A preparation method of Prunella Vulgaris formula granules

Abstract

The present invention relates to the technical field of preparation of Chinese medicinal material formula granules, and specifically discloses a preparation method of Prunella vulgaris formula granules, comprising the following steps: weighing Prunella vulgaris slices, adding water to cover the slices and soaking; treating the soaked Prunella vulgaris slices to obtain a filtrate; vacuum concentrating the filtrate to obtain a clear paste; drying the clear paste to prepare a dry paste powder, adding auxiliary materials, mixing evenly, dry granulating, preparing granules and packaging, and obtaining Prunella vulgaris formula granules. The preparation process of the Prunella vulgaris formula granules of the present invention is improved, the process step parameters in the soaking process, concentration process and drying process of the Prunella vulgaris slices are adjusted, the paste yield of the Prunella vulgaris slices is improved, the content of effective ingredients in the prepared formula granules is high, the dosage is small, the finished product has high stability, is easy to preserve, and is suitable for promotion to large-scale production.

Description

Technical Field

[0001] The invention specifically relates to the technical field of preparation of Chinese medicinal material formula granules, and in particular to a method for preparing Prunella vulgaris formula granules. Background Art

[0002] Prunella vulgaris is a traditional Chinese medicine that can clear internal heat and improve eyesight, and can treat red, swollen and painful eyes, headaches, etc. It is known as the "holy medicine for clearing and protecting the liver". It grows in wetlands in mountain valleys or wet grass on both sides of rivers, wastelands, and roadsides. It is widely distributed throughout China, with Henan, Anhui, Jiangsu, Hunan and other provinces as the main production areas.

[0003] Chinese medicine formula granules are granules made from standardized processed Chinese medicine pieces under the guidance of Chinese medicine theory. They can be used for flexible clinical prescriptions and preparations, and can also be used as industrial raw materials for Chinese medicine preparations, and also provide a new way for clinical use of Chinese medicine. Compared with traditional Chinese medicine decoctions, formula granules can be directly used for prescription preparation in Chinese medicine clinics. Patients can directly take them according to the prescribed dosage. They are convenient to take, with a small dosage, controllable quality, easy to store, and easy to carry.

[0004] In the prior art preparation process of Prunella vulgaris, the paste yield of Prunella vulgaris slices is low, and the prepared formula granules not only have a low finished product rate, but also have a low content of effective ingredients. Moreover, in the prior art preparation process of Prunella vulgaris, the formula granules have a high drug loading ratio requirement, and generally the amount of auxiliary materials used shall not be higher than 50%, and the particle size requirement and moisture resistance requirement are higher. If the existing auxiliary materials are used, the prepared formula granules have poor particle size, strong powderiness, low drug loading ratio, and are easy to absorb moisture. Summary of the invention

[0005] The object of the present invention is to provide a preparation method and application of selfheal formula granules, so as to solve the problem that in the selfheal preparation process in the prior art proposed in the above background technology, the yield of selfheal decoction pieces is low, and the prepared formula granules not only have a low finished product rate, but also have a low content of effective ingredients; and, in the selfheal preparation process in the prior art, the formula granules have a high drug loading ratio requirement, and generally the amount of auxiliary materials shall not be higher than 50%, and the particle size requirement and moisture resistance requirement are higher. If the existing auxiliary materials are used, the prepared formula granules have poor particle size, strong powderiness, low drug loading ratio, and easy moisture absorption.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] A method for preparing Prunella vulgaris formula granules comprises the following steps:

[0008] S10, soaking: weigh 4500g of Prunella vulgaris slices, add water to cover the slices and soak for 15-60min;

[0009] S20, solid-liquid separation: treating the soaked Prunella Vulgaris decoction pieces to obtain a filtrate, the treating method comprising the following steps:

[0010] S21, the soaked Prunella vulgaris slices are divided into two equal parts, and the parts are added into extraction tanks A and B respectively for extraction, and the extracts from each tank are combined after the extraction is completed;

[0011] S22, centrifuging the extract at high speed using a centrifuge to obtain a centrifuged liquid, performing microfiltration separation on the centrifuged liquid to obtain a microfiltration permeate, and performing ultrafiltration separation on the microfiltration permeate using an ultrafiltration membrane to obtain a filtrate;

[0012] S30, concentration: vacuum concentrate the filtrate to a relative density of 1.08-1.13 (measured at 60° C.) to obtain a clear paste;

[0013] S40, drying the clear paste to prepare dry paste powder, adding auxiliary materials, mixing evenly, dry granulating, preparing granules of 1000 g per package, and obtaining the Prunella Vulgaris formula granules.

