation liquid A for 3 hours, then add 75 parts of ethyl acetate for countercurrent percolation, control the percolation speed at 2 mL / kg, pay attention to sealing during the percolation process to prevent excessive volatilization of organic solvents, obtain percolation liquid B, reduce pressure and concentrate and evaporate the organic solvent to obtain a polygonum cuspidatum and phellodendron chinense composite extract, wherein the ethanol content is less than 0.01%, and the ethyl acetate content is less than 0.1%;

[0029] S4, crush 5 parts of borneol to 60 mesh, dissolve in 40 parts of propylene glycol, add the polygonum cuspidatum and phellodendron chinense composite extract, stir until fully dissolved, and add to 950 parts of sterile water to prepare an ethanol-free shenshangling tincture sample 1.

[0030] Example two

[0031] S1, take 40 parts of phellodendron chinense and crush to 20 mesh, soak the phellodendron chinense powder in 40 parts of dilute hydrochloric acid at a temperature of 50°C for 1 hour, filter and dry to remove the hydrochloric acid;

[0032] S2, soak the phellodendron chinense in 120 parts of 60% ethanol for 2 hours, then place it in a percolator for percolation, control the percolation speed at 3 mL / kg, collect the percolation liquid A, reduce the pressure and concentrate the collected percolation liquid A to 1 / 4 of the original volume, evaporate the ethanol to obtain concentrated percolation liquid A, and the ethanol content in the concentrated percolation liquid A is less than 0.5%;

[0033] S3, take 50 parts of polygonum cuspidatum and crush to 20 mesh, soak in concentrated percolation liquid A for 2 hours, then add 100 parts of methyl acetate for countercurrent percolation, control the percolation speed at 3 mL / kg, pay attention to sealing during the percolation process to prevent excessive volatilization of organic solvents, obtain percolation liquid B, reduce pressure and concentrate and evaporate the organic solvent to obtain a polygonum cuspidatum and phellodendron chinense composite extract, wherein the ethanol content is less than 0.01%, and the methyl acetate content is less than 0.1%;

[0034] S4, crush 10 parts of borneol to 70 mesh, dissolve in 45 parts of propylene glycol, add the polygonum cuspidatum and phellodendron chinense composite extract, stir until fully dissolved, and add to 925 parts of sterile water to prepare an ethanol-free shenshangling tincture sample 2.

[0035] Example three

[0036] S1, take 40 parts of phellodendron chinense and crush to 60 mesh, soak the phellodendron chinense powder in 50 parts of dilute hydrochloric acid at a temperature of 40°C for 2 hours, filter and dry to remove the hydrochloric acid;

[0037] S2. Soak the Phellodendron chinense soaked in hydrochloric acid in 160 parts of 80% ethanol for 4 hours, then place the percolator for percolation at a rate of 2 mL / kg, collect the percolate A, and concentrate the collected percolate A under reduced pressure to 1 / 3 of its original volume. Then, remove the ethanol by evaporation to obtain a concentrated percolate A. The ethanol content of the concentrated percolate A is less than 0.5%.

[0038] S3, take 50 parts of polygonum cuspidatum, crush them into 60 mesh, soak them with concentrated percolation liquid A for 4h, then add 80 parts of ethyl acetate for countercurrent percolation, control the percolation rate to 2.5mL / kg, pay attention to sealing during the percolation process to prevent excessive volatilization of the organic solvent, obtain percolation liquid B, concentrate under reduced pressure and evaporate the organic solvent to obtain a composite extract of polygonum cuspidatum and phellodendron, wherein the ethanol content is less than 0.01% and the ethyl acetate content is less than 0.1%;

[0039] S4. Crush 7.5 parts of borneol into 80 mesh size, dissolve in 50 parts of glycerol, add the composite extract of Polygonum cuspidatum and Phellodendron chinense, stir until fully dissolved, add to 900 parts of sterile water, and mix thoroughly to prepare ethanol-free Shaoshangling tincture sample 3.

