Extraction process and application of traditional Chinese medicinal material volatile oil

Abstract

The extraction process comprises the following steps: according to a raw material formula of eight-ingredient dysmenorrhea capsules, taking Chinese angelica, radix aucklandiae, 1 / 2 mass of moutan bark and 1 / 2 mass of cassia twig, crushing, carrying out enzymolysis pretreatment, then extracting volatile oil with water vapor, and collecting the volatile oil after the extraction is completed. By optimizing the extraction process of the volatile oil of the four traditional Chinese medicinal materials and further optimizing the mixing process of the volatile oil and other medicinal material extracts, the problems of low oil yield and unstable preparation can be well solved, and the quality and stability of the eight-ingredient dysmenorrhea capsule preparation are comprehensively improved.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of traditional Chinese medicine, and particularly relates to an extraction process of volatile oil of traditional Chinese medicinal materials and application thereof. BACKGROUND

[0002] Eight-ingredient dysmenorrhea capsules are composed of Radix Cyathulae (stir-baked with wine), Cortex Moutan, Radix Angelicae Sinensis, Radix Paeoniae Alba (stir-baked with wine), Rhizoma Corydalis (stir-baked with vinegar), Radix Aucklandiae, Semen Persicae and Ramulus Cinnamomi, are developed from eight-ingredient dysmenorrhea tablets recorded in the Surgery and Gynecology Volume of the State Traditional Chinese Medicine Standard Compilation, and are developed through dosage form reform. The eight-ingredient dysmenorrhea capsules have the effects of activating blood, regulating menstruation, resolving stasis and relieving pain, and are used for treating dysmenorrhea, purple clots and abdominal pain during menstruation.

[0003] In the preparation process of the eight-ingredient dysmenorrhea capsules, volatile oil is first extracted from four medicinal materials, i.e., Radix Angelicae Sinensis, Radix Aucklandiae, 1 / 2 prescription amount of Cortex Moutan and 1 / 2 prescription amount of Ramulus Cinnamomi, and then the remaining medicinal materials are mixed. However, the existing preparation process does not consider the oil yield of the four medicinal materials mixed for extraction of volatile oil, and does not consider the stability of the volatile oil. In fact, the types of traditional Chinese medicinal materials, processing methods, oil extraction methods and the like can all affect the oil yield of the medicinal materials. Although the four medicinal materials are mixed for extraction of volatile oil, the efficiency is higher, but the particularity of single medicinal material is ignored, the oil yield is more unstable, the quality of the eight-ingredient dysmenorrhea capsule product is unstable, and thus the stability of the preparation curative effect is affected.

[0004] Common extraction methods of volatile oil of traditional Chinese medicinal materials include steam distillation, organic solvent extraction, CO2 supercritical fluid extraction, ultrasonic extraction and microwave extraction. The organic solvent extraction needs to use a large amount of organic solvent, which is not environmentally friendly and may have solvent residue. The CO2 supercritical fluid extraction, ultrasonic extraction and microwave extraction have higher oil yield, but have higher cost and the process is not easy to control. The traditional steam distillation method has simple and easy-to-control process, but has lower oil yield.

[0005] In addition, after the volatile oil is extracted from the four medicinal materials, the volatile oil is directly mixed with the effective component particles (dry particles formed after granulation of clear paste) extracted from the remaining medicinal materials by oil spraying, and then the capsules are prepared. The volatile oil and dry particles are mixed by oil spraying, which is easy to cause loss of volatile oil and uneven mixing, which not only affects the dispersion of the capsule content, but also affects the qualified rate of the capsule preparation loading difference, and further affects the actual production.

[0006] To sum up, how to provide an extraction process of volatile oil of traditional Chinese medicinal materials and application thereof, optimize the extraction process of volatile oil of four traditional Chinese medicinal materials, and further optimize the mixing process of volatile oil and extracts of the remaining medicinal materials, and comprehensively improve the quality and stability of the eight-ingredient dysmenorrhea capsule preparation, is a problem to be solved. SUMMARY

[0007] The technical problem to be solved by the present invention is to overcome the shortcomings of the prior art and provide an extraction process for volatile oils of Chinese medicinal materials and its application, which can better solve the problems of low oil yield and unstable preparation.

[0008] The cell wall components (cellulose, hemicellulose, pectin, etc.) of Chinese medicinal materials are important factors affecting the extraction efficiency of volatile oils. Enzymatic hydrolysis of Chinese medicinal materials can destroy their cell walls and promote the extraction of volatile oils.

[0009] In this invention, among the four medicinal materials used for the mixed extraction of volatile oils, costus lactone and dehydrocostus lactone in the costus root volatile oil are relatively stable, but the dense cell structure of costus root makes them difficult to extract. Ligusticol in the volatile oil of angelica, paeonol in peony bark, and cinnamaldehyde in cinnamon twig are all unstable, easily oxidized and decomposed, and easily escape. Therefore, targeted enzymatic hydrolysis treatment is required for different medicinal materials.

[0010] The first objective of this invention is to provide an extraction process for volatile oils from Chinese medicinal herbs, which involves targeted enzymatic hydrolysis treatment of different herbs under different conditions (compound enzyme ratio, enzyme addition amount, enzymatic hydrolysis temperature, and enzymatic hydrolysis time) to effectively improve the oil yield and batch stability of four herbs.

[0011] To achieve the first objective, the present invention adopts the following technical solution: An extraction process for volatile oils from traditional Chinese medicinal materials includes: according to the raw material formula of Bawei Tongjing Capsules, angelica, costus root, 1 / 2 mass of peony bark, and 1 / 2 mass of cinnamon twig are pulverized (65 mesh) and subjected to enzymatic pretreatment, followed by steam extraction of volatile oils, and the volatile oils are collected after extraction.

[0012] This invention reveals that the volatile oils in Angelica sinensis, Paeonia suffruticosa, and Cinnamomum cassia are easily lost during enzymatic hydrolysis (the cell walls of the herbs are easily damaged, causing the volatile oils to escape), while the loss of volatile oils in Aucklandia lappa is not significant. To reduce this loss in these three herbs, this invention enzymatically hydrolyzes the relatively stable Aucklandia lappa to a certain extent, then mixes it with the products from the slight enzymatic hydrolysis of Angelica sinensis, Paeonia suffruticosa, and Cinnamomum cassia, and then performs enzymatic hydrolysis on this mixture to investigate its effect on improving the loss of volatile oils in these three herbs.

