CN112656834A - Angelica sinensis and astragalus membranaceus blood replenishing particles and preparation method thereof - Google Patents
Angelica sinensis and astragalus membranaceus blood replenishing particles and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a Chinese angelica and astragalus root blood-enriching particle and a preparation method thereof, wherein the preparation method comprises the following steps: (1) soaking radix astragali decoction pieces and radix Angelicae sinensis in water, reflux extracting, and collecting aromatic water during extraction process to obtain extractive solution and aromatic water; (2) concentrating the extract under reduced pressure to obtain concentrated solution; (3) uniformly mixing the concentrated solution and aromatic water, and spray-drying to obtain spray-dried powder; (4) and mixing the spray-dried powder and the auxiliary materials uniformly, and performing dry granulation to obtain the angelica sinensis and astragalus membranaceus blood replenishing granules. In the extraction process, the condensation device is adopted to collect the aromatic water, so that the volatilized ligustilide is reserved, the aromatic water is directly added back to the concentration for drying and granulation, the loss of volatile component ligustilide is avoided to a great extent, the retention rate of the ligustilide is improved from 0-1% to more than 40%, the effective utilization of water-soluble components and volatile components is effectively ensured, and the effective clinical effect of the angelica and astragalus membranaceus blood-enriching decoction granules is effectively exerted.
Description
Technical Field
The invention relates to the field of angelica sinensis blood enriching preparations, in particular to angelica sinensis and astragalus membranaceus blood enriching particles and a preparation method thereof.
Background
The angelica sinensis blood-enriching soup is made from astragalus and angelica sinensis according to a ratio of 5:1, wherein the astragalus membranaceus is used for greatly tonifying qi of spleen and lung, nourishing the source of qi and blood generation, and the angelica sinensis is used for nourishing blood and regulating nutrient, and is used for tonifying both qi and blood. Mainly treats the syndrome of fever caused by blood deficiency, has the efficacies of tonifying qi and generating blood and controlling blood circulation to defervesce, and is a classic and famous prescription for tonifying qi and generating blood. Modern clinical researches prove that the angelica sinensis blood-enriching soup can be used for treating various types of anemia, climacteric syndrome, immune system disorder, cardiovascular and cerebrovascular diseases, surgical and orthopedic operations and postoperative complications, and the adjuvant therapy of cancer patients undergoing radiotherapy and chemotherapy.
According to the original prescription, the traditional preparation process and taking method of the prescription are' a piece of chewing, and the piece of chewing is taken as one piece. Decocting two pieces of water to obtain a decoction, removing residues, and taking the decoction warm before eating. The traditional preparation process is rough, lacks of clear process parameters and evaluation indexes, and is difficult to meet the requirements of stable quality and curative effect. In addition, the traditional decoction is inconvenient to take and carry, takes time to decoct and the like, and is not beneficial to daily use of patients. At present, the Chinese pharmacopoeia 2020 edition pharmacopoeia has recorded the Chinese angelica blood-enriching oral liquid, but the ratio of the astragalus root and the Chinese angelica is 5:2, which is different from the original prescription composition. In the preparation method, the angelica needs to extract the distillate first, and then the dregs of a decoction are mixed with the astragalus to extract, so that the heating time of the water-soluble active ingredients is long, and the loss of the water-soluble active ingredients is serious; in addition, most of the polar components which are soluble in water and insoluble in alcohol are removed by alcohol precipitation after the extract is concentrated, and the process route and the material basis of the extract do not conform to the requirements of the traditional classical famous prescription decoction.