[0014] As a further solution of the present invention: in step S10, the reciprocal of the bulk density of the Prunella Vulgaris slices is 32, the volume of the Prunella Vulgaris slices is measured before soaking, 30-46 times of water is added to cover the slices, and the wetting percentage of the Prunella Vulgaris slices after soaking is greater than 75%.

[0015] As a further solution of the present invention: in step S20, the temperature at which the A and B extraction tanks extract the soaked Prunella Vulgaris slices is 60°C, the extraction solvent is 60% ethanol which is 6 times the weight of the Prunella Vulgaris slices, the filtrate after filtration has good thermal transmittance, and the apparent clarity percentage after cooling is greater than or equal to 80%, which effectively filters out most of the slice fragments and makes the finished product have better clarity.

[0016] As a further solution of the present invention: in step S30, the concentration temperature is set to 65°C and the vacuum degree reaches ≥-0.08mpa.

[0017] As a further solution of the present invention: in step S40, the method of drying the clear paste to prepare dry paste powder includes freeze drying and spray drying, wherein:

[0018] (1) Freeze drying: Freeze the paste for 4-6 hours and then dry it to obtain dry paste powder;

[0019] (2) Spray drying: Add 2% maltodextrin to the clear paste, mix evenly, and spray dry into dry paste powder.

[0020] As a further embodiment of the present invention: in the spray drying step, the inlet air temperature is 175-185°C, preferably 180-185°C.

[0021] As a further solution of the present invention: in step S40, the auxiliary material is one or more of corn starch, dextrin, and maltodextrin.

[0022] As a further solution of the present invention: the auxiliary material is dextrin.

[0023] As a further solution of the present invention: in step S40, the prepared particles are packaged with a composite aluminum film.

[0024] A selfheal formula granule, which is prepared according to the above preparation method.

[0025] Compared with the prior art, the beneficial effects of the present invention are as follows: the preparation process of the herbaceous prunellae formula granules of the present invention is improved, the process step parameters in the soaking process, concentration process and drying process of the herbaceous prunellae decoction pieces are adjusted, the paste yield of the herbaceous prunellae decoction pieces is improved, the prepared formula granules have a high content of effective ingredients, a small dosage, a high stability of the finished product, are easy to preserve, and are suitable for promotion to large-scale production. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 The present invention is a flow chart of the preparation method of Prunella Vulgaris formula granules. DETAILED DESCRIPTION

[0027] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0028] Unless otherwise specified, the raw materials, substrates or reagents in the following examples are all commercially available products. If appropriate, they can also be prepared by methods known in the art.

[0029] In the prior art preparation process of Prunella vulgaris, the paste yield of Prunella vulgaris slices is low, and the prepared formula granules not only have a low finished product rate, but also have a low content of effective ingredients. Moreover, in the prior art preparation process of Prunella vulgaris, the formula granules have a high drug loading ratio requirement, and generally the amount of auxiliary materials used shall not be higher than 50%, and the particle size requirement and moisture resistance requirement are higher. If the existing auxiliary materials are used, the prepared formula granules have poor particle size, strong powderiness, low drug loading ratio, and are easy to absorb moisture.

[0030] Example 1

[0031] See also Figure 1 The present invention discloses a method for preparing a herbaceous granule, comprising the following steps:

[0032] S10, soaking: weigh 4500g of Prunella vulgaris slices, add water to cover the slices and soak for 15 minutes;

[0033] In step S10 of the embodiment of the present invention, the reciprocal of the bulk density of the Prunella Vulgaris slices is 32. The volume of the Prunella Vulgaris slices is measured before soaking, and 30 times of water is added to cover the slices. After soaking, most of the Prunella Vulgaris slices are moistened, and the moistening percentage is greater than 75%.