[0013] The pretreatment before enzymatic hydrolysis includes the following steps: (1) Add water and compound enzyme 1 to the costus root, and enzymatically hydrolyze at 50-55℃ for 40-60 min to obtain product 1; the compound enzyme 1 includes cellulase and pectinase in a mass ratio of 1:(0.1-0.3); (2) Add water and compound enzyme 2 to Angelica sinensis, 1 / 2 mass of Paeonia suffruticosa root bark and 1 / 2 mass of Cinnamomum cassia twig, and enzymatically hydrolyze at 35-45℃ for 15-30 min to obtain product 2; the compound enzyme 2 includes cellulase and pectinase in a mass ratio of 1:(0.4-0.8); (3) Add product 1 to product 2 and mix well. Continue to enzymatically hydrolyze at 40-50℃ for 30-50 minutes.

[0014] Preferably, in step (1), the amount of water added is 2-4 times the mass of the costus root, the pH of the enzymatic hydrolysis system is 4-5, and the mass concentration of compound enzyme 1 in the enzymatic hydrolysis system is 1-2%.

[0015] Preferably, in step (2), the amount of water added is 5-10 times the total mass of the three raw materials: Angelica sinensis, 1 / 2 mass of Paeonia suffruticosa, and 1 / 2 mass of Cinnamomum cassia. The pH of the enzymatic hydrolysis system is 4-5, and the mass concentration of compound enzyme 2 in the enzymatic hydrolysis system is 0.8-1.5%.

[0016] The second objective of this invention is to apply the extraction process of the volatile oil from the Chinese medicinal materials to the preparation of the Eight-Ingredient Dysmenorrhea Capsule. By optimizing the mixing process of the volatile oil with the extracts of other medicinal materials, the quality and stability of the Eight-Ingredient Dysmenorrhea Capsule preparation are comprehensively improved.

[0017] To achieve the second objective, the present invention adopts the following technical solution: The application of an extraction process for the volatile oil of the aforementioned Chinese medicinal materials in the preparation of Eight-Flavor Dysmenorrhea Capsules.

[0018] The ingredients of the Eight-Ingredient Dysmenorrhea Capsules, by weight, include: 100-200 parts of Achyranthes bidentata (stir-fried with wine), 100-200 parts of Paeonia suffruticosa, 100-200 parts of Angelica sinensis, 100-200 parts of Paeonia lactiflora (stir-fried with wine), 100-200 parts of Corydalis yanhusuo (stir-fried with vinegar), 30-70 parts of Aucklandia lappa, 100-200 parts of Prunus persica, and 100-200 parts of Cinnamomum cassia.

[0019] The preparation process of the Eight-Flavor Dysmenorrhea Capsules includes: extracting volatile oil according to the process described above; collecting the volatile oil after extraction and storing the aqueous solution separately for later use; retaining the residue after extracting the volatile oil; adding four medicinal materials, namely, Achyranthes bidentata, Paeonia lactiflora, Corydalis yanhusuo, and Prunus persica; adding 8-12 times the amount of the medicinal materials to decoct twice, each time for 2 hours; combining the decoction with the aqueous solution after extracting the volatile oil; filtering (150 mesh); concentrating the filtrate to a relative density of 1.15-1.20 (60℃) to obtain a clear extract; sterilizing and pulverizing the remaining 1 / 2 mass of Paeonia suffruticosa bark and 1 / 2 mass of Cinnamomum cassia twigs; passing the powder through an 80-mesh sieve; mixing the fine powder with the clear extract; wet granulation; drying (60℃, moisture ≤6%); passing the powder through a 16-mesh sieve to obtain dry granules; spraying the dry granules with the above-mentioned volatile oil; sealing and storing for 24 hours; then filling the capsules; aluminum-plastic packaging; and finally, obtaining the Eight-Flavor Dysmenorrhea Capsules.

[0020] Volatile oil is a relatively unstable substance, and the stability of different components in a mixture of volatile oils varies even more. The volatile oil obtained in this invention is extracted from a mixture of medicinal materials, and its composition is complex with many unstable factors, making it difficult to control during the spraying and mixing process. Therefore, this invention first places the dry granules and volatile oil in the same sealed container and promotes the release of unstable components in the volatile oil to be absorbed by the dry granules under conditions slightly above room temperature. After absorption, the oil is sprayed and mixed, which can better avoid the loss of unstable components of the volatile oil or affect the mixing effect during the spraying process.

[0021] Preferably, the method for mixing dry particles with volatile oil by spraying includes: S1. Place the dry granules and volatile oil in the same sealed container, control the temperature in the sealed container to 25-30℃, and weigh the dry granules periodically until the weight growth rate of the dry granules begins to be less than 0.08% (within 1 hour). S2. Take out the dry granules and volatile oil separately, keep the temperature of the dry granules 5-8℃ higher than the temperature of the volatile oil, and then spray them together.

[0022] Preferably, in step S1, the sealed container is first vented with dry inert gas to reduce the influence of air, moisture, etc. on the adsorption of volatile oils.

[0023] Preferably, in step S1, the container for holding the dry particles has a mesh, and the mesh size is no larger than the particle size of the dry particles (16 mesh), which can promote the absorption of unstable components of volatile oil by the dry particles.

[0024] Preferably, in step S1, the moisture content of the dry granules is 2-4%.

[0025] Preferably, the time required for the dry particle weight growth rate to be less than 0.08% within 1 hour is 7-8 hours.

[0026] Preferably, the parameters for oil injection mixing include: an injection rate of 2-5 L / h, a rotation speed of 50-100 rpm, maintaining the temperature of dry particles at 25-33℃, and the temperature of volatile oil at 20-25℃.

[0027] Technical effects of the present invention: 1. To improve the oil yield of volatile oil extraction from four medicinal herbs (Angelica sinensis, Aucklandia lappa, Paeonia suffruticosa, and Cinnamomum cassia), this invention involves enzymatic hydrolysis of the four herbs. This effectively disrupts the cell wall components of the herbs, promoting the extraction of volatile oils. Because the stability of the main components of the volatile oils in the four herbs differs, the volatile oils become unstable during enzymatic hydrolysis, easily affecting the batch-to-batch stability of oil yield. Therefore, this invention further separates the enzymatic hydrolysis of Aucklandia lappa (with relatively good volatile oil stability) from that of Angelica sinensis, Paeonia suffruticosa, and Cinnamomum cassia (with relatively poor volatile oil stability). This allows for targeted enzymatic hydrolysis under different conditions (compound enzyme ratio, enzyme dosage, hydrolysis temperature, and hydrolysis time) for different herbs, effectively improving the batch-to-batch stability of oil yield from the four herbs.

[0028] 2. In this invention, the product 1 obtained by enzymatically hydrolyzing relatively stable costus root to a certain extent is mixed with the product 2 obtained by slightly enzymatically hydrolyzing angelica, peony bark, and cinnamon twig. It was found that the loss of volatile oil in the three medicinal materials was significantly improved, and the oil yield was further increased.

