CN111956703A - Preparation method of Zhengyuan capsule dry paste powder - Google Patents
Preparation method of Zhengyuan capsule dry paste powder Download PDFInfo
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Abstract
The application provides a preparation method of vital essence capsule dry paste powder. The preparation method of the Zhengyuan capsule dry paste powder comprises the following steps: mixing the extract, the mixed extract and the inclusion compound of the glossy privet fruit, and then carrying out cutting and crushing operation to obtain a cut crushed product; carrying out low-temperature drying operation on the cut and crushed object, and carrying out primary grinding and crushing operation to obtain a ground and crushed object; freeze drying the ground material, and grinding and pulverizing for the second time to obtain Zhengyuan capsule dry extract powder. In the preparation method of the vital essence capsule dry paste powder, the low-temperature drying operation, the primary grinding and crushing operation, the freeze drying operation and the secondary grinding and crushing operation are adopted, so that the risk of damaging the effective components of the traditional Chinese medicine herbs in the vital essence capsule dry paste powder is reduced under the condition of ensuring that the vital essence capsule dry paste powder has a good dispersion effect.
Description
Technical Field
The invention relates to the technical field of dry paste powder, in particular to a preparation method of vital essence capsule dry paste powder.
Background
At present, the method for treating malignant tumor mainly comprises three therapies of surgery, chemotherapy and radiotherapy, the chemotherapy and the radiotherapy have obvious relieving effect on malignant tumor, but have serious defects, such as low selectivity, narrow safety range, close to toxic dose, inhibition or killing effect on malignant tumor cells, great sequential injury on normal tissues, especially rapidly-proliferating cell groups such as hematopoietic tissues, immune organs and the like, and reduction of leucocytes and low immune function caused by the normal tissues become main limiting factors of radiotherapy and chemotherapy. A plurality of researches show that when patients with malignant tumors receive radiotherapy and chemotherapy, the traditional Chinese medicine body resistance strengthening treatment is adopted, so that the toxic and side effects of the radiotherapy and the chemotherapy can be relieved, the number of leucocytes is increased, the immunologic function is improved, the patients can successfully complete the course of treatment, the life quality is improved, the treatment effect is improved, and the service life of the patients is prolonged.
In order to reduce the toxic and side effects of patients after radiotherapy and chemotherapy, the Zhengyuan capsule and the preparation process thereof provide a novel pure traditional Chinese medicine capsule preparation which has the advantages of precise medicine selection, scientific compatibility, remarkable auxiliary effect and convenient oral administration for patients with toxic and side effects after radiotherapy and chemotherapy, and adopt the modern traditional Chinese medicine production process to integrate the effective components of the medicinal materials in the formula into a whole, better embody the overall concept and treatment principle of the traditional Chinese medicine, have the effects of synergism and toxicity reduction after the patients are taken together with the chemotherapy and the chemotherapy, particularly obviously improve the clinical symptoms of the tumor kidney qi deficiency syndrome, protect white blood cells, increase the weight of the patients and improve the immunity and the survival quality of the patients.
Through long-term application and continuous improvement, the functions of all the medicines in the prescription are complemented, the functions of tonifying qi, strengthening spleen, tonifying kidney and replenishing essence are realized together, the symptoms of mental fatigue, hypodynamia, qi deficiency, disinclination to speaking, shortness of breath, baldness, waist soreness, back pain, spontaneous perspiration and the like of patients can be improved, the toxic and side effects of the patients after radiotherapy and chemotherapy are relieved, and the immunologic function and the life quality are improved. In the preparation process of the traditional Chinese medicine capsule, an extraction part adopts an alcohol extraction method, a volatile oil extraction method and a water decoction method, so that fat-soluble ingredients, volatile oil and water-soluble active ingredients in the medicines can be effectively extracted, a drying part adopts a spray drying technology, the quality of an intermediate product is stable and controllable, the process technology is standard, the extraction rate of the active ingredients is high, and a finished product is safe, free of toxic and side effects, convenient to carry and convenient to take.
The vital essence capsule is prepared from the following raw material medicines in parts by weight: 24-48 parts of epimedium, 6-10 parts of ginseng, 24-48 parts of radix astragali preparata and 16-32 parts of wine-processed glossy privet fruit.
The main components of the Zhengyuan capsule are basically extracted from the traditional Chinese medicinal herbs, so that the medicinal effect stability of the Zhengyuan capsule is very dependent on the quality of dry extract powder extracted from the traditional Chinese medicinal herbs, and the existing preparation method of the dry extract powder of the Zhengyuan capsule still has the risk that the effective components of the traditional Chinese medicinal herbs are easily damaged.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a Zhengyuan capsule dry paste powder capable of reducing the risk of damaging the effective components of Chinese herbal medicine raw materials of the Zhengyuan capsule.