The granule is the most similar to the traditional decoction in the aspect of taking mode, is convenient to carry and take, and is one of the important dosage forms of the traditional Chinese medicine compound preparation at present. However, in actual mass production, the production equipment, process and process control of the granules are greatly different from the traditional decoction, for example, the traditional decoction is heated for a short time, and most of compound preparations are subjected to pressure reduction concentration and drying molding for a long time, so that the fluctuation of thermally unstable components is large, the loss of volatile components is serious, for example, the loss of ligustilide in angelica is serious. In the existing preparation of angelica sinensis blood-enriching granules, beta-cyclodextrin is adopted to perform inclusion treatment on ligustilide, so that the retention rate is improved, but the utilization degree of the ligustilide is obviously changed after the inclusion compound enters the body, and the change is shown as the change of pharmacokinetic parameters such as AUC, Cmax and the like, so that the clinical curative effect of the granules added with the ligustilide inclusion compound is different from that of the traditional decoction.
Disclosure of Invention
The invention aims to provide angelica and astragalus membranaceus blood-enriching particles which have the characteristics of high content of effective component ligustilide and good drug effect.
The invention also aims to provide a preparation method of the angelica sinensis and astragalus membranaceus blood-enriching particles, which has the characteristics of high retention rate and high production efficiency of an effective component ligustilide in the process flow.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of angelica sinensis and astragalus membranaceus blood replenishing particles comprises the following steps:
(1) soaking radix astragali decoction pieces and radix Angelicae sinensis in water, reflux extracting, and collecting aromatic water during extraction process to obtain extractive solution and aromatic water;
(2) concentrating the extract under reduced pressure to obtain concentrated solution;
(3) uniformly mixing the concentrated solution and aromatic water, and spray-drying to obtain spray-dried powder;
(4) and mixing the spray-dried powder and the auxiliary materials uniformly, and performing dry granulation to obtain the angelica sinensis and astragalus membranaceus blood replenishing granules.
Further, in the step (2), the relative density of the concentrated solution is 1.07-1.20 g/ml at the temperature of 60 ℃.
Further, in the step (3), the ratio of the concentrated solution to the aromatic water is 1:1 by weight.
Further, in the step (1), water with the weight ratio of 7-8 times of the total feeding amount is added for soaking for 25-35 minutes, and reflux extraction is carried out for 1-2 hours to obtain an extracting solution and aromatic water.
Further, in the step (1), the aromatic water accounts for 3.5-7% of the added water by weight.
Further, in the step (3), the process parameters of the spray drying are as follows: the air inlet temperature is 150-180 ℃, and the air outlet temperature is 80-90 ℃.
The angelica sinensis and astragalus membranaceus blood replenishing particle is prepared by the preparation method of the angelica sinensis and astragalus membranaceus blood replenishing particle, and comprises the following raw materials of astragalus membranaceus decoction pieces, wine-processed angelica sinensis and auxiliary materials, wherein the mass ratio of the astragalus membranaceus decoction pieces to the wine-processed angelica sinensis is 5: 1;
the grain diameters of the astragalus membranaceus decoction pieces and the wine angelica sinensis are respectively 4-24 meshes.
Furthermore, the auxiliary materials comprise maltodextrin, micropowder silica gel and magnesium stearate.
Further, in the step (4), the addition weight of the maltodextrin is 12-40% of the weight of the spray-dried powder;
the adding weight of the micro-powder silica gel is 0.5 to 1.0 percent of the weight of the spray-dried powder;
the addition weight of the magnesium stearate is 0.3-0.5% of the weight of the spray-dried powder.
Furthermore, the particle size of the angelica sinensis and astragalus membranaceus blood replenishing particles is 16-40 meshes.
The invention has the beneficial effects that:
1. therefore, the invention adopts a reflux extraction method to extract the astragalus decoction pieces and the wine angelica, avoids serious loss of volatile components, and adopts a condensing device to collect aromatic water in the extraction process, so that the volatilized ligustilide is reserved. Because the loss rate of the ligustilide is over 99 percent when the ligustilide is concentrated under reduced pressure, the extracting solution is mixed with aromatic water for drying and granulation, the loss of volatile component ligustilide is avoided to a great extent, the retention rate of the ligustilide is improved from 0-1 percent to more than 40 percent, and the effective utilization of water-soluble components and volatile components and the effective exertion of clinical curative effect of the angelica and astragalus blood-enriching decoction granules are effectively ensured.
