A kind of Xihuang pill and its preparation method and application

By controlling the particle size of beef yellow and musk and treating frankincense and myrrh with specific preparation methods, Xihuang Wan with significant analgesic and anti-inflammatory effects was prepared, which solved the problems of low activity and low efficacy of the active ingredients of the existing Xihuang Wan.

CN119280174BActive Publication Date: 2025-04-22CHANGCHUN HAIWANG BIOLOGICAL PHARM CO LTD
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Patent Information

Application Number
CN202411823433.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-12
Publication Date
2025-04-22
Estimated Expiration
2044-12-12

AI Technical Summary

Technical Problem

The existing preparation process of Xihuang Pills leads to low activity of active ingredients and low efficacy, and patients need to take a large amount of drugs and have low compliance.

Method used

By controlling the particle size of beef and musk, and burning the frankincense with ethanol-containing solution, heating step by step to obtain vinegar and frankincense with specific active ingredients; high-temperature preparation of myrrh to obtain vinegar and myrrh, and Xihuang Pills were prepared by mixing the components.

Benefits of technology

It significantly improves the analgesic and anti-inflammatory effects of Xihuang Wan, reduces the use of drug dosage, and improves efficacy and compliance.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention provides a Xihuang Pill and a preparation method and application thereof, and relates to the technical field of traditional Chinese medicine. The preparation method of the Xihuang Pill comprises the steps of: low-temperature crushing of bezoar and musk to obtain bezoar powder and musk powder; frankincense is mixed with an ethanol-containing solution, ignited and burned, 8%-15% vinegar is added, and the mixture is stirred at 80°C-100°C and then heated to 130°C-150°C and continued to stir-fry to obtain processed frankincense; myrrh is stir-fried at 100°C-150°C, and then vinegar equivalent to 10%-20% of the mass of myrrh is added, and the mixture is heated to 220°C-270°C and stir-fried to obtain processed myrrh; the components are mixed, and pills are made with water to obtain Xihuang Pills with significantly improved analgesic and anti-inflammatory effects.
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Description

Technical Field

[0001] The invention belongs to the technical field of traditional Chinese medicines, and particularly relates to a Xihuang Pill and a preparation method and application thereof. Background Art

[0002] Xihuang Pills have the effects of clearing away heat, detoxifying, reducing swelling and dispersing nodules. The traditional preparation process of Xihuang Pills is as follows: grind bezoar and musk into fine powder, steam and dry yellow rice, grind it into fine powder with vinegar frankincense and vinegar myrrh, sieve it, grind it with bezoar and musk powder, sieve it, mix it, make pills with water, and dry it in the shade.

[0003] The Xihuang Pills currently available on the market are prepared using traditional processes, which have the disadvantages of low activity of active ingredients and low efficacy. Due to the low efficacy, patients need to take a large amount of medicine, and patient compliance is low. Researchers have studied the components and preparation methods of Xihuang Pills in order to obtain products with high efficacy and stable performance.

[0004] Chinese invention patent CN105213458A discloses a Xihuang Pill and a preparation method thereof, comprising the steps of: crushing bezoar, bupleurum, frankincense, and myrrh into coarse powder, placing in a circulating ultrasonic extractor, adding water, germanium powder, and Tween 60 for ultrasonic extraction, jet spray drying, obtaining nano-extraction powder, and refining honey pills. The method prepares nano-extraction powder by ultrasonic and pressurized extraction of each component, and the obtained Xihuang Pill has a higher effective rate for the treatment of carbuncle furuncle, scrofula, flow injection, and cancer compared to the commercially available Xihuang Pill. However, compared to the traditional Xihuang Pill, the invention replaces musk with bupleurum, so the product of the invention is not a traditional Xihuang Pill product. In addition, the method of the invention adds the step of ultrasonic treatment, the process is complicated, and it is difficult to achieve in actual production.

[0005] Chinese invention patent CN114159489A discloses a method for preparing Xihuang Pills for detoxification and severing. The method comprises the following steps: using an ultra-low temperature pulverizer to pulverize bezoar and musk; then extracting vinegar frankincense and vinegar myrrh respectively: using 80% ethanol to soak and reflux extract the residues, and then using 60% ethanol to perform a second reflux extraction. The extracts are combined, freeze-dried, and air-flow pulverized into 200-mesh fine powders to obtain extracted vinegar frankincense and vinegar myrrh. The invention extracts vinegar frankincense and vinegar myrrh with ethanol, which will destroy the original active ingredient activity of the drug, and increases the extraction steps, which increases the cost.