[0034] S20, solid-liquid separation: treating the soaked Prunella Vulgaris decoction pieces to obtain a filtrate, the treating method comprising the following steps:

[0035] S21, the soaked Prunella vulgaris slices are divided into two equal parts, and the parts are added into extraction tanks A and B respectively for extraction, and the extracts from each tank are combined after the extraction is completed;

[0036] S22, centrifuging the extract at high speed using a centrifuge to obtain a centrifuged liquid, performing microfiltration separation on the centrifuged liquid to obtain a microfiltration permeate, and performing ultrafiltration separation on the microfiltration permeate using an ultrafiltration membrane to obtain a filtrate;

[0037] In step S20 of the embodiment of the present invention, the temperature at which the A and B extraction tanks extract the soaked Prunella vulgaris slices is 50° C., the extraction solvent is 60% ethanol at a weight of 4 times that of the Prunella vulgaris slices, the filtrate after filtration has good thermal transmittance, and the apparent clarity percentage after cooling is greater than or equal to 80%, which effectively filters most of the slice fragments and makes the finished product have good clarity;

[0038] Further, in the embodiment of the present invention, the two extraction tanks A and B are in the gradient formation stage, the extraction time of tank A is 30min and 60min respectively; the extraction time of tank B is 0min and 30min, the extraction time of each tank is 1h in the extraction stage, the heating time of the extraction tank is controlled within 10min in the extraction stage, and the extracts of each tank are combined after the extraction is completed;

[0039] In addition, in an embodiment of the present invention, an Alfa Laval disc centrifuge is used to perform high-speed centrifugation on the extract, the centrifuge speed is 5000r / min, and the centrifugation is performed for 20min to obtain a centrifuged liquid; a ceramic membrane unit with a membrane pore size of 0.05μ is used to perform microfiltration separation on the centrifuged liquid to obtain a microfiltration permeate, and the temperature of the microfiltration separation treatment is 30°C; a polyvinylidene fluoride ultrafiltration membrane is used to perform ultrafiltration separation on the microfiltration permeate to obtain an ultrafiltrate, and the ultrafiltration temperature is 30°C.

[0040] S30, concentration: vacuum concentrate the filtrate, set the concentration temperature to 65°C, and the vacuum degree to ≥-0.08 MPa, and concentrate to a relative density of 1.08 (measured at 60°C) to obtain a clear paste. The concentration standard of the clear paste is that the viscosity of the clear paste after concentration is just right and it is easy to spray;

[0041] It should be noted that the concentration step in the embodiment of the present invention adopts reduced pressure and low temperature concentration according to the concentration requirements in the Technical Requirements for Quality Control and Standardization of Traditional Chinese Medicine Formula Granules, and the concentration temperature needs to be lower than 65°C. Referring to the corresponding table of vacuum degree and boiling point of water, it can be seen that the vacuum degree corresponding to 65°C is -0.0761 MPa. Therefore, the concentration vacuum degree needs to reach -0.0761 or less. Therefore, it is preliminarily determined that the concentration vacuum degree is ≥-0.08 MPa, and the heating temperature is set to 65°C;

[0042] In addition, according to the requirements of standard decoctions in the "Technical Requirements for Quality Control and Standardization of Chinese Herbal Medicine Granules", low-temperature drying is adopted. The more mature drying method is spray drying. The requirement of spray drying for the concentrated liquid is mainly the relative density. The suitable relative density of the liquid medicine for spray drying is 1.10-1.15. Therefore, the liquid medicine is concentrated to a relative density of 1.08-1.13 (measured at 60°C).

[0043] S40, drying the clear paste to prepare dry paste powder, adding auxiliary materials, mixing evenly, dry granulating, preparing granules of 1000 g per package, and obtaining the Prunella Vulgaris formula granules.

[0044] In step S40 of the embodiment of the present invention, the method of drying the clear paste to prepare dry paste powder includes freeze drying and spray drying, wherein:

[0045] (1) Freeze drying: Freeze the paste for 4 hours and then dry it to obtain dry paste powder;

[0046] (2) Spray drying: Add 2% maltodextrin to the clear paste, mix evenly, and spray dry to form dry paste powder;

[0047] Furthermore, in the spray drying step, the inlet air temperature is 175-185°C, preferably 180°C.

[0048] In addition, in step S40 of the embodiment of the present invention, the auxiliary material is one or more of corn starch, dextrin, and maltodextrin. Preferably, the auxiliary material is dextrin. After the dry paste is added with the dextrin auxiliary material, it meets the standard requirements in terms of appearance, particle size, friability and solubility, and the hygroscopicity and fluidity are both above the requirements.

[0049] In addition, in step S40, the prepared particles are packaged in a composite aluminum film, which is a conventional packaging material for granules and is also a packaging material for existing formula granule manufacturers. The packaging process is mature and the industrialized production efficiency is high. The packaging has good sealing and moisture-proof properties, can effectively block the effects of light, heat, water vapor, oxygen, etc. on the drug, and is easy to carry and use.

