Guibingxugushubi paste and its preparation process

Abstract

This invention relates to the field of traditional Chinese medicine preparation technology, and discloses a Guihong Xugu Shubi Paste and its preparation process, comprising the following Chinese medicinal herbs: Angelica sinensis, Carthamus tinctorius, Angelica pubescens, Homalomena occulta, Commiphora myrrha, Catechu, Borneol, Frankincense, Eucommia ulmoides, Eupolyphaga sinensis, Prunus persica, Pheretima aspergillum, Angelica dahurica, Rheum palmatum, Dipsacus asper, Citrus reticulata peel, Glycyrrhiza uralensis, Pinellia ternata, Calcined natural copper, Bupleurum chinense, Drynaria fortunei, Acer palmatum bark, Trichosanthes kirilowii, Cinnamomum cassia, Dioscorea hypoglauca, Notopterygium incisum, and Dragon's Blood. This Guihong Xugu Shubi Paste, targeting the distinctly different properties of borneol (volatile crystalline), frankincense and myrrh (viscous resin), Carthamus tinctorius (fibrous), and Pheretima aspergillum (keratinous), abandons the practice of separately pulverizing and then mixing the herbs. Instead, it employs a process where all twenty-seven herbs are dried together and then mixed and pulverized. This utilizes the adsorption and encapsulation effect of the powder generated during the pulverization process of other powdery herbs on the viscous resin and the dispersing and grinding effect on the fibrous and keratinous herbs.

Description

Technical Field

[0001] This invention relates to the field of traditional Chinese medicine preparation technology, and in particular to a Guihong Xugu Shubi paste and its preparation process. Background Technology

[0002] Guihong Xugu Shubi Paste is a traditional Chinese medicine external preparation with the effects of promoting blood circulation, removing blood stasis, promoting tendon and bone healing, reducing swelling and relieving pain. Clinically, it is mainly used for tendon and bone pain, rheumatic pain, and traumatic injuries caused by wind-cold-dampness and blood stasis. It is suitable for the adjunctive treatment of soft tissue contusions, fractures, arthritis, cervical spondylosis, lumbar disc herniation and other diseases. This preparation is made into a paste by adding honey to more than 20 kinds of medicinal materials with different properties.

[0003] In the production and preparation of traditional Chinese medicine external pastes, the pulverization of medicinal materials is a fundamental step affecting product quality and production efficiency. However, the above-mentioned prescription contains numerous medicinal ingredients with vastly different physical properties, posing significant technical challenges to the pulverization process. Borneol, being a volatile crystalline medicinal material, is easily sublimated and lost during pulverization due to mechanical heat generation. Frankincense and myrrh, being resinous medicinal materials, contain a large amount of viscous components, and when pulverized alone, they easily soften and adhere to the inner wall of the pulverizer and the screen, resulting not only in material loss and low pulverization yield but also in difficulties in cleaning the process. Safflower and earthworm, respectively, are fibrous and keratinous medicinal materials, and their individual pulverization efficiency is low. How to efficiently and with low loss pulverize these more than twenty medicinal materials with different properties is the primary technical challenge in the production of this preparation.

[0004] In terms of formulation technology, topical pastes require the finished product to have moderate consistency and good spreadability so that they can be evenly applied to the affected area and maintain sufficient contact time. The ratio of finely powdered medicinal materials to honey, the excipient, directly determines the physical properties of the paste: too little honey results in a viscous paste with poor flowability and difficulty in even application; too much honey results in a thin paste that is prone to dripping and difficult to stay effectively on the affected area. For compound pastes composed of nearly thirty kinds of medicinal materials, the honey absorption characteristics of the finely powdered medicinal materials are significantly different from those of simple prescriptions. Conventional experience in the amount of honey used cannot be directly applied, and the optimal ratio needs to be determined through systematic experiments.

[0005] In terms of quality control, for large compound preparations composed of more than 20 medicinal materials, how to establish a systematic and highly specific identification method system to achieve simultaneous quality monitoring of multiple core medicinal materials is an important topic for the standardization and normalization research of this type of preparation.

[0006] Furthermore, some medicinal materials in the prescription require specific processing before they can be used in medicine. For example, frankincense and myrrh need to be processed with vinegar to reduce their irritation and enhance their blood-activating and pain-relieving effects; pinellia needs to be processed with ginger and alum to reduce its toxicity; and natural copper needs to be calcined and quenched to facilitate pulverization and the dissolution of active ingredients. The standardization of these pretreatment processes is also crucial to ensuring the quality stability of the final product. Summary of the Invention

[0007] Given that borneol is a volatile crystalline medicinal material, it is easily sublimated and lost during pulverization due to mechanical heat generation; frankincense and myrrh are resinous medicinal materials containing a large amount of viscous components, which easily soften and adhere to the inner wall of the pulverizer and the screen when pulverized alone, resulting not only in the loss of medicinal materials and low pulverization yield, but also in the difficulty of cleaning up; safflower and earthworm are fibrous and horny medicinal materials, respectively, and their individual pulverization efficiency is not high, this invention addresses the problem of how to efficiently and with low loss pulverize these more than twenty kinds of medicinal materials with different properties.