[0006] Chinese invention patent CN102266372A discloses a new preparation method for preparing frankincense and myrrh for Xihuang Pills, which improves the steps of degreasing and vinegar making: drying frankincense or myrrh for 2 hours, replacing oil-absorbing paper several times, drying until the oil-absorbing paper shows star-shaped oil marks, and the temperature control range during drying and degreasing is 40°C-150°C; vinegar making: placing frankincense or myrrh in a pot, controlling the temperature for frying, adding 5% of the weight of frankincense or myrrh vinegar and continuing to stir-fry until the surface is bright, then taking it out, cooling and sealing; or first mixing frankincense or myrrh with 5% vinegar, controlling the temperature for stir-frying until the surface is bright, then taking it out, controlling the temperature for vinegar making at 40°C-200°C, and the stir-frying time before adding vinegar is 5min-40min, and the stir-frying time after adding vinegar is 5min-40min. Although the volatile oil content in the "vinegar frankincense" and "vinegar myrrh" obtained by this method is reduced, the analgesic and anti-inflammatory effects still need to be improved.

[0007] In order to save time and cost, traditional processing methods often use higher temperatures for short-term processing or lower temperatures for long-term processing for frankincense and myrrh. This results in high volatile oil content and complex components in vinegar frankincense and vinegar myrrh, and reduced content and activity of effective ingredients, which in turn affects efficacy.

[0008] In view of this, further in-depth research is needed on the preparation method of Xihuang Pills, in order to improve the content of active ingredients in Xihuang Pills, significantly enhance the analgesic and anti-inflammatory effects, and reduce the use of drug dosage. Summary of the invention

[0009] Aiming at the problems existing in the prior art, the invention provides a Xihuang Pill and a preparation method and application thereof, and improves the preparation method of the Xihuang Pill by controlling the particle sizes of crushed bezoar and musk; performing combustion treatment on frankincense with an ethanol solution and then gradually raising the temperature to prepare vinegar frankincense with specific active ingredients; performing high-temperature preparation on myrrh under the action of vinegar with a relatively high content to obtain vinegar myrrh; and mixing the components to obtain the Xihuang Pill with significantly improved analgesic and anti-inflammatory effects.

[0010] To achieve the above purpose, the technical solution adopted by the present invention is as follows:

[0011] First, the present invention provides a method for preparing Xihuang Pills, comprising the steps of:

[0012] (1) grinding bezoar and musk at low temperature, the particle size of the grinding is 200-300 mesh, and the grinding temperature is -20°C to -10°C, to obtain bezoar powder and musk powder;

[0013] (2) Mix frankincense with an ethanol solution, ignite and burn until the frankincense turns brown, add vinegar and stir-fry at 80°C-100°C for 5-10 minutes; heat to 130°C-150°C and continue to stir-fry for 5-10 minutes to obtain processed frankincense;

[0014] The amount of vinegar added is 8%-15% of the mass of frankincense;

[0015] (3) stir-fry the myrrh at 100°C-150°C, then add vinegar equivalent to 10%-20% of the mass of the myrrh, heat to 220°C-270°C, stir-fry for 8min-15min, and obtain the processed myrrh;

[0016] (4) mixing the frankincense processed in step (2) and the myrrh processed in step (3) with yellow rice, and grinding them into fine powder to obtain vinegar frankincense powder and vinegar myrrh powder with a particle size of 150-200 mesh;

[0017] (5) The bezoar powder and musk powder of step (1), the vinegar frankincense powder and vinegar myrrh powder of step (4) are made into pills with water to obtain Xihuang pills.

[0018] Preferably, in step (1), the particle size of the pulverized product is 250 mesh and the pulverizing temperature is -15°C.

[0019] Preferably, in step (2), the particle size of the frankincense is 60 mesh to 100 mesh.

[0020] More preferably, in step (2), the particle size of the frankincense is 80 mesh.

[0021] Preferably, in step (2), the ethanol-containing solution is not limited to white wine, yellow wine and ethanol; and the volume concentration of ethanol is ≥52%.

[0022] Further preferably, in step (2), the volume concentration of ethanol is 52%-90%; further preferably, the volume concentration of ethanol is 56%-80%; further preferably, the volume concentration of ethanol is 56%-60%.

[0023] Preferably, in step (2), the solid-to-liquid ratio of the frankincense to the ethanol-containing solution is 1:0.1-0.5 g / mL.

[0024] Further preferably, in step (2), the solid-to-liquid ratio of the frankincense to the ethanol-containing solution is 1:0.3 g / mL.

[0025] Preferably, in step (2) and step (3), the vinegar is not limited to rice vinegar or white vinegar; and the acetic acid concentration in the vinegar is 3%-9%.

[0026] More preferably, the acetic acid concentration is 4%-8%.

[0027] In some embodiments of the present invention, the acetic acid concentration of the vinegar is not limited to any range and value of 3%-9%, and is not limited to 3%-5%, 4%-9%, 4%-8%, 6%-9%, 3%, 4%, 5%, 6%, 7%, 8%, and 9%.

[0028] Preferably, in step (2), the amount of vinegar added is 10%-13% of the mass of frankincense; further preferably, in step (2), the amount of vinegar added is 12% of the mass of frankincense.