[0050] Example 2

[0051] See also Figure 1 The present invention discloses a method for preparing a herbaceous granule, comprising the following steps:

[0052] S10, soaking: weigh 4500g of Prunella vulgaris slices, add water to cover the slices and soak for 60 minutes;

[0053] In step S10 of the embodiment of the present invention, the reciprocal of the bulk density of the Prunella Vulgaris slices is 32. The volume of the Prunella Vulgaris slices is measured before soaking, and 46 times of water is added to cover the slices. After soaking, most of the Prunella Vulgaris slices are moistened, and the moistening percentage is greater than 75%.

[0054] S20, solid-liquid separation: treating the soaked Prunella Vulgaris decoction pieces to obtain a filtrate, the treating method comprising the following steps:

[0055] S21, the soaked Prunella vulgaris slices are divided into two equal parts, and the parts are added into extraction tanks A and B respectively for extraction, and the extracts from each tank are combined after the extraction is completed;

[0056] S22, centrifuging the extract at high speed using a centrifuge to obtain a centrifuged liquid, performing microfiltration separation on the centrifuged liquid to obtain a microfiltration permeate, and performing ultrafiltration separation on the microfiltration permeate using an ultrafiltration membrane to obtain a filtrate;

[0057] In step S20 of the embodiment of the present invention, the temperature at which the A and B extraction tanks extract the soaked Prunella vulgaris slices is 80° C., the extraction solvent is 60% ethanol at 8 times the weight of the Prunella vulgaris slices, the filtrate after filtration has good thermal transmittance, and the apparent clarity percentage after cooling is greater than or equal to 80%, which effectively filters most of the slice fragments and makes the finished product have good clarity;

[0058] Further, in the embodiment of the present invention, the two extraction tanks A and B are in the gradient formation stage, the extraction time of tank A is 30min and 60min respectively; the extraction time of tank B is 0min and 30min, the extraction time of each tank is 1-2h in the extraction stage, the heating time of the extraction tank is controlled within 10min in the extraction stage, and the extracts of each tank are combined after the extraction is completed;

[0059] In addition, in an embodiment of the present invention, an Alfa Laval disc centrifuge is used to perform high-speed centrifugation on the extract, the centrifuge speed is 8000r / min, and the centrifugation is performed for 30min to obtain a centrifuged liquid; a ceramic membrane unit with a membrane pore size of 0.05μ is used to perform microfiltration separation on the centrifuged liquid to obtain a microfiltration permeate, and the temperature of the microfiltration separation treatment is 60°C; a polyvinylidene fluoride ultrafiltration membrane is used to perform ultrafiltration separation on the microfiltration permeate to obtain an ultrafiltrate, and the ultrafiltration temperature is 45°C.

[0060] S30, concentration: vacuum concentrate the filtrate, set the concentration temperature to 65°C, and the vacuum degree to ≥-0.08mpa, and concentrate to a relative density of 1.13 (measured at 60°C) to obtain a clear paste. The concentration standard of the clear paste is that the viscosity of the clear paste after concentration is just right and it is easy to spray;

[0061] It should be noted that the concentration step in the embodiment of the present invention adopts reduced pressure and low temperature concentration according to the concentration requirements in the Technical Requirements for Quality Control and Standardization of Traditional Chinese Medicine Formula Granules, and the concentration temperature needs to be lower than 65°C. Referring to the corresponding table of vacuum degree and boiling point of water, it can be seen that the vacuum degree corresponding to 65°C is -0.0761 MPa. Therefore, the concentration vacuum degree needs to reach -0.0761 or less. Therefore, it is preliminarily determined that the concentration vacuum degree is ≥-0.08 MPa, and the heating temperature is set to 65°C;

[0062] In addition, according to the requirements of standard decoctions in the "Technical Requirements for Quality Control and Standardization of Chinese Herbal Medicine Granules", low-temperature drying is adopted. The more mature drying method is spray drying. The requirement of spray drying for the concentrated liquid is mainly the relative density. The suitable relative density of the liquid medicine for spray drying is 1.10-1.15. Therefore, the liquid medicine is concentrated to a relative density of 1.08-1.13 (measured at 60°C).

[0063] S40, drying the clear paste to prepare dry paste powder, adding auxiliary materials, mixing evenly, dry granulating, preparing granules of 1000 g per package, and obtaining the Prunella Vulgaris formula granules.