2. The aromatic water collected in the preparation process of the angelica and astragalus membranaceus blood-enriching particles is directly added back into the concentrated solution for spray drying and granulation, a beta-cyclodextrin inclusion mode is not needed, and the change of pharmacokinetic parameters after the angelica and astragalus membranaceus blood-enriching particles enter the body is effectively avoided, so that the clinical curative effect of the angelica and astragalus membranaceus blood-enriching particles is influenced.
3. The invention adopts spray drying and dry granulation to prepare the granules, the spray drying has the characteristics of high drying speed and high production efficiency, the solvent of the atomized granules can be instantly volatilized, the heating time of the material is extremely short, and the thermal instability component can be protected.
Detailed Description
The technical solution of the present invention will be further described with reference to the following embodiments.
A preparation method of angelica sinensis and astragalus membranaceus blood replenishing particles comprises the following steps:
(1) soaking radix astragali decoction pieces and radix Angelicae sinensis in water, reflux extracting, and collecting aromatic water during extraction process to obtain extractive solution and aromatic water;
(2) concentrating the extract under reduced pressure to obtain concentrated solution;
(3) uniformly mixing the concentrated solution and aromatic water, and spray-drying to obtain spray-dried powder;
(4) and mixing the spray-dried powder and the auxiliary materials uniformly, and performing dry granulation to obtain the angelica sinensis and astragalus membranaceus blood replenishing granules.
It is worth to be noted that, the astragalus decoction pieces and the alcohol angelica have more volatile components, wherein the ligustilide is an important active component of the alcohol angelica and has volatility, during the processes of stewing and extraction, one part of the ligustilide is remained in the extracting solution, and the other part of the ligustilide is evaporated along with water vapor, so that the loss of the ligustilide is serious, the drug effect of the ligustilide is weakened, and when the extracting solution is subjected to reduced pressure concentration and drying, the loss of the ligustilide in the process of reduced pressure concentration is serious, and the loss rate exceeds 99%. Therefore, the radix astragali decoction pieces and the wine angelica are extracted by a reflux extraction method, so that the serious loss of volatile components is avoided, and the aromatic water is collected by a condensing device in the extraction process, wherein the content of the ligustilide in the aromatic water accounts for 9-10% of the total ligustilide by mass ratio, so that the volatilized ligustilide is reserved. Because the loss rate of the ligustilide is over 99 percent when the ligustilide is concentrated under reduced pressure, the extracting solution is mixed with aromatic water for drying and granulation, the loss of volatile component ligustilide is avoided to a great extent, the retention rate of the ligustilide is improved from 0-1 percent to more than 40 percent, and the effective utilization of water-soluble components and volatile components and the effective exertion of clinical curative effect of the angelica and astragalus blood-enriching decoction granules are effectively ensured.
Specifically, before being soaked in water, the astragalus decoction pieces and the wine-treated angelica are crushed and sieved to reduce the particle size, which is more favorable for soaking and extracting and ensures that the extraction rate of effective components is higher. However, the particle sizes of the astragalus decoction pieces and the angelica sinensis are not suitable to be too small, when the particle sizes of the astragalus decoction pieces and the angelica sinensis are smaller, the powder of the astragalus decoction pieces and the angelica sinensis are lighter, and the astragalus decoction pieces and the angelica sinensis are easy to adhere to the wall after water is boiled, so that part of powder is not effectively extracted, and the extraction rate of effective substances is reduced.
The invention adopts spray drying and dry granulation to prepare the granules, the spray drying has the characteristics of high drying speed and high production efficiency, the solvent of the atomized granules can be instantly volatilized, the heating time of the material is extremely short, and the thermal unstable components can be protected. The dry granulator can effectively avoid the heat influence in the granule forming process, so that the loss of effective components is serious, the granule forming rate reaches 85 percent, and the flowability and the dissolubility are good.