[0029] This invention optimizes the initial enzymatic hydrolysis of Costus root, obtaining optimal conditions for its initial enzymatic hydrolysis (50-55℃ for 40-60 min). Under these conditions, cellulose, hemicellulose, pectin, and other components in Costus root are degraded to a certain extent, and the resulting oligomers can impart good stability to the mixed enzymatic hydrolysis system. This can delay the escape of unstable components to a certain extent, thus stabilizing the enzymatic hydrolysis system of Angelica sinensis, Paeonia suffruticosa, and Cinnamomum cassia before the cell walls of the herbs are destroyed by slight enzymatic hydrolysis, thereby reducing component loss.

[0030] 3. In the process of preparing the Eight-Flavor Dysmenorrhea Capsules of the present invention, when the volatile oil is mixed with the extracts of other medicinal materials (dry granules), the dry granules and volatile oil are first placed in the same sealed container so that the unstable components in the volatile oil are absorbed by the dry granules. After absorption, the oil is sprayed and mixed. This can better avoid the loss of unstable components in the volatile oil or affect the mixing effect during the oil spraying process. At the same time, it can also reduce the difference in filling amount and improve the qualification rate and stability of the preparation.

[0031] This invention monitors the weight growth rate of the dry particles in real time when the dry particles and volatile oil are placed in the same sealed container. The adsorption endpoint is determined when the weight growth rate of the dry particles reaches a certain level (below 0.08% per hour), indicating that the unstable components of the volatile oil have been basically absorbed by the dry particles. If the container is left to stand, the volatile oil in the dry particles may escape (and the adsorption-escape process will continue to repeat). Therefore, it is necessary to strictly control the adsorption endpoint.

[0032] 4. In step S1, during the absorption of unstable volatile oil components by dry particles, the moisture content of the dry particles and the temperature inside the container have a significant impact on the absorption effect. If the moisture content of the dry particles is too low, the absorption rate will be too fast, causing partial pore blockage. If the moisture content is too high, the volatile oil will be difficult to absorb into the interior of the dry particles, remaining only on the surface. If the temperature inside the container is too low, the unstable components of the volatile oil will be difficult to volatilize. If the temperature inside the container is too high, the unstable components will escape too quickly, making it difficult for them to be evenly absorbed by the dry particles and causing them to adhere to the inner wall of the container, resulting in loss. Therefore, it is necessary to reasonably control parameters such as the moisture content of the dry particles (2-4%) and the temperature inside the container (25-30℃).

[0033] During the spray mixing stage, the temperature of the volatile oil is controlled to be lower than that of the dry particles. This serves two purposes: firstly, to prevent the volatile oil from decomposing; and secondly, when the lower-temperature volatile oil comes into contact with the higher-temperature dry particles, the increased contact temperature of the volatile oil provides adsorption power. The temperature difference between the dry particles and the volatile oil also affects the spray mixing effect. If the temperature difference is too small, the volatile oil lacks sufficient adsorption power, while if the temperature difference is too large, the contact between the volatile oil and the dry particles becomes unstable, resulting in uneven adsorption. Attached Figure Description

[0034] Figure 1 This is a flowchart illustrating the preparation process of the Eight-Ingredient Dysmenorrhea Capsule of the present invention. Figure 2 This invention describes the change in the weight growth rate of dry particles over 1 hour when dry particles and volatile oil are placed in a sealed container. Detailed Implementation

[0035] The above-mentioned solution will be further described below with reference to specific embodiments; it should be understood that these embodiments are used to illustrate the basic principles, main features and advantages of the present invention, and the present invention is not limited to the scope of the following embodiments; the implementation conditions used in the embodiments can be further adjusted according to specific requirements, and the implementation conditions not specified are usually the conditions in conventional experiments.

[0036] Unless otherwise specified in the following examples, all raw materials are commercially available or prepared by conventional methods in the art.

[0037] In the following examples, the raw material formula for the batch of Bawei Dysmenorrhea Capsules is as follows: 60 kg of Achyranthes bidentata (stir-fried with wine), 60 kg of Paeonia suffruticosa, 60 kg of Angelica sinensis, 60 kg of Paeonia lactiflora (stir-fried with wine), 60 kg of Corydalis yanhusuo (stir-fried with vinegar), 20.1 kg of Aucklandia lappa, 60 kg of Prunus persica, and 60 kg of Cinnamomum cassia; 300,000 Bawei Dysmenorrhea Capsules (0.31 g / capsule) are made.

[0038] The raw material formula for the small batch of Bawei Dysmenorrhea Capsules is as follows: 60g of Achyranthes bidentata (stir-fried with wine), 60g of Paeonia suffruticosa, 60g of Angelica sinensis, 60g of Paeonia lactiflora (stir-fried with wine), 60g of Corydalis yanhusuo (stir-fried with vinegar), 20.1g of Aucklandia lappa, 60g of Prunus persica, and 60g of Cinnamomum cassia; 300 Bawei Dysmenorrhea Capsules (0.31g / capsule) are made.

[0039] The preparation process of the Eight-Flavor Dysmenorrhea Capsules is as follows: Figure 1 .

[0040] In this embodiment of the invention, the enzyme activity of cellulase is ≥10,000 U / g, and the enzyme activity of pectinase is ≥10,000 U / g. Example 1

[0041] This embodiment provides an extraction process for volatile oils from traditional Chinese medicinal materials, including: taking 60 kg of Angelica sinensis, 20.1 kg of Aucklandia lappa, 30 kg of Paeonia suffruticosa, and 30 kg of Cinnamomum cassia according to the batch raw material formula of Bawei Tongjing Capsules, pulverizing them through a 65-mesh sieve to obtain medium powder, then performing enzymatic pretreatment, and then steam extracting the volatile oil for 6 hours. After extraction, the volatile oil is collected, and the aqueous solution is stored separately for later use.