[0040] Comparative Example 1

[0041] S1. Same as step S1 of Example 1, except that the cortex phellodendri was crushed to 60 mesh;

[0042] S2. The Phellodendron chinense and 50 parts of polygonum cuspidatum crushed to 60 mesh after being soaked in hydrochloric acid were extracted with 220 parts of 75% ethanol for 12 hours, and the extract was concentrated under reduced pressure to 1 / 3 of the original volume, and the ethanol was evaporated to obtain a composite extract of polygonum cuspidatum and Phellodendron chinense control 1, with the ethanol content being controlled to be less than 0.2%;

[0043] S3. Prepare the Shaoshangling Tincture Reference Substance 1 by the same method as S4 in Example 1.

[0044] Comparative Example 2

[0045] S1. Same as step S1 of Example 1, except that the cortex phellodendri was crushed to 60 mesh;

[0046] S2, the cortex phellodendri and 50 parts of polygonum cuspidatum crushed to 60 mesh after being soaked in hydrochloric acid were soaked in 220 parts of 75% ethanol for 3 hours, and then placed in a percolator for percolation, and the percolation rate was controlled at 2.5 mL / kg. The percolation liquid was concentrated under reduced pressure to 1 / 3 of the original volume, and the ethanol was evaporated to obtain the polygonum cuspidatum cortex composite extract control 2, and the ethanol content was controlled to be less than 0.2%;

[0047] S3. Prepare the Shaoshangling Tincture Reference Substance 2 by the same method as S4 in Example 1.

[0048] Comparative Example 3

[0049] S1. Same as step S1 of Example 1, except that the cortex phellodendri was crushed to 60 mesh;

[0050] S2, soak the cortex phellodendri and 50 parts of polygonum cuspidatum crushed to 60 mesh after being soaked in hydrochloric acid, soak them in 100 parts of ethyl acetate for 3 hours, then place them in a percolator and add 100 parts of water for countercurrent percolation, control the percolation rate to 2.5 mL / kg, and concentrate the percolation liquid under reduced pressure to 1 / 3 of the original volume, and evaporate the ethyl acetate to obtain the polygonum cuspidatum and cortex phellodendri composite extract control 3, controlling the ethyl acetate content to be less than 0.2%;

[0051] S3. Prepare the Shaoshangling Tincture Reference Substance 3 by the same method as S4 in Example 1.

[0052] Comparative Example 4

[0053] S1. Same as step S1 of Example 1, except that the cortex phellodendri was crushed to 60 mesh;

[0054] S2. Extracting the Phellodendron chinense soaked in hydrochloric acid with 140 parts of 75% ethanol for 12 hours, concentrating the extract under reduced pressure to 1 / 3 of its original volume, and removing the ethanol by evaporation to obtain a concentrated extract, wherein the ethanol content of the concentrated extract is less than 0.5%;

[0055] S3, take 50 parts of polygonum cuspidatum, crush them into 40 mesh, soak them with concentrated extract for 3h, then add 75 parts of ethyl acetate for countercurrent percolation, control the percolation rate to 2mL / kg, pay attention to sealing during the percolation process to prevent excessive volatilization of the organic solvent, obtain percolation solution B, concentrate under reduced pressure and evaporate the organic solvent to obtain a composite extract of polygonum cuspidatum and phellodendron, wherein the ethanol content is less than 0.01% and the ethyl acetate content is less than 0.1%;

[0056] S4. Prepare the Shaoshangling tincture reference substance 4 by the same method as step S4 in Example 1.

[0057] Comparative Example 5

[0058] The commercially available Shaoshangling tincture product (manufacturer: Hebei Aoxing Group Pharmaceutical Co., Ltd.) was used as the reference substance 5.

[0059] Analysis and testing

[0060] 1. According to the record on page 1524 of Part 1 of the 2020 edition of the Chinese Pharmacopoeia, the high performance liquid chromatography method was used to detect the emodin in the test sample. The Chinese Pharmacopoeia standard requires that the emodin content be no less than 0.35 mg / mL. The results are shown in Table 1.