[0029] Preferably, step (2) is specifically as follows: mixing frankincense with an ethanol solution, igniting and burning until the frankincense turns brown, adding vinegar at 85°C-95°C and stir-frying for 6-8 minutes; heating to 135°C-145°C and continuing to stir-fry for 6-8 minutes to obtain processed frankincense.

[0030] More preferably, step (2) is specifically as follows: mixing frankincense with an ethanol solution, igniting and burning until the frankincense turns brown, adding vinegar and stir-frying at 90° C. for 7 minutes; heating to 140° C. and continuing to stir-fry for 7 minutes to obtain processed frankincense.

[0031] Preferably, step (3) is specifically as follows: stir-frying the myrrh at 110°C-130°C, then adding vinegar equivalent to 12%-18% of the mass of the myrrh, heating to 230°C-260°C and stir-frying for 9min-13min to obtain the processed myrrh.

[0032] Further preferably, step (3) is specifically as follows: stir-frying the myrrh at 120° C., then adding vinegar equivalent to 15% of the mass of the myrrh, heating to 250° C. and stir-frying for 12 minutes to obtain the processed myrrh.

[0033] Preferably, in step (4), the particle size of the vinegar frankincense powder and the vinegar myrrh powder is 180 mesh.

[0034] Preferably, in step (4), the mass of the yellow rice is 25%-35% of the total mass of the vinegar frankincense and vinegar myrrh.

[0035] Further preferably, in step (4), the mass of the yellow rice is 28%-32% of the total mass of the vinegar frankincense and vinegar myrrh.

[0036] Preferably, in step (4), the yellow rice is steamed and dried yellow rice.

[0037] Then, the present invention provides Xihuang Pills prepared by the above preparation method.

[0038] Preferably, the Xihuang Pills include the following raw materials in parts by weight: 10-20 parts of bezoar, 10-20 parts of musk, 400-700 parts of frankincense and 400-700 parts of myrrh.

[0039] Further preferably, the Xihuang Pills comprise the following raw materials in parts by weight: 13-18 parts of bezoar, 13-18 parts of musk, 470-610 parts of frankincense and 470-610 parts of myrrh.

[0040] More preferably, the Xihuang Pills comprise the following raw materials in parts by weight: 15 parts of bezoar, 15 parts of musk, 550 parts of frankincense and 550 parts of myrrh.

[0041] Finally, the present invention provides the use of the Xihuang Pills in preparing medicines with anti-inflammatory and analgesic effects.

[0042] In the present invention, the bezoar is not limited to natural bezoar, cultured bezoar or in vitro cultured bezoar.

[0043] In the present invention, the musk is artificial musk.

[0044] Compared with the prior art, the present invention has the following beneficial effects:

[0045] 1. The present invention mixes frankincense with an ethanol-containing solution and performs combustion treatment. The principle of like dissolves like is adopted to facilitate the dissolution of irrelevant volatile oils, alcohols, organic acid esters and other components in the frankincense, thereby increasing the content and activity of components such as boswellic acid. In the subsequent vinegar-making process, a lower temperature can be used to achieve the preparation of vinegar frankincense, and the analgesic and anti-inflammatory effects can be effectively exerted.

[0046] 2. The present invention first stir-fries the myrrh at low temperature, and then adds vinegar equivalent to 10%-20% of the mass of the myrrh for high temperature stir-frying, thereby maintaining a high content of analgesic and antioxidant components and improving analgesic and anti-inflammatory effects.

[0047] 3. The various components in the preparation method of the present invention complement each other and significantly improve the analgesic and anti-inflammatory effects. DETAILED DESCRIPTION

[0048] The following non-limiting examples can enable those skilled in the art to more fully understand the present invention, but do not limit the present invention in any way. The following content is merely an exemplary description of the scope of the present invention, and those skilled in the art can make various changes and modifications to the present invention based on the disclosed content, which should also fall within the scope of the present invention.

[0049] When the embodiments give numerical ranges, it should be understood that, unless otherwise specified in the present invention, both endpoints of each numerical range and any numerical value between the two endpoints can be selected. Unless otherwise defined, all technical and scientific terms used in the present invention have the same meanings as those generally understood by those of ordinary skill in the art to which the present invention belongs.

[0050] The present invention is further described below by way of specific examples. The various chemical reagents used in the examples of the present invention are obtained through conventional commercial channels unless otherwise specified. Products from different manufacturers have no significant effect on the effect. The acetic acid concentration in the white vinegar used in the examples of the present invention is 4%, which is only an exemplary concentration, and the examples do not limit the concentration of acetic acid.

[0051] Basic Example 1

[0052] The raw material components of Xihuang Pills are calculated by weight as follows: 13-18 parts of bezoar, 13-18 parts of musk, 470-610 parts of frankincense and 470-610 parts of myrrh.