[0042] The pretreatment before enzymatic hydrolysis includes the following steps: (1) Add 3 times the mass of water to 20.1 kg of costus root, adjust the pH to 4.5, add compound enzyme 1 to make the enzyme mass concentration 1.5%, and enzymatically hydrolyze at 52℃ for 50 min to obtain product 1; compound enzyme 1 includes cellulase and pectinase in a mass ratio of 1:0.2. (2) At the same time, add 8 times the mass of water to 60 kg of Angelica sinensis, 30 kg of Paeonia suffruticosa, and 30 kg of Cinnamomum cassia, adjust the pH to 4.5, add compound enzyme 2 to make the enzyme mass concentration 1.0%, and enzymatically hydrolyze at 40℃ for 20 min to obtain product 2; compound enzyme 2 includes cellulase and pectinase in a mass ratio of 1:0.6. (3) Add product 1 to product 2 and mix well. Continue enzymatic hydrolysis at 45°C for 40 min. Example 2

[0043] The difference between this embodiment and Embodiment 1 is that the large-batch raw material formula of the Eight-Flavor Dysmenorrhea Capsules is replaced with a small-batch raw material formula for subsequent condition optimization experiments. Example 3

[0044] This embodiment applies the process from Example 1 to prepare the Eight-Flavor Dysmenorrhea Capsule, providing a method for preparing the Eight-Flavor Dysmenorrhea Capsule, with specific steps including: (a) Extraction of volatile oils Take 60 kg of Angelica sinensis, 20.1 kg of Aucklandia lappa, 30 kg of Paeonia suffruticosa, and 30 kg of Cinnamomum cassia. Grind them into a powder through a 65-mesh sieve. Then, perform enzymatic hydrolysis pretreatment and then steam extract the volatile oil for 6 hours. After extraction, collect the volatile oil and store the aqueous solution separately for later use.

[0045] The pretreatment before enzymatic hydrolysis includes the following steps: (1) Add 3 times the mass of water to 20.1 kg of costus root, adjust the pH to 4.5, add compound enzyme 1 to make the enzyme mass concentration 1.5%, and enzymatically hydrolyze at 52℃ for 50 min to obtain product 1; compound enzyme 1 includes cellulase and pectinase in a mass ratio of 1:0.2. (2) At the same time, add 8 times the mass of water to 60 kg of Angelica sinensis, 30 kg of Paeonia suffruticosa, and 30 kg of Cinnamomum cassia, adjust the pH to 4.5, add compound enzyme 2 to make the enzyme mass concentration 1.0%, and enzymatically hydrolyze at 40℃ for 20 min to obtain product 2; compound enzyme 2 includes cellulase and pectinase in a mass ratio of 1:0.6. (3) Add product 1 to product 2 and mix well. Continue enzymatic hydrolysis at 45°C for 40 min.

[0046] (II) Preparation of the ointment The residue after extracting the volatile oil was retained. Then, 60 kg each of four herbs—Sichuan Achyranthes bidentata (stir-fried with wine), Paeonia lactiflora (stir-fried with wine), Corydalis yanhusuo (stir-fried with vinegar), and Prunus persica—were added. Eight times the amount of water was added, and the mixture was decocted twice, 2 hours each time. The decoction was combined with the liquid from the volatile oil extraction and passed through a double filter equipped with a 150-mesh filter cloth or screen. The filtrate was then pumped to a double-effect concentrator (temperature: first effect 85-95℃, second effect 60-70℃; vacuum: first effect 0.04-0.06 MPa, second effect 0.06-0.06 MPa). Concentrate the paste to a relative density of 1.1-1.15 in a single-effect evaporator (temperature 60-70℃, vacuum 0.04-0.08Mpa, steam pressure ≤0.09Mpa) or a vacuum evaporator (temperature 60-70℃, vacuum 0.04-0.08Mpa, steam pressure ≤0.09Mpa), then transfer it to a scraped concentrator (temperature 60-85℃, vacuum 0.06-0.08Mpa, steam pressure ≤0.09Mpa) and concentrate it to a relative density of 1.15-1.20 (60℃). Then, transfer it to a mixing tank through a paste collector, and while still hot, pass it through an 80-mesh sieve to collect the paste and obtain a clear paste.

[0047] (III) Capsule Preparation The remaining 30 kg of peony bark and 30 kg of cinnamon twigs were sterilized and pulverized, then passed through an 80-mesh sieve to obtain fine powder. The fine powder was mixed with the clear extract, wet granulated, dried (60℃, moisture content ≤6%), and then passed through a 16-mesh sieve to obtain dry granules. The dry granules were then spray-mixed with the above-mentioned volatile oil at room temperature, with a spraying rate of 3 L / h and a rotation speed of 80 rpm. After the oil was sprayed and mixed, the mixture was sealed and left to stand for 24 hours. Then, the capsules were filled, packaged in aluminum-plastic packaging, and the outer packaging was completed to obtain the Eight-Flavor Dysmenorrhea Capsules. Example 4

[0048] This embodiment applies the process from Example 1 to prepare Eight-Flavor Dysmenorrhea Capsules, providing a method for preparing Eight-Flavor Dysmenorrhea Capsules and improving the oil spraying and mixing method. Specific steps include: (a) Extraction of volatile oils Take 60 kg of Angelica sinensis, 20.1 kg of Aucklandia lappa, 30 kg of Paeonia suffruticosa, and 30 kg of Cinnamomum cassia. Grind them into a powder through a 65-mesh sieve. Then, perform enzymatic hydrolysis pretreatment and then steam extract the volatile oil for 6 hours. After extraction, collect the volatile oil and store the aqueous solution separately for later use.

[0049] The pretreatment before enzymatic hydrolysis includes the following steps: (1) Add 3 times the mass of water to 20.1 kg of costus root, adjust the pH to 4.5, add compound enzyme 1 to make the enzyme mass concentration 1.5%, and enzymatically hydrolyze at 52℃ for 50 min to obtain product 1; compound enzyme 1 includes cellulase and pectinase in a mass ratio of 1:0.2. (2) At the same time, add 8 times the mass of water to 60 kg of Angelica sinensis, 30 kg of Paeonia suffruticosa, and 30 kg of Cinnamomum cassia, adjust the pH to 4.5, add compound enzyme 2 to make the enzyme mass concentration 1.0%, and enzymatically hydrolyze at 40℃ for 20 min to obtain product 2; compound enzyme 2 includes cellulase and pectinase in a mass ratio of 1:0.6. (3) Add product 1 to product 2 and mix well. Continue enzymatic hydrolysis at 45°C for 40 min.

[0050] (II) Preparation of the ointment The residue after extracting the volatile oil was retained. Then, 60 kg each of four herbs—Sichuan Achyranthes bidentata (stir-fried with wine), Paeonia lactiflora (stir-fried with wine), Corydalis yanhusuo (stir-fried with vinegar), and Prunus persica—were added. Eight times the amount of water was added, and the mixture was decocted twice, 2 hours each time. The decoction was combined with the liquid from the volatile oil extraction and passed through a double filter equipped with a 150-mesh filter cloth or screen. The filtrate was then pumped to a double-effect concentrator (temperature: first effect 85-95℃, second effect 60-70℃; vacuum: first effect 0.04-0.06 MPa, second effect 0.06-0.06 MPa). Concentrate the paste to a relative density of 1.1-1.15 in a single-effect evaporator (temperature 60-70℃, vacuum 0.04-0.08Mpa, steam pressure ≤0.09Mpa) or a vacuum evaporator (temperature 60-70℃, vacuum 0.04-0.08Mpa, steam pressure ≤0.09Mpa), then transfer it to a scraped concentrator (temperature 60-85℃, vacuum 0.06-0.08Mpa, steam pressure ≤0.09Mpa) and concentrate it to a relative density of 1.15-1.20 (60℃). Then, transfer it to a mixing tank through a paste collector, and while still hot, pass it through an 80-mesh sieve to collect the paste and obtain a clear paste.