[0008] Therefore, the purpose of this invention is to provide a preparation process for Guihong Xugu Shubi Paste, which aims to achieve a preparation process and quality control scheme for Guihong Xugu Shubi Paste that is feasible for compound prescriptions of multiple medicinal materials, has an optimized formulation ratio, and is quality controllable.

[0009] To solve the above-mentioned technical problems, the present invention provides the following technical solution: a preparation process for Guihong Xugu Shubi Paste, wherein the raw materials of Guihong Xugu Shubi Paste include the following Chinese medicinal herbs: Angelica sinensis, safflower, Angelica pubescens, Homalomena occulta, myrrh, catechu, borneol, frankincense, Eucommia ulmoides, Eupolyphaga sinensis, peach kernel, earthworm, Angelica dahurica, rhubarb, Dipsacus asper, tangerine peel, licorice, Pinellia ternata, calcined natural copper, Bupleurum chinense, Drynaria fortunei, Acer palmatum bark, Trichosanthes kirilowii, cinnamon twig, Dioscorea hypoglauca, Notopterygium incisum, and dragon's blood. The preparation process includes the following steps: Step 1: Drying the medicinal slices: Dry all the medicinal slices described above at 60±2℃; Step 2: Mixing and grinding: Mix all the dried Chinese herbal medicine pieces together and grind them to obtain fine powder; Step 3: Sieving and mixing: Pass the fine powder through a 100-mesh sieve, collect the sieved powder and mix it evenly to obtain the medicinal material fine powder; Step 4: Refining the honey: Take honey, add 20% water by weight, and heat to refine it into medium-quality honey; Step 5: Mixing and preparing paste: Mix the fine powder of the medicinal materials with the honey at a weight ratio of 1:2.9 and stir evenly to obtain Guihong Xugu Shubi Paste.

[0010] As a preferred embodiment of the preparation process of the Guihong Xugu Shubi Paste of the present invention, in step two, the mixing and pulverizing involves putting all the dried Chinese herbal medicine pieces into the same pulverizer for joint pulverization, utilizing the dispersion and adsorption effects of the powdery medicinal materials in the Chinese herbal medicine pieces on volatile medicinal materials, viscous resinous medicinal materials, fibrous medicinal materials and keratinous medicinal materials to complete the pulverization; cooling measures are taken during the pulverization process to control the material temperature.

[0011] As a preferred embodiment of the preparation process of the Guihong Xugu Shubi Paste of the present invention, the relative weight parts of each Chinese herbal medicine slice in the raw materials are as follows: Angelica sinensis 7-14 parts, Carthamus tinctorius 15-25 parts, Angelica pubescens 4-15 parts, Homalomena occulta 5-15 parts, Commiphora myrrha 5-15 parts, Catechu 2-7 parts, Borneol 3-9 parts, Frankincense 5-15 parts, Eucommia ulmoides 8-18 parts, Eupolyphaga sinensis 5-15 parts, Prunus persica 1-6 parts. Earthworm 5-15 parts, Angelica dahurica 5-15 parts, Rhubarb 13-24 parts, Dipsacus asper 5-15 parts, Tangerine peel 5-15 parts, Licorice 5-15 parts, Ginger-processed Pinellia ternata 4-12 parts, Calcined natural copper 5-14 parts, Bupleurum chinense 2-9 parts, Drynaria fortunei 5-15 parts, Acer palmatum bark 5-15 parts, Trichosanthes kirilowii root 5-15 parts, Cinnamomum cassia 5-15 parts, Dioscorea hypoglauca 5-15 parts, Notopterygium incisum 1-8 parts, Dragon's blood 2-12 parts.

[0012] As a preferred embodiment of the preparation process of the Guihong Xugu Shubi Paste of the present invention, the following are the ingredients of the Chinese herbal medicine: frankincense and myrrh are processed by stir-frying with vinegar until the surface is shiny; calcined natural copper is processed by calcining and quenching until it is dark red and then quenched with vinegar until the surface is blackish-brown and the luster disappears; ginger-processed Pinellia is processed by decocting fresh ginger slices, adding alum and cooking Pinellia together until thoroughly cooked; and hot-processed Drynaria fortunei is processed by scalding with sand until it bulges and the hair is removed by banging.

[0013] As a preferred embodiment of the preparation process of the Guihong Xugu Shubi Paste of the present invention, the Guihong Xugu Shubi Paste is packaged in a 20g or 500g box, using a polypropylene box.