Further, the angelica and astragalus membranaceus blood-enriching particles are simple in preparation method, high in particle forming rate and production efficiency, high in retention rate of an effective component ligustilide and beneficial to industrial production, and the angelica and astragalus membranaceus blood-enriching particles do not adopt a beta-cyclodextrin inclusion mode, so that pharmacokinetic parameter changes after the particles enter a body are avoided, and the clinical curative effect of the particles is influenced.
Furthermore, the relative density of the concentrated solution is 1.07-1.20 g/ml at the temperature of 60 ℃.
The invention adopts a low-temperature vacuum reduced pressure concentration method at 60 ℃ to prepare the concentrated solution, and the relative density of the concentrated solution can influence the content of active ingredients, the yield and the spray drying efficiency. The higher the relative density of the concentrated solution is, the higher the solid content of the concentrated solution is, the fluidity is reduced during discharging, the concentrated solution is easy to adhere to the inner wall and the pipeline of a concentration container, so that the yield is reduced, and when the relative density of the concentrated solution is more than 1.20g/ml, the yield is obviously reduced, so that the content of the effective components is reduced; when the relative density of the concentrated solution is less than 1.20g/ml, the solid content of the concentrated solution is low, and the fluidity of the product is high, so that the subsequent spray drying is not facilitated.
Preferably, under the condition of 60 ℃, when the relative density of the concentrated solution is 1.12-1.17 g/ml, the solid content of the concentrated solution is proper, which is more beneficial for subsequent spray drying, and when the relative density of the concentrated solution is 1.12-1.17 g/ml, the loss of the active ingredients in the concentrated solution is minimum, and the content of the active ingredients has no obvious difference with the content of the active ingredients in the extracting solution.
Further, in the step (3), the ratio of the concentrated solution to the aromatic water is 1:1 by weight.
In spray drying, the more the quality of the added aromatic water, the more the content of effective components in the mixed solution of the concentrated solution and the aromatic water, especially the content of ligustilide. However, with the increase of the quality of the aromatic water, the time of spray drying is prolonged and the temperature of the inlet air is increased, which leads to the loss and the weight increase of the content of the ligustilide, so that preferably, the aromatic water is added into the concentrated solution according to the weight ratio of 1:1, the mixture is evenly mixed and then is spray dried, the volatile component of the ligustilide is reserved in the spray dried powder, the retention rate exceeds 40 percent, and the loss of the medicinal components in the technical process is avoided.
Further, in the step (1), water with the weight ratio of 7-8 times of the total feeding amount is added for soaking for 25-35 minutes, and reflux extraction is carried out for 1-2 hours to obtain an extracting solution and aromatic water.
Before reflux extraction, the Chinese angelica and astragalus root are soaked in water at normal temperature for 25-35 min to dissolve partial effective components and reduce reflux extraction time, so as to avoid serious loss of thermosensitive and volatile effective components and reduce power consumption. Preferably, the soaking time is 30 minutes.
After the reflux extraction is finished, filtering is carried out to obtain an extracting solution, the reflux extraction time is 1-2 hours, effective components can be fully extracted, although the extraction time is prolonged and the content of the effective components is increased, the increase range is small, the process extraction efficiency is reduced, the energy consumption is large, and therefore, the preferred reflux extraction time is 1 hour.
Further, in the step (1), the aromatic water accounts for 3.5-7% of the added water by weight.
The distillation speed of the invention is calculated by the proportion of the aromatic water in the water adding amount obtained per hour, and the distillation speed is controlled by controlling factors such as the distillation temperature and the like, so that the ratio of the aromatic water in the water adding amount is controlled. When the added water amount of the aromatic water is 3.5-7%, the ligustilide in the aromatic water is higher, the content of the ligustilide in the aromatic water is basically consistent, and the influence on the content of the ligustilide is less. Preferably, the aromatic water accounts for 7% of the added water amount by mass ratio.