[0064] In step S40 of the embodiment of the present invention, the method of drying the clear paste to prepare dry paste powder includes freeze drying and spray drying, wherein:

[0065] (1) Freeze drying: Freeze the paste for 6 hours and then dry it to obtain dry paste powder;

[0066] (2) Spray drying: Add 2% maltodextrin to the clear paste, mix evenly, and spray dry to form dry paste powder;

[0067] Furthermore, in the spray drying step, the inlet air temperature is 175-185°C, preferably 185°C.

[0068] In addition, in step S40 of the embodiment of the present invention, the auxiliary material is one or more of corn starch, dextrin, and maltodextrin. Preferably, the auxiliary material is dextrin. After the dry paste is added with the dextrin auxiliary material, it meets the standard requirements in terms of appearance, particle size, friability and solubility, and the hygroscopicity and fluidity are both above the requirements.

[0069] In addition, in step S40, the prepared particles are packaged in a composite aluminum film, which is a conventional packaging material for granules and is also a packaging material for existing formula granule manufacturers. The packaging process is mature and the industrialized production efficiency is high. The packaging has good sealing and moisture-proof properties, can effectively block the effects of light, heat, water vapor, oxygen, etc. on the drug, and is easy to carry and use.

[0070] Example 3

[0071] See also Figure 1 The present invention discloses a method for preparing a herbaceous granule, comprising the following steps:

[0072] S10, soaking: weigh 4500g of Prunella vulgaris slices, add water to cover the slices and soak for 15 minutes;

[0073] In step S10 of the embodiment of the present invention, the reciprocal of the bulk density of the Prunella Vulgaris slices is 32. The volume of the Prunella Vulgaris slices is measured before soaking, and 38 times of water is added to cover the slices. After soaking, most of the Prunella Vulgaris slices are moistened, and the moistening percentage is greater than 75%.

[0074] S20, solid-liquid separation: treating the soaked Prunella Vulgaris decoction pieces to obtain a filtrate, the treating method comprising the following steps:

[0075] S21, the soaked Prunella vulgaris slices are divided into two equal parts, and the parts are added into extraction tanks A and B respectively for extraction, and the extracts from each tank are combined after the extraction is completed;

[0076] S22, centrifuging the extract at high speed using a centrifuge to obtain a centrifuged liquid, performing microfiltration separation on the centrifuged liquid to obtain a microfiltration permeate, and performing ultrafiltration separation on the microfiltration permeate using an ultrafiltration membrane to obtain a filtrate;

[0077] In step S20 of the embodiment of the present invention, the temperature at which the A and B extraction tanks extract the soaked Prunella vulgaris slices is 60° C., the extraction solvent is 60% ethanol, which is 6 times the weight of the Prunella vulgaris slices. The filtrate after filtration has good thermal transmittance, and the apparent clarity percentage after cooling is greater than or equal to 80%, which effectively filters most of the slice fragments and makes the finished product have good clarity.

[0078] Further, in the embodiment of the present invention, the two extraction tanks A and B are in the gradient formation stage, the extraction time of tank A is 30min and 60min respectively; the extraction time of tank B is 0min and 30min, the extraction time of each tank is 1-2h in the extraction stage, the heating time of the extraction tank is controlled within 10min in the extraction stage, and the extracts of each tank are combined after the extraction is completed;

[0079] In addition, in an embodiment of the present invention, an Alfa Laval disc centrifuge is used to perform high-speed centrifugation on the extract, the centrifuge speed is 6000r / min, and the centrifugation is performed for 30min to obtain a centrifuged liquid; a ceramic membrane unit with a membrane pore size of 0.05μ is used to perform microfiltration separation on the centrifuged liquid to obtain a microfiltration permeate, and the temperature of the microfiltration separation treatment is 45°C; a polyvinylidene fluoride ultrafiltration membrane is used to perform ultrafiltration separation on the microfiltration permeate to obtain an ultrafiltrate, and the ultrafiltration temperature is 30°C.