[0014] As a preferred embodiment of the Guihong Xugu Shubi Paste of the present invention, the Guihong Xugu Shubi Paste has at least one of the following quality inspection items: Microscopic identification based on the rubbery fibers in Eucommia ulmoides as a microscopic identification feature; Thin-layer chromatography identification of Angelica sinensis using ligustilide as a reference; Thin-layer chromatographic identification of safflower using safflower reference material as a control; Thin-layer chromatographic identification of Angelica pubescens using dihydroaperitol angelica ester as a reference; Thin-layer chromatographic identification of Dipsacus asperoides using Dipsacus saponin VI as a reference; Thin-layer chromatographic identification of borneol using borneol reference standard; Thin-layer chromatographic identification of frankincense using frankincense reference material as a reference; Thin-layer chromatographic identification of rhubarb using emodin as a reference; Thin-layer chromatography identification of dried tangerine peel with hesperidin as a reference; Thin-layer chromatographic identification of licorice with glycyrrhizin as a reference; Thin-layer chromatographic identification of Drynaria fortunei with naringin as a control; Thin-layer chromatographic identification of Notopterygium incisum with isoimperatorin as a reference.

[0015] As a preferred embodiment of the Guihong Xugu Shubi Paste of the present invention, the content of alcohol-soluble extract of the Guihong Xugu Shubi Paste, determined by cold soaking method with anhydrous ethanol as solvent, shall not be less than 29.6%.

[0016] Compared with the prior art, the present invention has at least the following beneficial effects: 1. This invention addresses the issue of borneol (volatile crystalline), frankincense and myrrh (viscous resins), safflower (fibrous), and earthworm (horny) in prescriptions, which have vastly different properties. Instead of separately pulverizing and then mixing them, this invention employs a process where all twenty-seven medicinal materials are dried together and then mixed and pulverized. By utilizing the adsorption and encapsulation effect of the powder generated during the pulverization process of other powdery medicinal materials on the viscous resin and the dispersing and grinding effect on the fibrous and horny medicinal materials, the problem of frankincense and myrrh adhering to the inner wall of the pulverizer is effectively reduced. At the same time, the measure of cooling before pulverization reduces the loss of volatile components.

[0017] 2. Through systematic screening experiments, this invention uses the appearance and coating performance of the paste as evaluation indicators to determine the optimal ratio of fine medicinal powder to honey as 1:2.9. When the two are mixed in this ratio, the resulting paste has moderate consistency, good fluidity, and is easy to apply evenly to the affected area. This overcomes the problems caused by traditional empirical ratios, such as pastes that are too thick to apply or too thin to flow. This ratio has been verified by three batches of pilot-scale production, with a yield rate of over 94% and stable and controllable physical properties of the preparation.

[0018] 3. This invention establishes a comprehensive and systematic thin-layer chromatography identification method for multiple core medicinal materials in the prescription. It can specifically identify at least twelve medicinal materials, including Eucommia ulmoides and Cinnamomum cassia (microscopic identification), Angelica sinensis (ligustilide), Carthamus tinctorius, Angelica pubescens (dihydroaperitol angelica ester), Dipsacus asper (dipsacus saponin VI), Borneol, Boswellia carterii, Rheum palmatum (emodin), Citrus reticulata (hesperidin), Glycyrrhiza uralensis (glycyrrhizin), Drynaria fortunei (naringin), and Notopterygium incisum (isoimperatorin). Moreover, this identification system covers a wide range of medicinal materials and has strong specificity, providing a scientific and systematic detection method for the accuracy of ingredient addition and batch-to-batch quality consistency of Guihong Xugu Shubi Paste.

[0019] 4. This invention has been verified through three batches of pilot-scale production tests. The complete process route parameters, from drying, mixing and pulverizing, sieving to refining with honey, mixing and making paste, and packaging, are clear, well-defined, and controllable. The pulverization yield of the three batches of samples is consistently above 95%, and the finished product rate is above 94%. All quality indicators meet the internal control standards, proving that the process route design is reasonable, has good reproducibility, and is suitable for promotion and application in preparation rooms and Chinese medicine production enterprises. Attached Figure Description

[0020] Figure 1This is a flowchart of the preparation process steps for the Guihong Xugu Shubi Paste of the present invention. Detailed Implementation

[0021] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.

[0022] I. Prescription Composition and Explanation This invention provides a Guihong Xugu Shubi Paste, the raw materials of which are composed of the following Chinese medicinal herbs: Angelica sinensis, safflower, Angelica pubescens, Homalomena occulta, myrrh, catechu, borneol, frankincense, Eucommia ulmoides, Eupolyphaga sinensis, peach kernel, earthworm, Angelica dahurica, rhubarb, Dipsacus asper, tangerine peel, licorice, Pinellia ternata, calcined natural copper, Bupleurum chinense, Drynaria fortunei, Acer palmatum bark, Trichosanthes kirilowii, cinnamon twig, Dioscorea hypoglauca, Notopterygium incisum, and dragon's blood.