Further, in the step (3), the spray drying process parameters are as follows: the air inlet temperature is 150-180 ℃, and the air outlet temperature is 80-90 ℃.
In the spray drying process, the higher the air inlet temperature is, the faster the solvent volatilizes, the lower the moisture content of the spray-dried powder is, but the too high air inlet temperature easily destroys the structure of the effective component, so that the content of the thermosensitive component is reduced, the preferable air inlet temperature is 150-180 ℃, the loss of the effective component is less at the moment, and the more preferable air inlet temperature is 150 ℃ in order to save energy consumption.
The angelica sinensis and astragalus membranaceus blood replenishing particle is prepared by the preparation method of the angelica sinensis and astragalus membranaceus blood replenishing particle, and comprises the following raw materials of astragalus membranaceus decoction pieces, wine-processed angelica sinensis and auxiliary materials, wherein the mass ratio of the astragalus membranaceus decoction pieces to the wine-processed angelica sinensis is 5: 1;
the grain diameters of the astragalus membranaceus decoction pieces and the wine angelica sinensis are respectively 4-24 meshes.
The astragalus membranaceus can greatly tonify qi of spleen and lung, nourish the source of qi and blood generation, the angelica sinensis can nourish blood and nourish ying, the astragalus membranaceus decoction pieces and the wine-processed angelica sinensis are combined according to the mass ratio of 5:1, and the effect is better when qi and blood are tonified. Specifically, when the particle sizes of the astragalus mongholicus decoction pieces and the angelica sinensis with wine are smaller, the powder of the astragalus mongholicus decoction pieces and the angelica sinensis with wine are lighter, and the powder is easy to adhere to the wall after water is boiled, so that part of powder is not effectively extracted, and therefore, the extraction rate of effective substances is reduced along with the reduction of the particle sizes of the astragalus mongholicus decoction pieces and the angelica sinensis with wine, preferably, the particle sizes of the astragalus mongholicus decoction pieces and the angelica sinensis with wine are 4 meshes respectively, and the content of.
Furthermore, the auxiliary materials comprise maltodextrin, micro-powder silica gel and magnesium stearate.
Further, in the step (4), the adding weight of the maltodextrin is 12-40% of the weight of the spray-dried powder;
the adding weight of the micro-powder silica gel is 0.5 to 1.0 percent of the weight of the spray-dried powder;
the adding weight of the magnesium stearate is 0.3-0.5% of the weight of the spray-dried powder.
The addition of the auxiliary materials during the compression molding of the particles can improve the viscosity, the hygroscopicity and the fluidity of the spray-dried powder, so that the powder is easier to be compressed and molded. If no auxiliary material is added, the powder has poor fluidity and strong adhesion, and is difficult to be pressed and molded, at the moment, the twice pressing and molding rate of the angelica and astragalus membranaceus blood-enriching particle is only 22.0%, and if only maltodextrin is added without micropowder silica gel and magnesium stearate, the twice pressing and molding rate of the angelica and astragalus membranaceus blood-enriching particle is only 60.1%, and the molding rate is poor. When the addition weight of the maltodextrin is 12-40% of the weight of the spray-dried powder, the addition weight of the aerosil is 0.5-1.0% of the weight of the spray-dried powder and the addition weight of the magnesium stearate is 0.3-0.5% of the weight of the spray-dried powder, the powder flowability and the adhesion can be effectively improved, and the twice compression molding rate of the angelica sinensis and astragalus membranaceus blood-enriching particles reaches 83.5-86.8%.
Preferably, according to the weight ratio, the addition weight of the maltodextrin is 12-20% of the weight of the spray-dried powder, the addition weight of the aerosil is 0.5% of the weight of the spray-dried powder, and the addition weight of the magnesium stearate is 0.3% of the weight of the spray-dried powder, so that the granule compression molding rate is the highest, and the using amount of the auxiliary materials is less.
Furthermore, the particle size of the angelica and astragalus membranaceus blood replenishing particles is 16-40 meshes.