[0061] 2. Use colorimetry to detect total anthraquinones and total alkaloids in the sample:

[0062] (1) Detection method of total anthraquinones:

[0063] Weigh 25 mg of the sample to be tested, place it in a 100 mL flat-bottom flask, add 6.0 mL of a mixed acid solution of hydrochloric acid and glacial acetic acid (2:18), reflux in a boiling water bath for 15 minutes, cool, add 30 mL of ether for extraction, filter and wash the extract, then add 4.0 mL of the mixed acid solution, reflux in a boiling water bath for 15 minutes, cool, extract, filter and wash with ether again, wash the extract twice with water, discard the water washing liquid, add a mixed alkali solution of sodium hydroxide and ammonia water (1:1) to the ether layer to make up the volume, let it stand for 30 minutes, use the mixed alkali solution as a blank control, and determine the absorbance colorimetrically at 525 nm.

[0064] Using 1,8-dihydroxyanthraquinone as the standard substance, a standard curve was drawn and a regression equation was obtained. The total anthraquinone content of the sample was calculated. The results are shown in Table 1.

[0065] (2) Detection method of total alkaloids:

[0066] Weigh 50 mg of the sample to be tested, place it in a 100 mL volumetric flask and dilute to volume with anhydrous ethanol. Use anhydrous ethanol as a blank control and measure the absorbance colorimetrically at 340 nm.

[0067] Berberine hydrochloride was used as the standard substance, a standard curve was drawn and a regression equation was obtained. The content of total alkaloids in the samples was calculated. The results are shown in Table 1.

[0068] 3. Use high performance liquid chromatography to detect the content of resveratrol and resveratrol glycosides in the sample to be tested:

[0069] The chromatographic conditions were an ODS Hypersil column (4.6 mm × 250.0 mm, 5 μm), a mobile phase of acetonitrile / water (20 / 80), a detection wavelength of 310 nm, a flow rate of 1 mL / min, an injection volume of 10 μL, and a column temperature of 25°C. The results are shown in Table 1.

[0070] 4. According to the general technical part of Part IV of the 2020 edition of the "Chinese Pharmacopoeia", the ethanol, ethyl acetate and methyl acetate in the test samples except the reference substance 5 were detected by high-performance gas chromatography. The determination of ethanol in the reference substance 5 was based on the record on page 1524 of Part I of the 2020 edition of the "Chinese Pharmacopoeia". The results are shown in Table 1.

[0071] 5. Test the moisturizing effect of the sample to be tested:

[0072] In a laboratory at a temperature of 25°C and a relative humidity of 45%, the test samples were sprayed on the skin surface of one group of test subjects, and a blank control group was used as a control group without spraying the test samples. Each group included 10 test subjects (aged 22 to 25 years old, with a male to female ratio of 1:1). The skin surface humidity was measured at 0h, 1h, 3h and 6h, and the average value of the measurements was used as the statistical result. The results are shown in Table 2.

[0073] 6. Investigation of the stability of the sample under accelerated conditions:

[0074] Sample 1, reference substance 4 and reference substance 5 were sealed and placed at a temperature of 40°C ± 2°C and a relative humidity of 75% ± 5% for 6 months. According to the record on page 1524 of Part 1 of the 2020 edition of the "Chinese Pharmacopoeia", the ethanol content and emodin content of the test samples were measured, and an identification test was carried out in the 6th month. The results are shown in Table 3.

[0075] Table 1: Summary of test results of main components in the tested samples

[0076]

[0077]

[0078] As can be seen from the results in Table 1, the samples of each embodiment of the present invention all meet the requirements of the pharmacopoeia standard for the content of emodin, and the test results of each major component are all higher than those of existing products. In contrast, the contents of emodin, total anthraquinones, resveratrol, and resveratrol glycosides in reference samples 1 to 3 are much lower than those in reference sample 5, and the content of total alkaloids is not much different from that in reference sample 5. This is mainly because the proportion of knotweed used in the control group is about 1 / 4 of that in the pharmacopoeia process, while the main components of knotweed are emodin, total anthraquinones, resveratrol, and resveratrol glycosides.

[0079] Since a large amount of ethanol is not used for extraction and preparation in the process of the present invention, no ethanol is detected in the sample, and only a small amount of ethyl acetate or methyl acetate remains, thereby minimizing the impact of organic solvents on the human body.