[0023] In a preferred embodiment, the relative weight parts of each Chinese herbal medicine slice are as follows: Angelica sinensis 10 parts, Carthamus tinctorius 19 parts, Angelica pubescens 10 parts, Homalomena occulta 10 parts, Commiphora myrrha 10 parts, Catechu 4 parts, Borneol 6 parts, Boswellia carterii 10 parts, Eucommia ulmoides 12 parts, Eupolyphaga sinensis 10 parts, Prunus persica 4 parts, Pheretima aspergillum 10 parts, Angelica dahurica 10 parts, Rheum palmatum 19 parts, Dipsacus asper 10 parts, Citrus reticulata peel 10 parts, Glycyrrhiza uralensis 10 parts, Pinellia ternata 8 parts, Calcined natural copper 8 parts, Bupleurum chinense 6 parts, Drynaria fortunei 10 parts, Acer palmatum 10 parts, Trichosanthes kirilowii 10 parts, Cinnamomum cassia 10 parts, Dioscorea hypoglauca 10 parts, Notopterygium incisum 4 parts, and Dracaena cochinchinensis 6 parts.

[0024] The formula consists of Angelica sinensis, Carthamus tinctorius, Prunus persica, and Dracaena cochinchinensis, which invigorate blood circulation, remove blood stasis, unblock meridians, and relieve pain; Frankincense and Myrrh, which invigorate blood circulation, reduce swelling, promote tissue regeneration, and relieve pain. These are the principal herbs. Rhubarb, Eupolyphaga sinensis, and Pheretima aspergillum break up blood stasis, remove blood stasis, unblock meridians, and invigorate collaterals; Calcined natural copper disperses blood stasis and promotes bone healing; Dipsacus asper and Drynaria fortunei tonify the liver and kidneys and promote tendon and bone healing. These are the assistant herbs. Angelica pubescens, Notopterygium incisum, Homalomena occulta, Angelica dahurica, and Cinnamomum cassia dispel wind and dampness, warm the meridians, and unblock collaterals; Eucommia ulmoides, Trichosanthes kirilowii, Dioscorea hypoglauca, and Ligusticum striatum promote diuresis, reduce swelling, and strengthen tendons and bones; Tangerine peel, Pinellia ternata, and Bupleurum chinense regulate qi, dry dampness, and harmonize the middle jiao. These are the adjuvant herbs. Catechu astringes dampness, promotes wound healing, and promotes tissue regeneration; Borneol clears heat, reduces swelling, and relieves pain; and Glycyrrhiza uralensis harmonizes the other herbs. These are the guiding herbs. The combined effects of these herbs are to invigorate blood circulation, remove blood stasis, promote tendon and bone healing, reduce swelling, and relieve pain.

[0025] II. Sources and Identification of Raw Materials for Traditional Chinese Medicine All Chinese medicinal herbs used in this invention have been identified and tested, and meet the requirements of the current Pharmacopoeia of the People's Republic of China or relevant local medicinal material standards. The sources and applicable standards of each medicinal material are shown in the table below:

[0026]

[0027]

[0028]

[0029] III. Processing and Preparation of Chinese Medicinal Herbs Some Chinese medicinal herbs require specific processing before use. The specific processing methods for each herb are as follows: Angelica sinensis: After harvesting, remove the fibrous roots and mud. After the moisture has evaporated slightly, bundle them into small bunches, put them on a shed, and slowly dry them with smoke.

[0030] Safflower: Pick the inflorescences and dry them in the shade or in the sun.

[0031] Angelica pubescens: After harvesting, remove the fibrous roots and mud, dry until semi-dry, pile for 2-3 days, soften, and then dry until completely dry.

[0032] Millennium Health Plant: After harvesting, wash it clean, remove the outer skin, and dry it in the sun.

[0033] Myrrh: Take clean myrrh and stir-fry it according to the vinegar-roasting method until the surface is shiny.

[0034] Catechu: Harvest branches and trunks, remove the outer skin, chop into large pieces, boil with water, concentrate, and dry.

[0035] Borneol: It is a colorless, transparent or white, semi-transparent, brittle crystalline flake. It is used directly as a medicinal herb without any special processing.

[0036] Frankincense: Take clean frankincense and stir-fry it according to the vinegar-roasting method until the surface is shiny.

[0037] Eucommia: Peel off the bark, scrape off the rough outer bark, pile it up to "sweat" until the inner bark turns purplish-brown, and then dry it in the sun.

[0038] Ground beetle: After being captured, it is scalded to death in boiling water and then dried in the sun or oven.

[0039] Peach kernels: Harvest the fruit, remove the pulp and shell, extract the seeds, and dry them in the sun.

[0040] Earthworms: After capture, promptly cut open their abdomens, remove the internal organs and mud, wash them clean, and sun-dry or dry them at low temperature.

[0041] Angelica dahurica: After harvesting, remove the fibrous roots and mud, and then sun-dry or dry at low temperature.

[0042] Rhubarb: Remove impurities, wash, soak thoroughly, cut into thick slices, and air dry.

[0043] Dipsacus: After harvesting, remove the root head and fibrous roots, dry them over a low fire until half-dry, pile them up to "sweat" until the inside turns green, and then dry them completely.

[0044] Dried tangerine peel: Harvest ripe fruit, peel off the peel, and sun-dry or dry at low temperature.

[0045] Licorice: After harvesting, remove the fibrous roots and dry in the sun.