[0051] (III) Capsule Preparation The remaining 30 kg of peony bark and 30 kg of cinnamon twigs were sterilized and pulverized, then passed through an 80-mesh sieve to obtain fine powder. The fine powder was mixed with the clear extract, wet granulated, dried (60℃, moisture content 3.5%), and then passed through a 16-mesh sieve to obtain dry granules. The dry granules were mixed with the above-mentioned volatile oil spray, sealed and placed for 24 hours, and then capsules were filled, aluminum-plastic packaging, and outer packaging were completed to obtain the Eight-Flavor Dysmenorrhea Capsules.

[0052] Methods for mixing dry particles with volatile oils by spraying include: S1. Place the dry granules (containing a mesh container) and volatile oil in the same sealed container (with dry inert gas exhaust). Control the temperature in the sealed container to 28°C. Weigh the dry granules periodically until the weight increase rate of the dry granules is less than 0.08% within 1 hour. S2. Take out the dry granules and volatile oil separately, and keep the temperature of the dry granules 6°C higher than that of the volatile oil. Specifically, keep the temperature of the dry granules at 30°C and the temperature of the volatile oil at 24°C. Then, perform oil spraying and mixing at an oil spraying rate of 3L / h and a rotation speed of 80rpm. Example 5

[0053] The difference between this embodiment and Embodiment 4 is that the large-batch raw material formula of the Eight-Flavor Dysmenorrhea Capsules is replaced with a small-batch raw material formula for subsequent condition optimization experiments. Example 6

[0054] This embodiment provides a method for preparing the Eight-Ingredient Dysmenorrhea Capsule, the specific steps of which include: (a) Extraction of volatile oils Take 60 kg of Angelica sinensis, 20.1 kg of Aucklandia lappa, 30 kg of Paeonia suffruticosa, and 30 kg of Cinnamomum cassia. Grind them into a powder through a 65-mesh sieve. Then, perform enzymatic hydrolysis pretreatment and then steam extract the volatile oil for 6 hours. After extraction, collect the volatile oil and store the aqueous solution separately for later use.

[0055] The pretreatment before enzymatic hydrolysis includes the following steps: (1) Add 2 times the mass of water to 20.1 kg of costus root, adjust the pH to 4, add compound enzyme 1 to make the enzyme mass concentration 1%, and enzymatically hydrolyze at 50℃ for 60 min to obtain product 1; the compound enzyme 1 includes cellulase and pectinase in a mass ratio of 1:0.1. (2) At the same time, add 5 times the mass of water to 60 kg of Angelica sinensis, 30 kg of Paeonia suffruticosa, and 30 kg of Cinnamomum cassia, adjust the pH to 4, add compound enzyme 2 to make the enzyme mass concentration 0.8%, and enzymatically hydrolyze at 35℃ for 30 min to obtain product 2; the compound enzyme 2 includes cellulase and pectinase in a mass ratio of 1:0.4. (3) Add product 1 to product 2 and mix well. Continue enzymatic hydrolysis at 40℃ for 50 min.

[0056] (II) Preparation of the ointment The steps are the same as in Example 4.

[0057] (III) Capsule Preparation The remaining 30 kg of peony bark and 30 kg of cinnamon twigs were sterilized and pulverized, then passed through an 80-mesh sieve to obtain fine powder. The fine powder was mixed with the clear extract, wet granulated, dried (60℃, moisture content 3.2%), and then passed through a 16-mesh sieve to obtain dry granules. The dry granules were mixed with the above-mentioned volatile oil spray, sealed and placed for 24 hours, and then capsules were filled, aluminum-plastic packaging, and outer packaging were completed to obtain the Eight-Flavor Dysmenorrhea Capsules.

[0058] Methods for mixing dry particles with volatile oils by spraying include: S1. Place the dry granules (containing a mesh container) and volatile oil in the same sealed container (with dry inert gas exhaust). Control the temperature in the sealed container to 25°C. Weigh the dry granules periodically until the weight increase rate of the dry granules is less than 0.08% within 1 hour. S2. Take out the dry granules and volatile oil separately, and keep the temperature of the dry granules 5°C higher than that of the volatile oil. Specifically, keep the temperature of the dry granules at 25°C and the temperature of the volatile oil at 20°C. Then, perform oil spraying and mixing at an oil spraying rate of 2L / h and a rotation speed of 50rpm. Example 7

[0059] This embodiment provides a method for preparing the Eight-Ingredient Dysmenorrhea Capsule, the specific steps of which include: (a) Extraction of volatile oils Take 60 kg of Angelica sinensis, 20.1 kg of Aucklandia lappa, 30 kg of Paeonia suffruticosa, and 30 kg of Cinnamomum cassia. Grind them into a powder through a 65-mesh sieve. Then, perform enzymatic hydrolysis pretreatment and then steam extract the volatile oil for 6 hours. After extraction, collect the volatile oil and store the aqueous solution separately for later use.

[0060] The pretreatment before enzymatic hydrolysis includes the following steps: (1) Add 4 times the mass of water to 20.1 kg of costus root, adjust the pH to 5, add compound enzyme 1 to make the enzyme mass concentration 2%, and enzymatically hydrolyze at 55℃ for 40 min to obtain product 1; the compound enzyme 1 includes cellulase and pectinase in a mass ratio of 1:0.3. (2) At the same time, add 10 times the mass of water to 60 kg of Angelica sinensis, 30 kg of Paeonia suffruticosa, and 30 kg of Cinnamomum cassia, adjust the pH to 5, add compound enzyme 2 to make the enzyme mass concentration 1.5%, and enzymatically hydrolyze at 45℃ for 15 min to obtain product 2; the compound enzyme 2 includes cellulase and pectinase in a mass ratio of 1:0.8. (3) Add product 1 to product 2 and mix well. Continue to enzymatically hydrolyze at 50°C for 30 minutes.

[0061] (II) Preparation of the ointment The steps are the same as in Example 4.

[0062] (III) Capsule Preparation The remaining 30 kg of peony bark and 30 kg of cinnamon twigs were sterilized and pulverized, then passed through an 80-mesh sieve to obtain fine powder. The fine powder was mixed with the clear extract, wet granulated, dried (60℃, moisture content 2.8%), and then passed through a 16-mesh sieve to obtain dry granules. The dry granules were mixed with the above-mentioned volatile oil spray, sealed and placed for 24 hours, and then capsules were filled, aluminum-plastic packaging, and outer packaging were completed to obtain the Eight-Flavor Dysmenorrhea Capsules.