[0053] Basic Example 2

[0054] The raw material components of Xihuang Pills are calculated by weight as follows: 10-20 parts of bezoar, 10-20 parts of musk, 400-700 parts of frankincense and 400-700 parts of myrrh.

[0055] The Xihuang Pills of the above basic embodiments can all achieve the technical effects of the present invention.

[0056] In the following examples, the raw material components of Xihuang Pills are calculated by weight as follows: 15 parts of bezoar, 15 parts of musk, 550 parts of frankincense and 550 parts of myrrh.

[0057] Example 1

[0058] A preparation method of Xihuang Pills is:

[0059] (1) natural bezoar and musk are ground at low temperature at -15°C to a particle size of 250 meshes to obtain bezoar powder and musk powder;

[0060] (2) Frankincense was mixed with an ethanol solution having a volume concentration of 56% at a solid-liquid ratio of 1:0.3 g / mL, and ignited until the frankincense turned brown, and white vinegar was added and stir-fried at 90°C for 7 min; then the temperature was raised to 140°C and stir-fried for another 7 min to obtain processed frankincense;

[0061] The amount of white vinegar added is 12% of the mass of frankincense; the concentration of acetic acid in white vinegar is 4%;

[0062] (3) Stir-fry myrrh at 120°C, then add white vinegar equivalent to 15% of the mass of myrrh, heat to 250°C and stir-fry for 12 minutes to obtain processed myrrh; the concentration of acetic acid in the white vinegar is 4%;

[0063] (4) mixing the frankincense prepared in step (2), the myrrh prepared in step (3) and the steamed and dried yellow rice and grinding them into fine powder to obtain vinegar frankincense powder and vinegar myrrh powder with a particle size of 180 mesh;

[0064] The amount of yellow rice added is 30% of the total mass of vinegar frankincense and vinegar myrrh;

[0065] (5) The bezoar powder and musk powder of step (1), the vinegar frankincense powder and vinegar myrrh powder of step (4) are made into pills with water to obtain Xihuang pills.

[0066] Example 2

[0067] A preparation method of Xihuang Pills is:

[0068] (1) Crush the in vitro cultured bezoar and musk at -20°C to obtain bezoar powder and musk powder with a particle size of 300 meshes;

[0069] (2) Frankincense was mixed with an ethanol solution having a volume concentration of 60% at a solid-liquid ratio of 1:0.2 g / mL, and ignited until the frankincense turned brown. White vinegar was added and stir-fried at 95°C for 6 min. The temperature was then raised to 135°C and stir-fried for 8 min to obtain processed frankincense.

[0070] The amount of white vinegar added is 12% of the mass of frankincense; the concentration of acetic acid in white vinegar is 4%;

[0071] (3) Stir-fry the myrrh at 110°C, then add white vinegar equivalent to 12% of the mass of the myrrh, heat to 230°C and stir-fry for 13 minutes to obtain the processed myrrh; the concentration of acetic acid in the white vinegar is 4%;

[0072] (4) mixing the frankincense prepared in step (2), the myrrh prepared in step (3) and the steamed and dried yellow rice and grinding them into fine powder to obtain vinegar frankincense powder and vinegar myrrh powder with a particle size of 150 mesh;

[0073] The amount of yellow rice added is 30% of the total mass of vinegar frankincense and vinegar myrrh;

[0074] (5) The bezoar powder and musk powder of step (1), the vinegar frankincense powder and vinegar myrrh powder of step (4) are made into pills with water to obtain Xihuang pills.

[0075] Example 3

[0076] A preparation method of Xihuang Pills is:

[0077] (1) Cultivating bezoar and musk and grinding them at low temperature at -10°C, with the particle size of the grinding being 200 meshes, to obtain bezoar powder and musk powder;

[0078] (2) Frankincense was mixed with an ethanol solution having a volume concentration of 60% at a solid-liquid ratio of 1:0.1 g / mL. The mixture was ignited and burned until the frankincense turned brown, then white vinegar was added and stir-fried at 85°C for 8 min. The mixture was then heated to 145°C and stir-fried for 6 min to obtain processed frankincense.

[0079] The amount of white vinegar added is 10% of the mass of frankincense; the concentration of acetic acid in white vinegar is 4%;

[0080] (3) Stir-fry the myrrh at 130°C, then add white vinegar equivalent to 15% of the mass of the myrrh, heat to 260°C and stir-fry for 9 minutes to obtain the processed myrrh; the concentration of acetic acid in the white vinegar is 4%;

[0081] (4) mixing the frankincense processed in step (2), the myrrh processed in step (3) and the steamed and dried yellow rice and grinding them into fine powder to obtain vinegar frankincense powder and vinegar myrrh powder with a particle size of 200 mesh;

[0082] The amount of yellow rice added is 30% of the total mass of vinegar frankincense and vinegar myrrh;

[0083] (5) The bezoar powder and musk powder of step (1), the vinegar frankincense powder and vinegar myrrh powder of step (4) are made into pills with water to obtain Xihuang pills.