[0080] S30, concentration: vacuum concentrate the filtrate, set the concentration temperature to 65°C, and the vacuum degree to ≥-0.08mpa, and concentrate to a relative density of 1.10 (measured at 60°C) to obtain a clear paste. The concentration standard of the clear paste is that the viscosity of the clear paste after concentration is just right and it is easy to spray;

[0081] It should be noted that the concentration step in the embodiment of the present invention adopts reduced pressure and low temperature concentration according to the concentration requirements in the Technical Requirements for Quality Control and Standardization of Traditional Chinese Medicine Formula Granules, and the concentration temperature needs to be lower than 65°C. Referring to the corresponding table of vacuum degree and boiling point of water, it can be seen that the vacuum degree corresponding to 65°C is -0.0761 MPa. Therefore, the concentration vacuum degree needs to reach -0.0761 or less. Therefore, it is preliminarily determined that the concentration vacuum degree is ≥-0.08 MPa, and the heating temperature is set to 65°C;

[0082] In addition, according to the requirements of standard decoctions in the "Technical Requirements for Quality Control and Standardization of Chinese Herbal Medicine Granules", low-temperature drying is adopted. The more mature drying method is spray drying. The requirement of spray drying for the concentrated liquid is mainly the relative density. The suitable relative density of the liquid medicine for spray drying is 1.10-1.15. Therefore, the liquid medicine is concentrated to a relative density of 1.10 (measured at 60°C).

[0083] S40, drying the clear paste to prepare dry paste powder, adding auxiliary materials, mixing evenly, dry granulating, preparing granules of 1000 g per package, and obtaining the Prunella Vulgaris formula granules.

[0084] In step S40 of the embodiment of the present invention, the method of drying the clear paste to prepare dry paste powder includes freeze drying and spray drying, wherein:

[0085] (1) Freeze drying: Freeze the paste for 4 hours and then dry it to obtain dry paste powder;

[0086] (2) Spray drying: Add 2% maltodextrin to the clear paste, mix evenly, and spray dry to form dry paste powder;

[0087] Furthermore, in the spray drying step, the inlet air temperature is 175-185°C, preferably 180°C.

[0088] In addition, in step S40 of the embodiment of the present invention, the auxiliary material is one or more of corn starch, dextrin, and maltodextrin. Preferably, the auxiliary material is dextrin. After the dry paste is added with the dextrin auxiliary material, it meets the standard requirements in terms of appearance, particle size, friability and solubility, and the hygroscopicity and fluidity are both above the requirements.

[0089] In addition, in step S40, the prepared particles are packaged in a composite aluminum film, which is a conventional packaging material for granules and is also a packaging material for existing formula granule manufacturers. The packaging process is mature and the industrialized production efficiency is high. The packaging has good sealing and moisture-proof properties, can effectively block the effects of light, heat, water vapor, oxygen, etc. on the drug, and is easy to carry and use.

[0090] Process research experiment:

[0091] Experiment 1: Soaking time

[0092] 1. Instruments and test drugs

[0093] Instruments: JJ1000 electronic balance, TC20K-H electronic balance, Sartorius SQP 1 / 10,000 balance, round bottom flask, electric heating mantle, etc.

[0094] Test drugs: Prunella vulgaris slices (batch numbers: 2011001, 2103001, 2104001), drinking water, purified water;

[0095] 2. Experimental methods

[0096] Take 100g of Prunella Vulgaris slices of different batches, three times, in a beaker, record the volume of the slices of the three batches, calculate the bulk density, and then transfer them to a beaker. Add 33 times water to cover the slices and start soaking. Soak for 15, 30, 45, and 60 minutes respectively, take samples for inspection, break the slices apart, observe whether they are moistened, and record the apparent wetting percentage. Finally, comprehensively evaluate the soaking time before extraction according to the wetting effect.

[0097] 3. Experimental results and analysis

[0098] The experimental results are shown in Table 1:

[0099] Table 1 Results of wetting percentage by immersion time

[0100]

[0101] From the results, we can see that the reciprocal of the bulk density is about 32, the amount of water added can be 33-40 times, and after soaking for 15 minutes, the wetting percentage is greater than 75%, which means that most of the material is wetted. Therefore, soaking for 15 minutes is determined as the preferred soaking time.

[0102] Experiment 2: Water Addition

[0103] 1. Instruments and test drugs

[0104] Instruments: JJ1000 electronic balance, TC20K-H electronic balance, Sartorius SQP 1 / 10,000 balance, liquid chromatograph, round bottom flask, electric heating mantle, etc.