[0046] Ginger-processed Pinellia: Take clean Pinellia, separate the large and small ones, soak in water until there is no dry core inside, then take it out; separately take sliced ​​ginger and decoct it in water, add alum and cook together with Pinellia until thoroughly cooked, take it out, and air dry, or air dry until half dry, or dry; or cut into thin slices and dry.

[0047] Calcined natural copper: Take clean natural copper, calcine it until it turns dark red according to the calcination and quenching method, and then quench it in vinegar until the surface turns blackish-brown, the luster disappears and it becomes brittle.

[0048] Bupleurum chinense: After harvesting, remove the stems, leaves, and mud, and then dry.

[0049] Hot-fried Drynaria fortunei: Take clean Drynaria fortunei or slices, and fry it in sand until it puffs up, then remove the hairs.

[0050] Ground maple bark: The bark is peeled off and dried in the sun or at low temperature.

[0051] Trichosanthes kirilowii: After harvesting, wash clean, remove the outer skin, cut into sections or longitudinally split into petals, and dry.

[0052] Cinnamon twigs: Harvest tender twigs, remove leaves, and sun-dry, or slice and sun-dry.

[0053] Dioscorea opposita: After harvesting, remove the fibrous roots, wash, slice, and sun-dry.

[0054] Notopterygium root: After harvesting, remove the fibrous roots and mud, and then dry it in the sun.

[0055] Dragon's Blood: Remove impurities and crush into small pieces or grind into a fine powder.

[0056] All of the above-mentioned Chinese medicinal herbs were added in the form of medicinal slices without any special treatment.

[0057] IV. Preparation Process Example: Preparation of Guihong Xugu Shubi Paste at the preferred dosage According to the preferred weight ratio, take 10g of Angelica sinensis, 19g of Carthamus tinctorius, 10g of Angelica pubescens, 10g of Homalomena occulta, 10g of Commiphora myrrha, 4g of Catechu, 6g of Borneol, 10g of Frankincense, 12g of Eucommia ulmoides, 10g of Eupolyphaga sinensis, 4g of Prunus persica, 10g of Pheretima aspergillum, 10g of Angelica dahurica, 19g of Rheum palmatum, 10g of Dipsacus asper, 10g of Citrus reticulata peel, 10g of Glycyrrhiza uralensis, 8g of Pinellia ternata, 8g of Calcined Natural Copper, 6g of Bupleurum chinense, 10g of Drynaria fortunei, 10g of Acer palmatum bark, 10g of Trichosanthes kirilowii root, 10g of Cinnamomum cassia, 10g of Dioscorea hypoglauca, 4g of Notopterygium incisum, and 6g of Dragon's Blood, totaling twenty-seven kinds of Chinese medicinal herbs. Prepare according to the following steps: Step 1: Drying the medicinal slices All twenty-seven kinds of Chinese medicinal herbs were placed in a drying device and dried at 60±2℃. The purpose of drying is to remove excess moisture from the herbs, reducing their moisture content to a suitable range for pulverization, while also increasing their brittleness, which is beneficial for subsequent pulverization processes.

[0058] Step 2: Mixing and grinding After drying, all the Chinese herbal medicine slices are mixed and then fed into a single grinder for pulverization. During the pulverization process, the following precautions should be taken: the prescription contains viscous resinous herbs such as frankincense and myrrh, volatile components such as borneol, fibrous herbs such as safflower, and horny herbs such as earthworm. By using a mixed pulverization method, the powder generated during the pulverization process of other powdery herbs in the prescription (such as trichosanthes root, rhubarb, and dipsacus root) can effectively overcome the technical challenge of frankincense and myrrh easily adhering to the inner wall of the grinder when pulverized alone, due to the adsorption and encapsulation effect of the viscous resins and the dispersing and grinding effect of the fibrous and horny herbs. Simultaneously, the mechanical heat generated during pulverization will raise the machine temperature, potentially causing the loss of volatile components (such as borneol). Therefore, intermittent pulverization or cooling before pulverization should be adopted to control the material temperature.

[0059] To verify the feasibility and stability of this mixed pulverizing process, three batches of pulverizing tests were conducted according to the above-mentioned formulation ratios. The results are shown in the table below:

[0060] The results show that by using mixed grinding combined with temperature control, the powder yield can be kept stable at over 94%, and the grinding effect is good.

[0061] Step 3: Sieve and mix Pass the fine powder obtained in step two through a 100-mesh sieve, take the sieved powder, put it into a mixer and mix it thoroughly to obtain the fine powder of medicinal materials, which can be set aside for later use.

[0062] Step 4: Honey Refining Take an appropriate amount of honey, add about 20% purified water by weight, and heat to refine until it reaches a medium consistency. The degree of refinement can be judged by observing phenomena such as "dropping water into beads," or by dropping refined honey into cold water; if it forms beads that do not disperse, it is at the desired consistency.

[0063] Step 5: Mix and prepare the paste Mix the fine powder of medicinal materials obtained in step three with the medium honey obtained in step four at a weight ratio of 1:2.9 (i.e., fine powder of medicinal materials: medium honey = 1:2.9), and stir thoroughly to obtain Guihong Xugu Shubi Paste.