[0084] Example 4

[0085] A preparation method of Xihuang Pills is:

[0086] (1) Same as Example 1;

[0087] (2) Frankincense was mixed with an ethanol solution having a volume concentration of 56% at a solid-liquid ratio of 1:0.4 g / mL. The mixture was ignited and burned until the frankincense turned brown, then white vinegar was added and stir-fried at 100°C for 5 min. The mixture was then heated to 150°C and stir-fried for another 5 min to obtain processed frankincense.

[0088] The amount of white vinegar added is 15% of the mass of frankincense; the concentration of acetic acid in white vinegar is 4%;

[0089] (3) Stir-fry the myrrh at 100°C, then add white vinegar equivalent to 10% of the mass of the myrrh, heat to 220°C and stir-fry for 8 minutes to obtain the processed myrrh; the concentration of acetic acid in the white vinegar is 4%;

[0090] (4) mixing the frankincense prepared in step (2), the myrrh prepared in step (3) and the steamed and dried yellow rice and grinding them into fine powder to obtain vinegar frankincense powder and vinegar myrrh powder with a particle size of 180 mesh;

[0091] The amount of yellow rice added is 25% of the total mass of vinegar frankincense and vinegar myrrh;

[0092] (5) Same as Example 1.

[0093] Example 5

[0094] (1) Same as Example 1;

[0095] (2) Frankincense was mixed with an ethanol solution with a volume concentration of 80% at a solid-liquid ratio of 1:0.5 g / mL. The mixture was ignited and burned until the frankincense turned brown, then white vinegar was added and stir-fried at 80°C for 10 min. The temperature was then raised to 130°C and stir-fried for another 10 min to obtain processed frankincense.

[0096] The amount of white vinegar added is 8% of the mass of frankincense; the concentration of acetic acid in white vinegar is 4%;

[0097] (3) Stir-fry the myrrh at 150°C, then add white vinegar equivalent to 20% of the mass of the myrrh, heat to 270°C and stir-fry for 15 minutes to obtain the processed myrrh; the concentration of acetic acid in the white vinegar is 4%;

[0098] (4) mixing the frankincense prepared in step (2), the myrrh prepared in step (3) and the steamed and dried yellow rice and grinding them into fine powder to obtain vinegar frankincense powder and vinegar myrrh powder with a particle size of 180 mesh;

[0099] The amount of yellow rice added is 35% of the total mass of vinegar frankincense and vinegar myrrh;

[0100] (5) Same as Example 1.

[0101] Comparative Example 1

[0102] According to the process of invention patent CN102266372A, vinegar myrrh and vinegar frankincense are prepared, and the obtained vinegar myrrh and vinegar frankincense are prepared into Xihuang Pills. The specific steps are:

[0103] (1) Same as Example 1;

[0104] (2) Take 1 kg of the medicinal material frankincense, chop it into pieces the size of soybeans, spread it flat on a plate lined with oil-absorbing paper, control the temperature to 95°C and dry it for 2 hours, move the frankincense to another plate lined with oil-absorbing paper and continue drying; replace the oil-absorbing paper several times according to the above drying method, and dry it until the oil-absorbing paper is no longer oily (there are spots of oil); put the frankincense in a pot, control the temperature to 120°C and stir-fry for 10 minutes, add 5% vinegar (acetic acid concentration is 4%), continue to stir-fry for 5 minutes, take it out after the surface is shiny, and cool it to obtain the processed frankincense;

[0105] (3) Take 1 kg of the medicinal material myrrh, chop it into pieces the size of soybeans, spread it flat on a plate lined with oil-absorbing paper, control the temperature to 95°C and dry it for 2 hours, move the myrrh to another plate lined with oil-absorbing paper and continue drying; change the oil-absorbing paper several times according to the above drying method, and dry it until the oil-absorbing paper is no longer oily (there are spots of oil); put the myrrh in a pot, control the temperature to 120°C and stir-fry for 10 minutes, add 5% vinegar (acetic acid concentration is 4%), continue to stir-fry for 5 minutes, remove it after the surface is shiny, and cool it to obtain the processed myrrh;

[0106] Step (4)-Step (5): Same as Example 1.

[0107] Comparative Example 2

[0108] The difference from Example 1 is that step (2) does not involve the step of heating and stir-frying, and specifically comprises:

[0109] Step (2): frankincense is mixed with an ethanol solution with a volume concentration of 56% at a solid-liquid ratio of 1:0.3 g / mL, and white vinegar is added after igniting and burning until the frankincense turns brown, and stir-frying is continued at 140° C. for 14 minutes to obtain processed frankincense; the amount of white vinegar added is 12% of the mass of the frankincense; and the concentration of acetic acid in the white vinegar is 4%.

[0110] The remaining steps are the same as those in Example 1.