[0063] Methods for mixing dry particles with volatile oils by spraying include: S1. Place the dry granules (in a container with mesh) and volatile oil in the same sealed container (with dry inert gas exhaust). Control the temperature in the sealed container to 30°C. Weigh the dry granules periodically until the weight increase rate of the dry granules is less than 0.08% within 1 hour. S2. Take out the dry granules and volatile oil separately, and keep the temperature of the dry granules 8°C higher than that of the volatile oil. Specifically, keep the temperature of the dry granules at 33°C and the temperature of the volatile oil at 25°C. Then, perform oil spraying and mixing at a spraying rate of 5L / h and a rotation speed of 100rpm.

[0064] I. Extraction effect of volatile oils from Chinese medicinal materials in this invention To investigate the effects of different pretreatments and hydrolysis conditions (compound enzyme ratio, enzyme dosage, hydrolysis temperature, hydrolysis time, etc.) on the extraction rate (oil yield) of volatile oil, comparative examples 1-21 were set up.

[0065] Comparative Example 1 The difference between this comparative example and Example 2 is that no pretreatment with enzymatic hydrolysis was performed.

[0066] Comparative Example 2 The difference between this comparative example and Example 2 is that Angelica sinensis, Paeonia suffruticosa, and Cinnamomum cassia are enzymatically hydrolyzed separately. The pretreatment of the four medicinal materials before enzymatic hydrolysis includes the following steps: (1) Add 3 times the mass of water to 20.1 kg of costus root, adjust the pH to 4.5, add compound enzyme 1 to make the enzyme mass concentration 1.5%, and enzymatically hydrolyze at 52℃ for 90 min to obtain product 1; compound enzyme 1 includes cellulase and pectinase in a mass ratio of 1:0.2. (2) Add 8 times the mass of water to 60 kg of Angelica sinensis, adjust the pH to 4.5, add compound enzyme 2 to make the enzyme mass concentration 1.0%, and enzymatically hydrolyze at 40℃ for 60 min to obtain product 2; compound enzyme 2 includes cellulase and pectinase in a mass ratio of 1:0.6. (3) Add 8 times the mass of water to 30 kg of peony bark, adjust the pH to 4.5, add compound enzyme 2 to make the enzyme mass concentration 1.0%, and enzymatically hydrolyze at 40℃ for 60 min to obtain product 3; (4) Add 8 times the mass of water to 30 kg of cinnamon twigs, adjust the pH to 4.5, add compound enzyme 2 to make the enzyme mass concentration 1.0%, and enzymatically hydrolyze at 40℃ for 60 min to obtain product 4; (5) Add 8 times the mass of water to 30 kg of cinnamon twigs, adjust the pH to 4.5, add compound enzyme 2 to make the enzyme mass concentration 1.0%, and enzymatically hydrolyze at 40℃ for 60 min. Mix product 1, product 2, product 3 and product 4 to obtain the mixed enzymatic hydrolysate of the four herbs.

[0067] Comparative Example 3 The difference between this comparative example and Example 2 is that step (3) is not included. The pretreatment before enzymatic hydrolysis includes the following steps: (1) Add 3 times the mass of water to 20.1 kg of costus root, adjust the pH to 4.5, add compound enzyme 1 to make the enzyme mass concentration 1.5%, and enzymatically hydrolyze at 52℃ for 90 min to obtain product 1; (2) At the same time, add 8 times the mass of water to 60 kg of Angelica sinensis, 30 kg of Paeonia suffruticosa and 30 kg of Cinnamomum cassia, adjust the pH to 4.5, add compound enzyme 2 to make the enzyme mass concentration 1.0%, and enzymatically hydrolyze at 40℃ for 60 min to obtain product 2.

[0068] Comparative Example 4 The difference between this comparative example and Example 2 is that the enzyme concentration of complex enzyme 1 in step (1) is 0.5%.

[0069] Comparative Example 5 The difference between this comparative example and Example 2 is that the enzyme concentration of complex enzyme 1 in step (1) is 2.5%.

[0070] Comparative Example 6 The difference between this comparative example and Example 2 is that the enzymatic hydrolysis temperature in step (1) is 45°C.

[0071] Comparative Example 7 The difference between this comparative example and Example 2 is that the enzymatic hydrolysis temperature in step (1) is 60°C.

[0072] Comparative Example 8 The difference between this comparative example and Example 2 is that the enzymatic hydrolysis time in step (1) is 30 min.

[0073] Comparative Example 9 The difference between this comparative example and Example 2 is that the enzymatic hydrolysis time in step (1) is 70 min.

[0074] Comparative Example 10 The difference between this comparative example and Example 2 is that in step (1), the complex enzyme 1 includes cellulase and pectinase in a mass ratio of 1:0.05.

[0075] Comparative Example 11 The difference between this comparative example and Example 2 is that in step (1), the complex enzyme 1 includes cellulase and pectinase in a mass ratio of 1:0.4.

[0076] Comparative Example 12 The difference between this comparative example and Example 2 is that the enzyme concentration of complex enzyme 2 in step (2) is 0.5%.

[0077] Comparative Example 13 The difference between this comparative example and Example 2 is that the enzyme concentration of complex enzyme 2 in step (2) is 2.0%.

[0078] Comparative Example 14 The difference between this comparative example and Example 2 is that the enzymatic hydrolysis temperature in step (2) is 30°C.

[0079] Comparative Example 15 The difference between this comparative example and Example 2 is that the enzymatic hydrolysis temperature in step (2) is 50°C.

[0080] Comparative Example 16 The difference between this comparative example and Example 2 is that in step (2), the complex enzyme 2 includes cellulase and pectinase in a mass ratio of 1:0.3.

[0081] Comparative Example 17 The difference between this comparative example and Example 2 is that in step (2), the complex enzyme 2 includes cellulase and pectinase with a mass ratio of 1:9.

[0082] Comparative Example 18 The difference between this comparative example and Example 2 is that in step (2), the enzymolysis time is 10 min.

[0083] Comparative Example 19 The difference between this comparative example and Example 2 is that in step (2), the enzymolysis time is 40 min.

[0084] Comparative Example 20 The difference between this comparative example and Example 2 is that in step (3), the enzymolysis time is 20 min.

[0085] Comparative Example 21 The difference between this comparative example and Example 2 is that in step (3), the enzymolysis time is 60 min.