The invention is further illustrated below by the examples and comparative examples.
Example set 1
A granule for tonifying blood is prepared from radix astragali decoction pieces, radix Angelicae sinensis processed with wine and adjuvants, wherein the adjuvants comprise maltodextrin, micropowder silica gel and magnesium stearate. The weight and particle size of the astragalus decoction pieces and the alcohol angelica in this example group are shown in table 1 below.
A preparation method of angelica sinensis and astragalus membranaceus blood replenishing particles comprises the following steps:
(1) adding water 7 times of the total amount of the materials into astragalus decoction pieces and Chinese angelica wine, soaking for 30 minutes, extracting under reflux for 1-2 hours, and collecting aromatic water in the extraction process to obtain an extracting solution and aromatic water; wherein the aromatic water accounts for 7% of the added water amount by weight.
(2) Concentrating the extractive solution at 60 deg.C under reduced pressure to relative density of 1.12g/ml to obtain concentrated solution;
(3) uniformly mixing the concentrated solution and aromatic water according to the mass ratio of 1:1, and then carrying out spray drying to obtain spray-dried powder; wherein the technological parameters of the spray drying are as follows: the air inlet temperature is 150 ℃, and the air outlet temperature is 80 ℃.
(4) And uniformly mixing the spray-dried powder and the auxiliary materials, and performing dry granulation to obtain the angelica sinensis and astragalus membranaceus blood enriching soup granules with the particle size of 16-40 meshes. Specifically, the adding weight of the maltodextrin is 12-40% of the weight of the spray-dried powder; the adding weight of the micro-powder silica gel is 0.5 to 1.0 percent of the weight of the spray-dried powder; the adding weight of the magnesium stearate is 0.3-0.5% of the weight of the spray-dried powder.
TABLE 1
Specifically, the angelica sinensis and astragalus membranaceus blood enriching particles are prepared by respectively adopting the formula and the process parameters in the table 1, the content of the effective components of the extracting solution and the aromatic water obtained in the step (1) is detected, and the detection results are shown in the table 2:
TABLE 2
In Table 2, the contents of calycosin glucoside, astragaloside IV and ferulic acid were calculated as the amount (mg) of the component contained in each gram of the dried extract, and the content of ligustilide was calculated as the amount (mg) of the component contained in each ml of aromatic water. As shown in the test results in Table 2, when the decoction pieces of Astragalus membranaceus and alcohol processed Angelica sinensis were cut into 4-mesh pieces, the content of calycosin glucoside, astragaloside IV and ferulic acid in each gram of the extract was 0.20mg/g, 15.0mg/g and 0.33mg/g, respectively. As the particle size decreases, the contents of the above three components also decrease. Similarly, the aromatic water cut into 4 meshes has the highest ligustilide content of 0.061mg/ml, while the 10 meshes, 15 meshes and 24 meshes are respectively 0.053mg/ml, 0.480mg/ml and 0.043 mg/ml. Therefore, the particle size of the astragalus mongholicus decoction pieces and the radix angelicae sinensis are preferably 4 meshes because the powder of the astragalus mongholicus decoction pieces and the radix angelicae sinensis is light in texture and easy to adhere to the wall after water is boiled, so that part of the powder is not effectively extracted.
Example group 2
According to the formulation and preparation method of examples 1-2, only the relative density of the concentrate after vacuum concentration was changed, and the solid content and yield of the concentrate in this example group and examples 1-2 were examined during vacuum concentration as shown in Table 3 below:
TABLE 3
Specifically, the content of active ingredients in the concentrated solutions with different relative densities in the preparation process of this example group was measured and compared with the content of active ingredients in the extract, as shown in table 4 below:
TABLE 4
As is clear from the results of the measurements in tables 3 and 4, too high relative density tends to result in too high solid content of the concentrated solution, and the fluidity during discharge tends to decrease, and the concentrated solution tends to adhere to the inner wall and the pipe of the concentration vessel, resulting in a decrease in yield. Specifically, under the condition of 60 ℃, the yield of the concentrated solution is obviously reduced when the relative density is 1.20, which is reduced by 17 percent compared with 1.17 g/ml. Preferably, when the relative density of the concentrated liquid phase is 1.12-1.17 g/ml, the solid content is proper, and the concentrated liquid is more suitable for subsequent spray drying. In addition, as can be seen from the content comparison results in table 4, there was no significant difference in the contents of calycosin glucoside, astragaloside IV and ferulic acid in the concentrated solution and the extract, indicating that the active ingredients were not destroyed during the concentration heating process. In summary, the relative density of the preferred concentrate of the present invention is preferably in the range of 1.12 to 1.17 g/ml.