[0111] Comparative Example 3

[0112] The difference from Example 1 is that in step (2), no ethanol is added for ignition and combustion treatment before stir-frying, specifically:

[0113] Step (2): frankincense and white vinegar are mixed, stir-fried at 90°C for 7 minutes; then the temperature is raised to 140°C and stir-fried for 7 minutes to obtain processed frankincense; the amount of white vinegar added is 12% of the mass of the frankincense; the concentration of acetic acid in the white vinegar is 4%.

[0114] The remaining steps are the same as those in Example 1.

[0115] Comparative Example 4

[0116] The difference from Example 1 is that the volume concentration and the amount of ethanol solution added in step (2) are different, specifically:

[0117] Step (2): frankincense is mixed with an ethanol solution with a volume concentration of 43% at a solid-liquid ratio of 1:0.05 g / mL, and white vinegar is added after igniting and burning until the frankincense turns brown, and stir-fried at 90° C. for 7 minutes; then the temperature is raised to 140° C. and stir-fried for 7 minutes to obtain processed frankincense; the amount of white vinegar added is 12% of the mass of the frankincense; and the concentration of acetic acid in the white vinegar is 4%.

[0118] The remaining steps are the same as those in Example 1.

[0119] Comparative Example 5

[0120] The difference from Example 1 is that the amount of white vinegar added in step (2) is different, specifically:

[0121] Step (2): frankincense is mixed with an ethanol solution with a volume concentration of 56% at a solid-liquid ratio of 1:0.3 g / mL, and white vinegar is added after igniting and burning until the frankincense turns brown, and stir-fried at 90° C. for 7 minutes; then the temperature is raised to 140° C. and stir-fried for 7 minutes to obtain processed frankincense; the amount of white vinegar added is 5% of the mass of the frankincense; and the concentration of acetic acid in the white vinegar is 4%.

[0122] The remaining steps are the same as those in Example 1.

[0123] Comparative Example 6

[0124] The difference from Example 1 is that the amount of vinegar added in step (3) is different, specifically:

[0125] Step (3): stir-fry the myrrh at 120° C., then add white vinegar equivalent to 5% of the mass of the myrrh, heat to 250° C. and stir-fry for 12 minutes to obtain the processed myrrh; the concentration of acetic acid in the white vinegar is 4%.

[0126] The remaining steps are the same as those in Example 1.

[0127] Comparative Example 7

[0128] The difference from Example 1 is that the stir-frying temperature in step (3) is different, specifically:

[0129] Step (3): stir-fry the myrrh at 120° C., then add white vinegar equivalent to 15% of the mass of the myrrh, heat to 180° C. and stir-fry for 12 minutes to obtain the processed myrrh; the concentration of acetic acid in the white vinegar is 4%.

[0130] The remaining steps are the same as those in Example 1.

[0131] Test 1: Color uniformity test

[0132] Experimental method: Use a colorimeter to detect the color of Xihuang Pills. The colorimeter illumination source is D65, the slit width is 1nm, the field of view is selected as 10°, and the wavelength scanning range is 380-780nm, so as to evaluate the effect of the preparation method of Xihuang Pills on the appearance color.

[0133] Chromaticity parameter value L of Xihuang Pills The test results of appearance and color are shown in Table 1.

[0134] Table 1

[0135]

[0136] In Table 1, each comparative example group is compared with Example 1. &&& P<0.001, with statistical significance (x±s, n=10); each comparative example group was compared with Example 2 group ###P<0.001, indicating statistically significant difference (x±s, n=10); each comparative example group was compared with Example 3 group $ P<0.05, $$$ P<0.001, indicating statistically significant difference (x±s, n=10); each comparative example group was compared with Example 4 group △△△ P<0.001, indicating statistically significant difference (x±s, n=10); each comparative example group was compared with Example 5 group ¢¢¢ P<0.001, indicating statistical significance (x±s, n=10).

[0137] As can be seen from Table 1, the Xihuang Pills obtained by the present invention have a bright surface and uniform color. The specific processing method adopted by the present invention can obtain Xihuang Pills with bright color, while the Xihuang Pills of the comparative example using the conventional method have a bright surface and uniform color. Uneven, dull surface.

[0138] Experiment 2: Analgesia and anti-inflammatory test

[0139] 1. Experimental animals and groups, experimental drugs and reagents

[0140] 1.1 Experimental Animals:

[0141] SPF-grade ICR mice, weighing 18 g-22 g, animal certificate number: 210726240100647226, were purchased from Liaoning Changsheng Biotechnology Co., Ltd., production license number: SCK (Liao) 2020-001.

[0142] The mice were divided into two groups, one for analgesia experiment (females) and the other for anti-inflammatory experiment (half males and half females).

[0143] Feed: SPF mouse feed was purchased from Liaoning Changsheng Biotechnology Co., Ltd.

[0144] Breeding environment: barrier environment animal observation room, temperature: 20℃-24℃, relative humidity: 40%-70%, mouse use license: (Ji) 2022-004.