[0064] The formulation was determined based on the following screening experiment: 100g of finely powdered medicinal materials were added to different amounts of refined honey, stirred evenly, and the state of the resulting paste was observed. The results are shown in the table below:

[0065] Experimental results show that when the ratio of honey to fine medicinal powder is 2.9:1, the resulting paste has moderate consistency, good fluidity, and is easy to apply evenly to the affected area, resulting in the best physical properties of the preparation.

[0066] Step Six: Packaging The prepared Guihong Xugu Shubi Paste was packaged according to specifications. Polypropylene boxes were used as packaging materials. This material has the advantages of being durable, having good sealing performance, being moisture-proof, and hygienic, and can be used directly for pharmaceutical packaging without the need for pretreatment steps such as washing and drying.

[0067] There are two packaging options: Specification 1: 20g per box (equivalent to 5.1g of medicinal slices); Specification 2: 500g per box (equivalent to 128g of medicinal slices).

[0068] V. Formulation and Production Validation To verify the feasibility and reproducibility of the preparation process of this invention, three batches of pilot-scale production tests were conducted for two specifications according to the above-mentioned process formula and parameters, with batch numbers 20250101, 20250102, and 20250103, respectively. The preparation and production data of the three batches are shown in the table below:

[0069] As can be seen from the data in the table above, the pulverization yield of the three batches of experiments was consistently above 95%, and the finished product rate was above 94%. The data differences between batches were small and the reproducibility was good. All three batches of samples were tested according to the internal control quality standards, and the results all met the requirements. This indicates that the process route design of the present invention is reasonable, the quality of intermediates is controllable, and it is suitable for large-scale mass production.

[0070] VI. Quality Standards The Guihong Xugu Shubi Paste prepared according to the present invention was tested according to the internal control quality standards, and the main quality indicators are as follows: (a) Characteristics This product is a thick paste, ranging from brown to dark brown, with a fragrant aroma.

[0071] (ii) Identification This invention establishes a thin-layer chromatography identification system covering multiple medicinal materials in a prescription, capable of specific identification of at least twelve medicinal materials, ensuring accurate ingredient dosage and controllable product quality. (1) Microscopic identification of Eucommia ulmoides and Cinnamomum cassia: Take an appropriate amount of this product, place it in a centrifuge tube, add 25 ml of warm water (40-50℃), shake to dissolve and suspend the drug, dissolve it in honey, centrifuge for 3-5 min (4000 r / min), discard the supernatant, add 20 ml of warm water to the precipitate, repeat the above operation 3-4 times until the supernatant is basically colorless, evaporate the precipitate, and take the precipitate powder for observation under a microscope: rubber filaments are strip-shaped or twisted into clumps, and the surface is granular (Eucommia ulmoides). Cork cells are yellowish-brown, polygonal in surface view, and contain reddish-brown substances (Cinnamomum cassia). Body wall fragments are dark brown or yellow, with irregular textures on the surface, and short, thick or thin bristles are attached to them. Circular hair nests after the bristles fall off are often visible (Eupolyphaga sinensis).

[0072] (2) Identification of Angelica sinensis: Using ligustilide as a reference, the test solution was extracted with 1% sodium bicarbonate solution, acidified, and extracted with ether. The chromatogram was then examined under ultraviolet light (365 nm) using a silica gel G thin-layer plate with n-hexane-ethyl acetate (9:1) as the developing solvent. In the chromatogram of the test sample, fluorescent spots of the same color appeared at the corresponding positions as in the chromatogram of the reference sample.

[0073] (3) Identification of safflower: Using safflower reference material as a reference, the test sample solution was extracted with 80% acetone solution and then processed using silica gel H thin-layer plate with ethyl acetate-formic acid-water-methanol (7:2:3:0.4) as the developing solvent. In the chromatogram of the test sample, spots of the same color appeared at the corresponding positions as in the chromatogram of the reference material.

[0074] (4) Identification of Angelica pubescens: Using dihydroaperitol angelica ester as a reference, the test solution was extracted with petroleum ether and examined under ultraviolet light (365 nm) using a silica gel G thin-layer plate with petroleum ether (60-90℃)-ethyl acetate (7:3) as the developing solvent. In the chromatogram of the test sample, fluorescent spots of the same color appeared at the corresponding positions as in the chromatogram of the reference standard.

[0075] (5) Identification of Dipsacus asperoides: Using Dipsacus asperoides saponin VI as a reference, the test sample solution was extracted with water-saturated n-butanol, washed with ammonia solution and then with n-butanol-saturated water. A silica gel G thin-layer plate was used, with the upper layer of n-butanol-glacial acetic acid-water (4:1:5) as the developing solvent, and 10% sulfuric acid ethanol solution was sprayed for color development. In the chromatogram of the test sample, spots of the same color appeared at the corresponding positions as in the chromatogram of the reference standard.