[0086] 1. Oil yield The four traditional Chinese medicine materials of Angelica sinensis, Aucklandia lappa, Cortex Moutan, and Ramulus Cinnamomi were subjected to enzymolysis pretreatment and volatile oil extraction according to the methods of Examples 1 - 2 and Comparative Examples 1 - 21. The volatile oil was collected, and the oil yield was calculated. The results are shown in Table 1. Among them, the oil yield % = 100% × volume of the collected volatile oil (in ml) / mass of the charged materials (in g).

[0087] Table 1

[0088] As can be seen from Table 1, compared with Comparative Examples 1 - 21, in Examples 1 - 2 of the present invention, after the four traditional Chinese medicine materials of Angelica sinensis, Aucklandia lappa, Cortex Moutan, and Ramulus Cinnamomi were subjected to enzymolysis pretreatment and then volatile oil extraction, by optimizing process parameters such as the ratio of the complex enzyme, enzyme addition amount, enzymolysis temperature, and enzymolysis time in the enzymolysis process, the oil yield can be effectively increased.

[0089] Comparing Example 2 with Comparative Example 1, it can be seen that in the present invention, after the four traditional Chinese medicine materials are subjected to enzymolysis pretreatment and then volatile oil extraction, the extraction efficiency of the volatile oil can be promoted. Comparing Example 2 with Comparative Example 2, it can be seen that in the present invention, the Aucklandia lappa medicinal material with better volatile oil stability is enzymolyzed separately from the Angelica sinensis, Cortex Moutan, and Ramulus Cinnamomi medicinal materials with poorer volatile oil stability, which can perform targeted enzymolysis treatment on different medicinal materials and effectively increase the oil yield. Comparing Example 2 with Comparative Example 3, it can be seen that in the present invention, the product 1 obtained by enzymolyzing the relatively stable Aucklandia lappa medicinal material to a certain extent is mixed with the product 2 obtained by slightly enzymolyzing the three medicinal materials of Angelica sinensis, Cortex Moutan, and Ramulus Cinnamomi for enzymolysis, and the oil yield is further improved.

[0090] Comparison of Comparative Examples 4-11 and 12-21 shows that the degree of enzymatic hydrolysis of Costus root has a significant impact on the oil yield. The enzymatic hydrolysis conditions of Costus root need to be controlled within the range of this invention in order to achieve the specific effect.

[0091] 2. Batch stability of oil yield Following the methods of Example 2 and Comparative Examples 2-3, the four medicinal materials Angelica sinensis, Aucklandia lappa, Paeonia suffruticosa, and Cinnamomum cassia were subjected to enzymatic pretreatment and volatile oil extraction. Ten batches were set up simultaneously for each example or comparative example. The relative standard deviation (RSD) of the oil yield of Example 2 and Comparative Examples 1-3 was used to characterize the batch stability. The results are shown in Table 2.

[0092] Table 2

[0093] As shown in Table 2, compared with Comparative Examples 2-3, the targeted enzymatic hydrolysis of the four medicinal materials in Example 2 of the present invention can effectively improve the batch stability of the oil yield.

[0094] II. Basic Quality Testing of the Eight-Ingredient Dysmenorrhea Capsules Prepared by This Invention The quality of the eight-ingredient dysmenorrhea capsules prepared in Examples 3-7 of this invention was tested in accordance with standard YBZ00252010, and the results are shown in Table 3.

[0095] Table 3

[0096] As shown in Table 3, the eight-ingredient dysmenorrhea capsules prepared in Examples 3-7 of this invention all meet the relevant provisions of standard YBZ00252010.

[0097] III. Optimization of the oil spraying method in the preparation process of Eight-Flavor Dysmenorrhea Capsules 1. Endpoint determination of adsorption of unstable components of volatile oil by dry particles Eight-ingredient dysmenorrhea capsules were prepared according to the method in Example 5. In the oil spraying and mixing process step S1, the real-time weight (m³) of the dry granules was monitored every 1 hour. t ), calculate the dry particle weight growth rate within 1 hour, dry particle weight growth rate (within 1 hour, %) = 100% × (m t - m t-1 ) / m0,m t-1 The weight of dry particles 1 hour before time t.

[0098] The study examined changes in the growth rate, and the results are shown in Table 4 and... Figure 2It can be seen that when dry particles and volatile oil are placed in a sealed container, the dry particles gradually adsorb unstable components in the volatile oil over time, and the adsorption is basically complete after 7-8 hours. At this time, the weight growth rate of dry particles (within 1 hour, %) is 0.0281%. Before 7-8 hours, the weight growth rate of dry particles (within 1 hour, %) is higher than 0.08%, and after 8 hours, the weight growth rate of dry particles decreases or even becomes negative, indicating that the endpoint criterion of the dry particle weight growth rate being lower than 0.08% for the first time within 1 hour is reasonable.

[0099] Table 4

[0100] 2. The effect of oil spraying and mixing process on the quality of Bawei Dysmenorrhea Capsules To investigate the effect of the spray mixing step of the present invention with the extracts (dry granules) of other medicinal materials on the quality of the Eight-Flavor Dysmenorrhea Capsules, comparative examples 22-30 were set up respectively.

[0101] Comparative Example 22 The difference between this comparative example and Example 5 is that, in step S1, the moisture content of the dry particles is 1%.

[0102] Comparative Example 23 The difference between this comparative example and Example 5 is that, in step S1, the moisture content of the dry particles is 5%.

[0103] Comparative Example 24 The difference between this comparative example and Example 5 is that the temperature in the sealed container in step S1 is 20°C.

[0104] Comparative Example 25 The difference between this comparative example and Example 5 is that, in step S1, the temperature in the sealed container is 35°C.

[0105] Comparative Example 26 The difference between this comparative example and Example 5 is that in step S1, the dry particles and volatile oil are placed in the same sealed container until the weight growth rate of the dry particles is less than 0.10% within 1 hour.

[0106] Comparative Example 27 The difference between this comparative example and Example 5 is that in step S1, the dry particles and volatile oil are placed in the same sealed container until the weight growth rate of the dry particles is less than 0.03% within 1 hour.

[0107] Comparative Example 28 The difference between this comparative example and Example 5 is that in step S2, the temperature of the dry particles is maintained at 35°C and the temperature of the volatile oil is maintained at 25°C.

[0108] Comparative Example 29 The difference between this comparative example and Example 5 is that, in step S2, the temperature of the dry particles is maintained at 25°C and the temperature of the volatile oil is maintained at 25°C.

[0109] Comparative Example 30 The difference between this comparative example and Example 5 is that in step S2, the temperature of the dry particles is maintained at 20°C and the temperature of the volatile oil is maintained at 25°C.