Comparative example 1
The preparation method of the comparative example 1 is basically the same as that of the examples 1-2, except that the beta-cyclodextrin is added into the extracted and collected aromatic water according to the mass ratio of 10:1, the mixture is ground and included for 40min at 40 ℃ by a homogenizer, the mixture is refrigerated overnight at 4 ℃, the mixture is taken out, filtered, decompressed and dried at 40 ℃ to obtain an inclusion compound, the inclusion compound is weighed and added into spray-dried powder by an equivalent incremental method, and the spray-dried powder P1 is obtained after the mixture is uniformly mixed. It is worth noting that the concentrate of this comparative example was spray dried without the addition of aromatic water.
The quality of ligustilide was measured in the extract and spray dried powder P2 of example 1-2 and the spray dried powder P1 prepared in this comparative example 1, as shown in table 5 below:
TABLE 5
As shown in Table 5, the spray dried powder P2 prepared by adding aromatic water in example 1-2 has ligustilide content closer to that of the extractive solution, and the content is 9.35mg and 9.63mg, respectively, which indicates that the material basis of the volatile parts is substantially the same. The comparative example adopts a grinding method, aromatic water is coated by beta-cyclodextrin to prepare solid, the mass of ligustilide in the obtained spray-dried powder P1 is 14.1mg, which is about 33 percent higher than that of spray-dried powder P2 prepared by adding aromatic water, the retention rate of ligustilide is higher, and the spray-dried powder conforms to the characteristics of coating technology. However, studies have shown that the bioavailability of ligustilide is significantly altered after inclusion in vivo, as manifested by changes in pharmacokinetic parameters, such as AUC, Cmax, etc. The Chinese herbal compound has the characteristics of multiple components and multiple target points in the body, and the change of the content of the ligustilide can change the operation of other components in the body, namely the interaction of the medicines, thereby causing the difference of curative effects. Therefore, the drug effect base of the granule after being added with the ligustilide inclusion compound is not consistent with that of the traditional decoction. In addition, the inclusion effect of ligustilide is the best when the mass ratio of the aromatic water to the beta-cyclodextrin is 10:1, but the addition amount of the beta-cyclodextrin is larger and accounts for 23.6 percent of the dry extract, and the dosage of a patient is increased after the particles are prepared, which is not beneficial to the medication compliance of the patient. Considering the foundation of curative effect and patient compliance, the spray drying method with aromatic water in the embodiments 1-2 better meets the quality requirement of the product.
Comparative example 2
Comparative example 2 and examples 1-2 were prepared in substantially the same manner except that the concentrate was spray-dried directly without adding perfume water back to the concentrate and spray-dried, and the content of ligustilide in the spray-dried powder during the preparation of comparative example 2 and examples 1-1, 1-2 and 1-3 was measured and the retention thereof was calculated as shown in table 6 below:
TABLE 6
As shown in Table 6, ligustilide is an important active ingredient of alcohol processed radix Angelicae sinensis, has volatility, and can be evaporated with water vapor, so the ligustilide is seriously lost in the process of vacuum concentration. And if the concentrated solution is not added with aromatic water for spray drying, the spray dried powder basically does not contain ligustilide, so the invention collects the aromatic water simultaneously in the extraction process, the concentrated solution and the aromatic water are mixed and then are spray dried, the liquid material is sprayed into superfine fog-like liquid drops by utilizing the action of a sprayer, and the liquid drops are quickly vaporized to form the dry powder in a very short time when being contacted with hot air. In the drying process, the temperature of the air flow is 150-180 ℃ higher than the boiling point of water, the water in each liquid drop is evaporated in a short retention time, and the boiling point of the ligustilide is 377.9 ℃ higher than the boiling point of water, so that most of the ligustilide is solidified and stored in the spray-dried powder in the spray-drying process, the retention rate exceeds 40%, and the angelica and astragalus blood-enriching decoction granules are guaranteed to effectively exert clinical curative effect.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive effort, which would fall within the scope of the present invention.