[0076] (6) Identification of borneol: Using borneol reference standard as a reference, the test solution was extracted by water reflux and ethyl acetate extraction. A silica gel G thin-layer plate was used with cyclohexane-ethyl acetate (17:3) as the developing solvent, sprayed with 5% vanillin-sulfuric acid solution, and heated to 105℃ until the spots were clearly visible. In the chromatogram of the test sample, spots of the same color appeared at the corresponding positions as in the chromatogram of the reference standard.

[0077] (7) Identification of frankincense: Using frankincense as a reference material, the test sample solution was extracted with methanol by ultrasonication. A silica gel G thin-layer plate was then used with cyclohexane-ethyl acetate (11:1) as the developing solvent, sprayed with 5% vanillin-sulfuric acid solution, and heated to 105℃ until the spots were clearly visible. In the chromatogram of the test sample, spots of the same color appeared at the corresponding positions as in the chromatogram of the reference material.

[0078] (8) Identification of rhubarb: Using rhein reference standard as a reference, the test solution was hydrolyzed by heating and reflux with hydrochloric acid and extracted with ether. The solution was then examined under ultraviolet light (365 nm) using a silica gel G thin-layer plate with n-hexane-ethyl acetate-formic acid (6:2:0.1) as the developing solvent. In the chromatogram of the test sample, orange-yellow fluorescent spots appeared at the same positions as those in the chromatogram of the reference standard; after being exposed to ammonia vapor, the spots turned red.

[0079] (9) Identification of dried tangerine peel: Using hesperidin reference standard as a reference, the test solution was defatted with ether and extracted with acetone. A polyamide thin-layer chromatography plate was then used with chloroform-acetone-methanol (5:5:1) as the developing solvent at a distance of 12 cm. The plate was sprayed with aluminum chloride test solution, heated at 105℃ for several minutes, and examined under ultraviolet light (365 nm). In the chromatogram of the test sample, fluorescent spots of the same color appeared at the corresponding positions as in the chromatogram of the reference standard.

[0080] (10) Identification of licorice: Using glycyrrhizin reference standard as a reference, the test sample solution was defatted with ether, extracted with methanol, and extracted with n-butanol. A silica gel G thin-layer plate prepared with 1% sodium hydroxide solution was used, with ethyl acetate-formic acid-glacial acetic acid-water (15:1:1:2) as the developing solvent. The plate was sprayed with 10% sulfuric acid ethanol solution and heated to 105℃ until the spots were clearly visible. The plate was then examined under ultraviolet light (365nm). In the chromatogram of the test sample, fluorescent spots of the same color appeared at the corresponding positions as in the chromatogram of the reference standard.

[0081] (11) Identification of Drynaria fortunei: Using naringin as a reference, the test solution was extracted with methanol and then with water-saturated n-butanol. A polyamide membrane was used with chloroform-acetone-methanol (5:1:1) as the developing solvent at a distance of 15 cm. Aluminum chloride solution was sprayed on the membrane, and the sample was examined under ultraviolet light (365 nm). In the chromatogram of the test sample, fluorescent spots of the same color appeared at the corresponding positions as in the chromatogram of the reference standard.

[0082] (12) Identification of Notopterygium incisum: Using isoimperatorin as a reference, the test solution was extracted with anhydrous ethanol by ultrasonication and then analyzed using silica gel GF. 254 Thin-layer plates were developed using toluene-ethyl acetate (9:1) and examined under ultraviolet light (254 nm). The test sample chromatogram showed spots of the same color at the corresponding positions as the reference sample chromatogram.

[0083] (III) Inspection It should comply with all relevant provisions under the paste section of the Chinese Pharmacopoeia.

[0084] (4) Leaching matter The extract content shall be determined by cold maceration method under the alcohol-soluble extract determination method (General Chapter 2201, Part IV of the Chinese Pharmacopoeia), using anhydrous ethanol as solvent, and shall not be less than 29.6%.

[0085] VII. Functions, Indications and Applications The Guihong Xugu Shubi Paste of this invention has the effects of promoting blood circulation and removing blood stasis, promoting tendon and bone healing, reducing swelling and relieving pain. It is used for tendon and bone injuries, rheumatic pain, and traumatic injuries caused by wind-cold-dampness and blood stasis obstructing the meridians. It is suitable for external treatment of soft tissue contusions, fractures, arthritis, cervical spondylosis, lumbar disc herniation, etc., with the above symptoms.

[0086] VIII. Usage and Dosage For external use only. Apply this product evenly to the affected area and change it every 48 hours. One box is used per application.

[0087] IX. Storage Conditions Store in a sealed container.

[0088] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all such modifications or substitutions should be covered within the scope of the claims of the present invention.