[0110] (1) Loss of volatile oils in the oil spraying and mixing process Eight-ingredient dysmenorrhea capsules were prepared according to the methods of Examples 3-7 and Comparative Examples 22-30, respectively. The loss of volatile oil was measured. The volatile oil loss rate (%) was calculated as follows: 100% × (total mass of dry particles and volatile oil before oil spraying and mixing - total mass of particles after oil spraying and mixing) / total mass of dry particles and volatile oil before oil spraying and mixing. The results are shown in Table 5.

[0111] Table 5

[0112] As shown in Table 5, compared with Example 3, the improved method of spray mixing of volatile oil and dry particles in Examples 4-7 of the present invention can effectively reduce the loss rate of volatile oil and improve the quality and stability of the formulation. Comparative Examples 22-30 changed the spray mixing steps, resulting in increased loss of volatile oil.

[0113] In the oil spraying and mixing step, dry particles and volatile oil are placed in the same sealed container, allowing the dry particles to adsorb unstable components of the volatile oil. Comparing Example 5 and Comparative Examples 22-27, it is evident that the moisture content of the dry particles and the temperature inside the container have a significant impact on the volatile oil loss rate. Comparing Example 5 and Comparative Examples 28-30, it is evident that the temperature difference between the dry particles and the volatile oil during the oil spraying and mixing stage also significantly affects the volatile oil loss rate.

[0114] 3. The pass rate of multiple batches of the "Eight-Ingredient Dysmenorrhea Capsules" filler content variation test. Eight-ingredient dysmenorrhea capsules were prepared according to the methods of Examples 3-7 and Comparative Examples 22-30, respectively. Twenty batches were prepared for each example or comparative example. The pass rate (%) of the multiple batches for the content difference test was calculated as 100% × number of qualified batches / 20. The results are shown in Table 6.

[0115] Table 6

[0116] As shown in Table 6, compared with Example 3, the improved method of spray mixing of volatile oil and dry granules in Examples 4-7 of the present invention can effectively reduce the content difference of capsules and improve the qualification rate and stability of the formulation. Comparative Examples 22-30 changed the spray mixing steps, resulting in increased content difference of capsules and worsened qualification rate and stability of the formulation.

[0117] Finally, it should be noted that the above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A process for extracting volatile oils from traditional Chinese medicinal materials, characterized in that: According to the raw material formula of the Eight-Flavor Dysmenorrhea Capsules, Angelica sinensis, Aucklandia lappa, 1 / 2 mass of Paeonia suffruticosa bark, and 1 / 2 mass of Cinnamomum cassia twig are pulverized and subjected to enzymatic pretreatment, and then the volatile oil is extracted by steam extraction. After extraction, the volatile oil is collected. The pretreatment before enzymatic hydrolysis includes the following steps: (1) Add water and compound enzyme 1 to the costus root, and enzymatically hydrolyze at 50-55℃ for 40-60 min to obtain product 1; the compound enzyme 1 includes cellulase and pectinase in a mass ratio of 1:(0.1-0.3); (2) Add water and compound enzyme 2 to Angelica sinensis, 1 / 2 mass of Paeonia suffruticosa root bark and 1 / 2 mass of Cinnamomum cassia twig, and enzymatically hydrolyze at 35-45℃ for 15-30 min to obtain product 2; the compound enzyme 2 includes cellulase and pectinase in a mass ratio of 1:(0.4-0.8); (3) Add product 1 to product 2 and mix well. Continue to enzymatically hydrolyze at 40-50℃ for 30-50 minutes.

2. The process according to claim 1, characterized in that: In step (1), the amount of water added is 2-4 times the mass of the costus root, the pH of the enzymatic hydrolysis system is 4-5, and the mass concentration of compound enzyme 1 in the enzymatic hydrolysis system is 1-2%.

3. The process according to claim 1, characterized in that: In step (2), the amount of water added is 5-10 times the total mass of the three raw materials: Angelica sinensis, 1 / 2 mass of Paeonia suffruticosa, and 1 / 2 mass of Cinnamomum cassia. The pH of the enzymatic hydrolysis system is 4-5, and the mass concentration of compound enzyme 2 in the enzymatic hydrolysis system is 0.8-1.5%.

4. The application of the process described in claim 1 in the preparation of Eight-Flavor Dysmenorrhea Capsules.

5. The application according to claim 4, characterized in that: The ingredients of the Eight-Ingredient Dysmenorrhea Capsules, by weight, include: 100-200 parts of Achyranthes bidentata, 100-200 parts of Paeonia suffruticosa, 100-200 parts of Angelica sinensis, 100-200 parts of Paeonia lactiflora, 100-200 parts of Corydalis yanhusuo, 30-70 parts of Aucklandia lappa, 100-200 parts of Prunus persica, and 100-200 parts of Cinnamomum cassia.

6. The application according to claim 4, characterized in that: The preparation process of the Eight-Flavor Dysmenorrhea Capsules includes: extracting volatile oil according to the process described in claim 1; collecting the volatile oil after extraction; storing the aqueous solution separately for later use; retaining the residue after extracting the volatile oil; adding four medicinal materials, namely, Achyranthes bidentata, Paeonia lactiflora, Corydalis yanhusuo, and Prunus persica; decocting with water; combining the decoction with the aqueous solution after extracting the volatile oil; filtering and concentrating to obtain a clear extract; sterilizing and pulverizing the remaining 1 / 2 mass of Paeonia suffruticosa bark and 1 / 2 mass of Cinnamomum cassia twig to obtain a fine powder; mixing the fine powder with the clear extract; wet granulating; drying and granulating to obtain dry granules; mixing the dry granules with the above-mentioned volatile oil by spraying; and then filling the capsules to obtain the Eight-Flavor Dysmenorrhea Capsules.

7. The application according to claim 6, characterized in that: Methods for mixing dry particles with volatile oils by spraying include: S1. Place the dry granules and volatile oil in the same sealed container, control the temperature in the sealed container to 25-30℃, and weigh the dry granules periodically until the weight growth rate of the dry granules is less than 0.08% within 1 hour. S2. Take out the dry granules and volatile oil separately, keep the temperature of the dry granules 5-8℃ higher than the temperature of the volatile oil, and then spray them together.

8. The application according to claim 6 or 7, characterized in that: The parameters for fuel injection mixing include: fuel injection rate of 2-5L / h, rotation speed of 50-100rpm, maintaining the temperature of dry particles at 25-33℃, and the temperature of volatile oil at 20-25℃.

9. The application according to claim 7, characterized in that: In step S1, the sealed container is first vented with dry inert gas, and the container for holding the dry particles has a mesh.

10. The application according to claim 7, characterized in that: In step S1, the moisture content of the dry granules is 2-4%, and the time required for the dry granule weight growth rate to be less than 0.08% within 1 hour is 7-8 hours.

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