[0105] Test drugs: Prunella vulgaris slices, drinking water, purified water, and reagents are all analytical and chromatographic grade;

[0106] 2. Experimental methods

[0107] Take 100g of Prunella vulgaris slices, add 30, 38, and 46 times water respectively, soak for 15 minutes, heat and extract for 1 hour, and filter. Take samples of the three groups of water extracts to determine the dry paste yield, and freeze-dry the remaining parts into dry paste for determination of the index component content.

[0108] 3. Experimental results and analysis

[0109] The experimental results are shown in Table 2:

[0110] Table 2 Water addition test results

[0111]

[0112] Analysis of results: The national standard for Prunella Vulgaris formula granules requires a dry paste yield of 9%-15%. From the results, it can be seen that adding 30 times the water meets the requirements, adding 38 times the water also meets the requirements, and adding 46 times the water also meets the requirements. Adding 38 times the water is 9.79% higher than adding 30 times the water, and adding 46 times the water is 0.21% higher than adding 38 times the water. From the content point of view, the requirement is 7.0-20.0mg / 4.5g of decoction piece. From the results, it can be seen that adding 30 times the water meets the requirements, adding 38 times the water meets the requirements, and adding 46 times the water also meets the requirements. Adding 38 times the water is 24.64% higher than adding 30 times the water, but the difference between adding 46 times the water and adding 38 times the water is 0.74%. Considering all factors, 38 times the amount of water is selected.

[0113] Experiment 3: Concentration process research

[0114] 1. Instruments and test drugs

[0115] Instruments: JJ1000 electronic balance, TC20K-H electronic balance, RE-6000A rotary evaporator, liquid chromatograph, round bottom flask, electric heating mantle, etc.

[0116] Test drugs: Prunella vulgaris slices (batch number: 2103001), drinking water, purified water, and reagents were all analytical and chromatographic grade.

[0117] 2. Experimental methods

[0118] Take 100g of Prunella vulgaris slices, add 38 times water to cover the slices, soak for 15 minutes, heat and extract for 1 hour, and filter. The filtrate is vacuum concentrated, the concentration temperature is set to 65°C, the vacuum degree reaches ≥-0.08mpa, and when it is concentrated to a relative density of 1.10, take half of the sample, and continue to concentrate. When it is concentrated to a relative density of 1.15, stop concentrating, sample the 2 groups of concentrated liquids to measure the dry paste yield, and freeze-dry the remaining part into a dry paste for determination of the content of the index components.

[0119] 3. Experimental results and analysis

[0120] The experimental results are shown in Table 3:

[0121] Table 3 Concentration degree experimental results

[0122]

[0123] Analysis of results: The national standard for Prunella Vulgaris formula granules requires a dry paste yield of 9%-15%. The results show that the concentration to 1.15 is 0% higher than that to 1.10. From the content point of view, the requirement is 7.0-20.0mg / 4.5g of decoction piece. The results show that the concentration to 1.15 is 0.27% lower than that to 1.10. When the clear paste is concentrated to 1.10, the viscosity is just right and it is easier to spray. Taking all factors into consideration, it is chosen to concentrate to a relative density of 1.08-1.13 (60℃).

[0124] Experiment 4: Drying process research

[0125] 1. Instruments and test drugs

[0126] Instruments: JJ1000 electronic balance, TC20K-H electronic balance, RE-6000A rotary evaporator, freeze dryer, spray dryer, round bottom flask, electric heating mantle, etc.

[0127] Test drug: Prunella vulgaris slices (batch number: 2011001), drinking water, purified water, and reagents were all analytical and chromatographic grade.

[0128] 2. Experimental methods

[0129] Grind the dry paste into fine powder, take an appropriate amount, weigh it accurately, spread it in a clean weighing bottle, the thickness is ≤5mm, and the total weight is accurate. At the same time, take four portions of dry paste powder, add different auxiliary materials (corn starch, dextrin, maltodextrin) according to the maximum amount of auxiliary materials M, mix evenly, spread it in a weighing bottle according to the previous method, weigh it accurately, put five samples into a desiccator (relative humidity 58%) filled with sulfuric acid solution (39.5ml sulfuric acid plus 100ml water), take them out at 0.25h, 0.5h, 1h, 1.5h, 2h, 3h, 4h, 6h, 8h, 10h, and 24h, weigh them accurately, and calculate the moisture absorption of the samples.