Claims

1. A preparation process for Guihong Xugu Shubi Paste, characterized in that, The raw materials of the Guihong Xugu Shubi Paste include the following Chinese medicinal herbs: Angelica sinensis, safflower, Angelica pubescens, Homalomena occulta, myrrh, catechu, borneol, frankincense, Eucommia ulmoides, Eupolyphaga sinensis, peach kernel, earthworm, Angelica dahurica, rhubarb, Dipsacus asper, tangerine peel, licorice, ginger-processed Pinellia ternata, calcined natural copper, Bupleurum chinense, Drynaria fortunei, Acer palmatum bark, Trichosanthes kirilowii root, cinnamon twig, Dioscorea hypoglauca, Notopterygium incisum, and dragon's blood. The preparation process includes the following steps: Step 1: Drying the medicinal slices: Dry all the medicinal slices described above at 60±2℃; Step 2: Mixing and grinding: Mix all the dried Chinese herbal medicine pieces together and grind them to obtain fine powder; Step 3: Sieving and mixing: Pass the fine powder through a 100-mesh sieve, collect the sieved powder and mix it evenly to obtain the medicinal material fine powder; Step 4: Refining the honey: Take honey, add 20% water by weight, and heat to refine it into medium-quality honey; Step 5: Mixing and preparing paste: Mix the fine powder of the medicinal materials with the honey at a weight ratio of 1:2.9 and stir evenly to obtain Guihong Xugu Shubi Paste.

2. The preparation process of the Guihong Xugu Shubi Paste according to claim 1, characterized in that: In step two, the mixed pulverization involves putting all the dried Chinese herbal medicine pieces into the same pulverizer for joint pulverization. The pulverization is completed by utilizing the dispersion and adsorption effects of the powdery medicinal materials in the Chinese herbal medicine pieces on volatile medicinal materials, viscous resinous medicinal materials, fibrous medicinal materials, and keratinous medicinal materials. Cooling measures are taken during the pulverization process to control the temperature of the materials.

3. The preparation process of Guihong Xugu Shubi Paste according to claim 2, characterized in that: The relative weight parts of each Chinese herbal medicine slice in the raw materials are as follows: Angelica sinensis 7-14 parts, Carthamus tinctorius 15-25 parts, Angelica pubescens 4-15 parts, Homalomena occulta 5-15 parts, Commiphora myrrha 5-15 parts, Catechu 2-7 parts, Borneol 3-9 parts, Frankincense 5-15 parts, Eucommia ulmoides 8-18 parts, Eupolyphaga sinensis 5-15 parts, Prunus persica 1-6 parts, Pheretima aspergillum 5-15 parts, Angelica dahurica 5-15 parts, Rheum palmatum 13-24 parts, Dipsacus asper 5-15 parts, Citrus reticulata 5-15 parts, Glycyrrhiza uralensis 5-15 parts, Pinellia ternata 4-12 parts, Calcined natural copper 5-14 parts, Bupleurum chinense 2-9 parts, Drynaria fortunei 5-15 parts, Acer palmatum 5-15 parts, Trichosanthes kirilowii 5-15 parts, Cinnamomum cassia 5-15 parts, Dioscorea hypoglauca 5-15 parts, Notopterygium incisum 1-8 parts, and Dragon's blood 2-12 parts.

4. The preparation process of Guihong Xugu Shubi Paste according to claim 1, characterized in that: Among the Chinese medicinal herbs mentioned, frankincense and myrrh are processed by stir-frying with vinegar until the surface is shiny; calcined natural copper is processed by calcining and quenching until it is dark red and then quenched with vinegar until the surface is blackish-brown and the luster disappears; ginger-processed Pinellia is processed by decocting sliced ​​ginger, adding alum and cooking Pinellia together until thoroughly cooked; and scalded Drynaria fortunei is processed by scalding with sand until it bulges and then removing the hairs.

5. The preparation process of the Guihong Xugu Shubi Paste according to claim 1, characterized in that: The Guihong Xugu Shubi Paste is packaged in boxes of 20g or 500g each, using polypropylene boxes.

6. A kind of Guihong Xugu Shubi Paste, characterized in that, The Guihong Xugu Shubi Paste is prepared using the formulation process described in any one of claims 1 to 5.

7. The Guihong Xugu Shubi Paste according to claim 6, characterized in that: The Guihong Xugu Shubi Paste has at least one of the following quality test items: Microscopic identification based on the rubbery fibers in Eucommia ulmoides as a microscopic identification feature; Thin-layer chromatography identification of Angelica sinensis using ligustilide as a reference; Thin-layer chromatographic identification of safflower using safflower reference material as a reference; Thin-layer chromatographic identification of Angelica pubescens using dihydroaperitol angelica ester as a reference; Thin-layer chromatography identification of Dipsacus asperoides using Dipsacus saponin VI as a reference; Thin-layer chromatographic identification of borneol using borneol reference standard; Thin-layer chromatographic identification of frankincense using frankincense reference material as a reference; Thin-layer chromatographic identification of rhubarb using emodin as a reference; Thin-layer chromatographic identification of dried tangerine peel with hesperidin as a reference; Thin-layer chromatographic identification of licorice with glycyrrhizin as a reference; Thin-layer chromatographic identification of Drynaria fortunei with naringin as a control; Thin-layer chromatographic identification of Notopterygium incisum with isoimperatorin as a reference.

8. The Guihong Xugu Shubi Paste according to claim 7, characterized in that: The alcohol-soluble extract content of the Guihong Xugu Shubi Paste, determined by cold soaking with anhydrous ethanol as solvent, shall not be less than 29.6%.

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