Claims (10)
1. A preparation method of angelica sinensis and astragalus membranaceus blood replenishing particles is characterized by comprising the following steps:
(1) soaking radix astragali decoction pieces and radix Angelicae sinensis in water, reflux extracting, and collecting aromatic water during extraction process to obtain extractive solution and aromatic water;
(2) concentrating the extract under reduced pressure to obtain concentrated solution;
(3) uniformly mixing the concentrated solution and aromatic water, and spray-drying to obtain spray-dried powder;
(4) and mixing the spray-dried powder and the auxiliary materials uniformly, and performing dry granulation to obtain the angelica sinensis and astragalus membranaceus blood replenishing granules.
2. The method for preparing the angelica sinensis and astragalus membranaceus blood-enriching particles as claimed in claim 1, wherein in the step (2), the relative density of the concentrated solution is 1.07-1.20 g/ml at 60 ℃.
3. The method for preparing angelica sinensis and astragalus membranaceus blood-enriching particles according to claim 1, wherein in the step (3), the ratio of the concentrated solution to the aromatic water is 1:1 by weight.
4. The preparation method of the angelica sinensis and astragalus membranaceus blood-enriching particles as claimed in claim 1, wherein in the step (1), water with the amount 7-8 times of the total feeding amount is added according to the weight ratio to soak for 25-35 minutes, and the reflux extraction is performed for 1-2 hours to obtain an extracting solution and aromatic water.
5. The method for preparing angelica sinensis and astragalus membranaceus blood-enriching particles according to claim 4, wherein in the step (1), the aromatic water accounts for 3.5% -7% of the added water according to the weight ratio.
6. The method for preparing angelica sinensis and astragalus membranaceus blood-enriching particles according to claim 1, wherein in the step (3), the spray drying process parameters are as follows: the air inlet temperature is 150-180 ℃, and the air outlet temperature is 80-90 ℃.
7. The angelica and astragalus membranaceus blood-enriching particle is prepared by the preparation method of the angelica and astragalus membranaceus blood-enriching particle as claimed in any one of claims 1 to 6, raw materials of the angelica and astragalus membranaceus blood-enriching particle comprise astragalus membranaceus decoction pieces, wine-processed angelica sinensis and auxiliary materials, and the mass ratio of the astragalus membranaceus decoction pieces to the wine-processed angelica sinensis is 5: 1;
the grain diameters of the astragalus membranaceus decoction pieces and the wine angelica sinensis are respectively 4-24 meshes.
8. The angelica and astragalus hematinic granule of claim 7 wherein the excipient comprises maltodextrin, micronized silica gel and magnesium stearate.
9. The angelica sinensis astragalus membranaceus hematinic particle according to claim 8, wherein in the step (4), the addition weight of the maltodextrin is 12% -40% of the weight of the spray-dried powder;
the adding weight of the micro-powder silica gel is 0.5 to 1.0 percent of the weight of the spray-dried powder;
the addition weight of the magnesium stearate is 0.3-0.5% of the weight of the spray-dried powder.
10. The angelica and astragalus membranaceus blood-enriching particle as claimed in claim 7, wherein the particle size of the angelica and astragalus membranaceus blood-enriching particle is 16-40 meshes.
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