[0130] 3. Experimental results and analysis

[0131] The experimental results are shown in Table 4:

[0132] Table 4 Dry paste powder moisture absorption test results

[0133]

[0134] Analysis of results: From the results, it can be seen that this variety has obvious moisture absorption when no auxiliary materials are added, and the moisture absorption is 5.5% when reaching the equilibrium point. It is significantly reduced after adding auxiliary materials. After adding maltodextrin, the moisture absorption is 3%. Therefore, maltodextrin is selected as an auxiliary material during spray drying.

[0135] In summary, the preparation process of the herbaceous prunellae formula granules of the present invention is improved, the process step parameters in the soaking process, concentration process and drying process of the herbaceous prunellae decoction pieces are adjusted, the paste yield of the herbaceous prunellae decoction pieces is improved, the prepared formula granules have a high content of effective ingredients, a small dosage, high stability of the finished product, are easy to preserve, and are suitable for promotion to large-scale production.

[0136] It will be apparent to those skilled in the art that the invention is not limited to the details of the exemplary embodiments described above and that the invention can be implemented in other specific forms without departing from the spirit or essential features of the invention. Therefore, the embodiments should be considered exemplary and non-limiting in all respects, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations falling within the meaning and scope of the equivalent elements of the claims be included in the invention. Any reference numeral in a claim should not be considered as limiting the claim to which it relates.

[0137] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. A method for preparing a herbaceous granule, characterized in that: The following steps are involved: S10, soaking: weigh 4500g of Prunella vulgaris slices, add water to cover the slices and soak for 15-60min; S20, solid-liquid separation: treating the soaked Prunella Vulgaris decoction pieces to obtain a filtrate, the treating method comprising the following steps: S21, the soaked Prunella vulgaris slices are divided into two equal parts, and the parts are added into extraction tanks A and B respectively for extraction, and the extracts from each tank are combined after the extraction is completed; The temperature of extracting the soaked Prunella vulgaris slices by the A and B extraction tanks is 50-80° C., and the extraction solvent is 60% ethanol in an amount of 4-8 times the weight of the Prunella vulgaris slices; The two extraction tanks A and B are in the gradient formation stage. The extraction time of tank A is 30min and 60min respectively; the extraction time of tank B is 0min and 30min. During the extraction stage, the extraction time of each tank is 1h. During the extraction stage, the heating time of the extraction tank is controlled within 10min. After the extraction, the extracts of each tank are combined. S22, centrifuging the extract at high speed using a centrifuge to obtain a centrifuged liquid, performing microfiltration separation on the centrifuged liquid to obtain a microfiltration permeate, and performing ultrafiltration separation on the microfiltration permeate using an ultrafiltration membrane to obtain a filtrate; S30, concentration: vacuum concentrating the filtrate to a relative density of 1.08-1.13, wherein the relative density is measured at 60° C., to obtain a clear paste; S40, drying the clear paste to prepare dry paste powder, adding auxiliary materials, mixing evenly, dry granulating, preparing granules of 1000g per pack, and obtaining the herbaceous prunella vulgaris formula granules; In step S10, the reciprocal of the bulk density of the Prunella Vulgaris slices is 32. The volume of the Prunella Vulgaris slices is measured before soaking, and 30-46 times of water is added to cover the slices. The wetting percentage of the Prunella Vulgaris slices after soaking is greater than 75%.

2. The method for preparing the herbaceous granules according to claim 1, characterized in that: In step S30, the concentration temperature is set to 65°C and the vacuum degree reaches ≥-0.08 MPa.

3. The method for preparing the herbaceous granules according to claim 1, characterized in that: In step S40, the method of drying the clear paste to prepare dry paste powder includes freeze drying and spray drying, wherein: Freeze drying: Freeze the paste for 4-6 hours and then dry it to obtain dry paste powder; (2) Spray drying: Add 2% maltodextrin to the clear paste, mix evenly, and spray dry into dry paste powder.

4. The method for preparing the herbaceous granules according to claim 3, characterized in that: In the spray drying step, the inlet air temperature is 175-185°C, preferably 180-185°C.

5. The method for preparing the herbaceous granules according to claim 1, characterized in that: In step S40, the auxiliary material is one or more of corn starch, dextrin, and maltodextrin.

6. The method for preparing the herbaceous granules according to claim 5, characterized in that: The auxiliary material is dextrin.

7. The method for preparing the herbaceous granules according to claim 1, characterized in that: In step S40, the prepared particles are packaged with a composite aluminum film.

8. A formula granule of Prunella vulgaris, characterized in that: The Prunella Vulgaris formula granules are prepared according to the preparation method according to any one of claims 1 to 7.

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