[0145] 1.2 Experimental reagents and instruments: Xylene was purchased from Tianjin Yongsheng Fine Chemical Co., Ltd., and RB-200 intelligent hot plate instrument was produced by Chengdu Taimeng Software Co., Ltd.

[0146] 1.3 Experimental drugs: Xihuang Pills of Examples 1 to 5, and Xihuang Pills of Comparative Examples 1 to 7.

[0147] 1.4 Experimental animal grouping and drug administration:

[0148] Analgesia experiment: After 3 days of adaptive feeding, female mice were randomly divided into 13 groups, with 10 mice in each group, namely: Example 1 group, Example 2 group, Example 3 group, Example 4 group, Example 5 group, Comparative Example 1 group, Comparative Example 2 group, Comparative Example 3 group, Comparative Example 4 group, Comparative Example 5 group, Comparative Example 6 group, Comparative Example 7 group, and were gavaged with 2.5 g / kg dose of Xihuang Pills; the model control group was gavaged with the same dose of normal saline; the mice were gavaged with a volume of 20 mL / kg, once a day, for 7 consecutive days.

[0149] Anti-inflammatory experiment: After adaptive feeding for 3 days, mice (half male and half female) were randomly divided into 13 groups, with 10 mice in each group, namely: Example 1 group, Example 2 group, Example 3 group, Example 4 group, Example 5 group, Comparative Example 1 group, Comparative Example 2 group, Comparative Example 3 group, Comparative Example 4 group, Comparative Example 5 group, Comparative Example 6 group, Comparative Example 7 group, and were gavaged with 2.5 g / kg dose of Xihuang Pills; the model control group was gavaged with the same dose of normal saline; the mice were gavaged with a volume of 20 mL / kg, once a day, for 7 consecutive days.

[0150] 2. Experimental methods

[0151] 2.1 Hot plate method for pain threshold detection:

[0152] At room temperature of 25°C, mice were placed on a hot plate analgesia instrument preheated to (55±0.5)°C. The time (s) from when the mouse touched the hot plate to when it licked its hind paw was taken as the pain threshold of the mouse. Mice with a pain threshold of 5s-30s were subjected to subsequent testing experiments.

[0153] One hour after the last intragastric administration of the test substance, the mice were placed in a hot plate analgesia instrument. The time until the mice licked their hind paws was the pain threshold of the mice (s). The pain threshold time of each group of mice was recorded, and the significance of the differences among the groups was compared.

[0154] 2.2 Detection method of xylene-induced ear swelling in mice:

[0155] 1 hour after the last intragastric administration of the test substance, 0.04 mL of xylene was immediately applied to the front and back surfaces of the left ear of the mouse. The mouse was killed 2 hours later, the left and right ear pieces were cut off, and a 7 mm diameter puncher was used to punch round ear pieces at the same position. The weight of the two ear pieces was weighed with an analytical balance, and the weight of the left ear piece of each mouse was subtracted from the weight of the right ear piece to calculate the swelling degree of the ear piece of each group (swelling degree = left ear piece weight - right ear piece weight). The swelling rate was also calculated, swelling rate (%) = (left ear piece weight - right ear piece weight) / left ear piece weight × 100%.

[0156] 2.3 Statistical analysis

[0157] SPSS 26.0 software was used to process the data.

[0158] 3. Experimental results

[0159] The analgesic test results of Xihuang Pills are shown in Table 2, and the anti-inflammatory test results of Xihuang Pills are shown in Table 3.

[0160] Table 2

[0161]

[0162] In Table 2, the embodiment and comparative example groups were compared with the model control group. ▲ P<0.05, ▲▲ P<0.01, ▲▲▲ P<0.001, with statistically significant difference; Comparative Example 1 compared each group, aa P<0.01, aaa P<0.001, with statistically significant difference; Comparative Example 2 compared each group, bb P<0.01, bbb P<0.001, with statistically significant difference; Comparative Example 3 compared each group, c P<0.05, cc P<0.01, ccc P<0.001, with statistically significant difference; Comparative Example 4 compared each group, d P<0.05, dd P<0.01, ddd P<0.001, with statistically significant difference; Comparative Example 5 compared each group, e P<0.05, ee P<0.01, eee P<0.001, which was statistically significant.

[0163] Table 3

[0164]

[0165] In Table 3, the embodiment and comparative example groups were compared with the model control group. ▲▲▲ P<0.001, with statistically significant difference; Comparative Example 1 compared each group, aaa P<0.001, with statistically significant difference; Comparative Example 2 compared each group, bbb P<0.001, with statistically significant difference; Comparative Example 3 compared each group, ccc P<0.001, with statistically significant difference; Comparative Example 4 compared each group, dd P<0.01, ddd P<0.001, with statistically significant difference; Comparative Example 5 compared each group, ee P<0.01, eeeP<0.001, which was statistically significant.