[0080] Table 2: Test results of moisturizing effect of the samples to be tested

[0081] Average skin surface humidity (%) 0h 1h 3h 6h Sample 1 85.5 78.6 69.2 55.3 Sample 2 86.1 79.1 69.5 55.5 Sample 3 84.9 78.4 68.8 55.4 Reference substance 1 85.2 78.5 68.2 55.3 Reference substance 2 86.2 79.1 69.2 55.2 Reference substance 3 84.3 78.9 60.2 50.1 Reference substance 4 85.6 79.0 59.8 51.2 Reference substance 5 86.2 71.2 30.7 31.2 Blank control 48.7 48.5 48.1 48.2

[0082] As can be seen from the results in Table 2, the control product 5, i.e. the commercially available product, not only has no moisturizing effect, but also the humidity of the test skin surface drops rapidly 3 hours after use, indicating that the large amount of ethanol evaporates, causing the test subject's skin to become dry, reducing the comfort of use.

[0083] In order to make borneol dissolve in water, propylene glycol or glycerol is used to dissolve borneol first, and the process of propylene glycol or glycerol assisted dissolution is used. In addition, propylene glycol or glycerol can also have a moisturizing effect at a low concentration, which shows that there is still a moisturizing effect after 6 hours of use, thereby improving the comfort of use. Furthermore, propylene glycol or glycerol has a penetration effect, which can help the absorption of effective components in the product and improve the utilization rate of effective components.

[0084] Table 3: Accelerated stability test results of the samples to be tested

[0085]

[0086] As can be seen from the results in Table 3, under the accelerated stability test conditions, i.e. high temperature and high humidity conditions, the content of emodin in the product of the present application is still much higher than the standard of the pharmacopoeia after being placed for 6 months, and the product of the present application meets the requirements of the identification test. The content of emodin in the product of the present application is reduced by 28.3%, while the content of emodin in the commercially available product is reduced by 49.4%, and the content of emodin in the control product 4 is reduced by 43.5%, which shows that the product prepared by the present application has more stable properties. If the process of the present application is applied to the production of the product, the shelf life of the product can be prolonged.​

Claims

1. A method for preparing a traditional Chinese medicine composition for treating burns and scalds, wherein the composition is composed of Phellodendron chinense, Polygonum cuspidatum and Borneol, characterized in that: The preparation method is: First, percolation extraction is performed on Phellodendron chinense, the Phellodendron chinense is crushed, soaked in ethanol for 2 to 4 hours, and then percolated with ethanol to collect percolation liquid A; the collected percolation liquid A is concentrated under reduced pressure to 1 / 3 to 1 / 4 of the original volume, and the ethanol is evaporated to obtain concentrated percolation liquid A; the concentrated percolation liquid A and an organic solvent are then used to countercurrently percolate on Polygonum cuspidatum to obtain a composite extract of Polygonum cuspidatum and Phellodendron chinense; borneol is then crushed and dissolved in propylene glycol or glycerol, and the composite extract of Polygonum cuspidatum and Phellodendron chinense and sterile water are added to obtain the product; The ethanol concentration is 60% to 80%, and the mass of the ethanol is 3 to 4 times that of the cortex phellodendri; The organic solvent refers to either ethyl acetate or methyl acetate; The mass ratio of the cortex phellodendri, knotweed and borneol is 8:10:1-2, and the mass ratio of the borneol, propylene glycol or glycerol and sterile water is 1-2:8-10:180-190; Before soaking Phellodendron chinense in ethanol, it needs to be soaked in dilute hydrochloric acid at 40℃~50℃ for 1h~2h. The specific operating steps of countercurrent percolation of Japanese knotweed using concentrated percolate A and an organic solvent are as follows: The Polygonum cuspidatum was crushed and soaked in concentrated percolation solution A for 2 to 4 hours, and then an organic solvent was added for countercurrent percolation to obtain percolation solution B, which was concentrated under reduced pressure and the solvent was evaporated to obtain a composite extract of Polygonum cuspidatum and Phellodendron chinense.

2. The method for preparing a Chinese medicine composition for treating burns and scalds according to claim 1, wherein: The mass of the organic solvent used is 1.5 to 2 times that of the knotweed.

3. The method for preparing a Chinese medicine composition for treating burns and scalds according to claim 1, wherein: The pulverization is to pulverize to a particle size of 20 mesh to 60 mesh.

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