[0166] 4. Summary

[0167] The hot plate method and xylene induced inflammation method were used to determine the analgesic and anti-inflammatory effects of Xihuang Pills. The pain threshold, swelling degree and swelling rate of each group of mice in the example were significantly lower than those in the model control group at 30min and 60min after administration, and there was a very significant difference (P<0.001); the pain threshold of each group of mice in the control group was significantly lower than that in the model control group after administration, and the swelling degree and swelling rate were significantly increased, with significant differences; the pain threshold, swelling degree and swelling rate of Example 1 after administration were statistically different from those of the control group.

[0168] Therefore, although the Xihuang Pills prepared by the prior art also have certain analgesic and anti-inflammatory effects, the Xihuang Pills prepared by the specific preparation method of the present invention have better analgesic and anti-inflammatory effects than the Xihuang Pills prepared by the conventional method. The technical solution of the present invention brings about significantly improved analgesic and anti-inflammatory effects.

[0169] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, rather than to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions of the technical solution of the present invention by ordinary technicians in this field do not deviate from the essence and scope of the technical solution of the present invention.

Claims

1. A method for preparing Xihuang Pills, characterized in that: Includes steps: (1) grinding bezoar and musk at low temperature to a particle size of 200-300 meshes at a temperature of -20 to -10°C to obtain bezoar powder and musk powder; the bezoar is not limited to natural bezoar, cultured bezoar or in vitro cultured bezoar; (2) Mix frankincense with an ethanol solution, ignite and burn until the frankincense turns brown, add vinegar and stir-fry at 80-100°C for 5-10 minutes; heat to 130-150°C and continue to stir-fry for 5-10 minutes to obtain processed frankincense; In the ethanol-containing solution, the volume concentration of ethanol is ≥52%; the solid-liquid ratio of frankincense to the ethanol-containing solution is 1:0.1-0.5 g / mL; the amount of vinegar added is 8%-15% of the mass of frankincense; (3) Stir-fry the myrrh at 100-150°C, then add vinegar equivalent to 10%-20% of the mass of the myrrh, heat to 220-270°C and stir-fry for 8-15 minutes to obtain the processed myrrh; (4) mixing the frankincense processed in step (2) and the myrrh processed in step (3) with yellow rice, and grinding them into fine powder to obtain vinegar frankincense powder and vinegar myrrh powder with a particle size of 150-200 mesh; (5) The bezoar powder and musk powder of step (1), the vinegar frankincense powder and vinegar myrrh powder of step (4) are made into pills with water to obtain Xihuang pills.

2. The preparation method according to claim 1, characterized in that: In step (1), the particle size of the pulverized product is 250 mesh and the pulverizing temperature is -15°C.

3. The preparation method according to claim 1, characterized in that: In step (2), the particle size of the frankincense is 60-100 mesh.

4. The preparation method according to claim 1, characterized in that: In step (2), the amount of vinegar added is 10%-13% of the mass of frankincense; Step (2) is specifically as follows: mix frankincense with an ethanol solution, ignite and burn until the frankincense turns brown, add vinegar and stir-fry at 85-95° C. for 6-8 minutes; heat to 135-145° C. and continue to stir-fry for 6-8 minutes to obtain processed frankincense.

5. The preparation method according to claim 4, characterized in that: In step (2), the amount of vinegar added is 12% of the mass of frankincense; Step (2) is specifically as follows: mix frankincense with an ethanol solution, ignite and burn until the frankincense turns brown, add vinegar and stir-fry at 90° C. for 7 minutes; heat to 140° C. and continue to stir-fry for 7 minutes to obtain processed frankincense.

6. The preparation method according to claim 1, characterized in that: Step (3) is specifically as follows: stir-frying the myrrh at 110-130° C., then adding vinegar equivalent to 12%-18% of the mass of the myrrh, heating to 230-260° C. and stir-frying for 9-13 minutes to obtain the processed myrrh.

7. The preparation method according to claim 6, characterized in that: Step (3) is specifically as follows: stir-frying the myrrh at 120° C., then adding vinegar equivalent to 15% of the mass of the myrrh, heating to 250° C. and stir-frying for 12 minutes to obtain the processed myrrh.

8. The preparation method according to claim 1, characterized in that: In step (4), the particle size of the vinegar frankincense powder and vinegar myrrh powder is 180 mesh; In step (4), the yellow rice accounts for 25%-35% of the total mass of the vinegar frankincense and vinegar myrrh.

9. Xihuang Pills prepared by the preparation method according to any one of claims 1 to 8, characterized in that: The invention comprises the following raw materials in parts by weight: 10-20 parts of bezoar, 10-20 parts of musk, 400-700 parts of frankincense and 400-700 parts of myrrh.

10. Use of the Xihuang Pills according to claim 9 in the preparation of medicines with anti-inflammatory and analgesic effects.

Citation Information

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