The purpose of the invention is realized by the following technical scheme: a preparation method of Zhengyuan capsule dry paste powder comprises the following steps:
providing the following components in parts by mass: 24 to 48 parts of epimedium, 6 to 10 parts of ginseng, 24 to 48 parts of radix astragali preparata, 16 to 32 parts of glossy privet fruit, 4 to 8 parts of tortoise powder, 8 to 16 parts of turtle powder, 16 to 32 parts of fried bighead atractylodes rhizome and 8 to 16 parts of dried orange peel;
crushing the glossy privet fruit to obtain glossy privet fruit fine powder, adding ethanol to perform reflux extraction, and then performing first concentration operation to obtain glossy privet fruit extract;
mixing parched Atractylodis rhizoma and pericarpium Citri Tangerinae, adding pure water, decocting with water, and collecting volatile oil, first water extractive solution and first residue;
clathrating the volatile oil with hydroxypropyl beta-cyclodextrin to obtain clathrate;
mixing the epimedium, the ginseng, the astragalus and the first decoction dregs to obtain a mixture, then carrying out decoction operation, and then carrying out second concentration operation to obtain a mixed extract;
mixing the extract of glossy privet fruit, the mixed extract and the inclusion compound, and then cutting and crushing the mixture to obtain cut and crushed materials;
carrying out low-temperature drying operation on the cut and crushed object, and carrying out primary grinding and crushing operation to obtain a ground and crushed object; and
and (3) freeze-drying the ground and crushed material, and then carrying out secondary grinding and crushing operation to obtain the vital essence capsule dry paste powder.
In one embodiment, after the glossy privet fruit is crushed, the glossy privet fruit fine powder is screened by a 24-mesh screen.
In one embodiment, the reflux extraction operation by adding ethanol specifically includes the following steps:
adding 10 times (ml/g) of 75% (volume concentration) ethanol into the glossy privet fruit fine powder, carrying out first reflux extraction for 2 hours, and then carrying out first filtration operation to obtain first medicine residues and a first ethanol extracting solution;
adding 8 times (ml/g) of 70% (volume concentration) ethanol into the primary medicine residue, performing secondary reflux extraction for 1.5 hours, and performing secondary filtration operation to obtain secondary medicine residue and secondary ethanol extract;
adding 6 times (ml/g) of 85% (volume concentration) ethanol into the secondary residue, reflux-extracting for three times for 0.5 hr, and filtering for three times to obtain tertiary residue and tertiary ethanol extractive solution.
In one embodiment, the first concentrating operation specifically includes the following steps:
mixing the primary ethanol extract, the secondary ethanol extract and the tertiary ethanol extract to obtain a mixed ethanol extract;
and carrying out reduced pressure distillation and concentration operation on the mixed ethanol extract, and carrying out recovery operation on the volatilized ethanol to obtain the wine glossy privet fruit extract, wherein the relative density of the wine glossy privet fruit extract is 1.30-1.35 (measured at 50 ℃).
In one embodiment, in the inclusion operation, the inclusion operation is performed at a temperature of 50 to 60 degrees celsius;
the time of the inclusion operation is 2.5 to 3.5 hours.
In one embodiment, the decoction operation specifically comprises the following steps:
adding 8 times (ml/g) of pure water to the mixture, boiling for 1 hour, and performing a first filtration operation to obtain a second residue and a second water extract;
adding 6 times (ml/g) of pure water into the second decoction dregs, decocting for 5 hours at the temperature of 60-75 ℃, and then carrying out second filtering operation to obtain third decoction dregs and a third water extracting solution;
adding 2 times (ml/g) of pure water into the third decoction dregs, decocting for 2 hours at the temperature of 35-50 ℃, and then carrying out third filtration operation to obtain a fourth decoction dregs and a fourth water extracting solution.
In one embodiment, the second concentrating operation specifically includes the following steps:
mixing the first water extracting solution, the second water extracting solution and the third water extracting solution to obtain mixed water extracting solution;
and carrying out reduced pressure distillation and concentration operation on the mixed water extract to obtain a mixture extract, wherein the relative density of the mixture extract is 1.04-1.08 (measured at 50 ℃).
In one embodiment, the low-temperature drying operation is performed at 35-50 ℃;
and the low-temperature drying operation is carried out in a closed environment.
In one embodiment, the mass ratio of the volatile oil to the hydroxypropyl beta-cyclodextrin is 1: (7-9).
In one embodiment, the water content of the vital capsules is 3 to 5 percent.
Compared with the prior art, the application at least comprises the following advantages:
in the preparation method of the Zhengyuan capsule dry paste powder, low-temperature drying operation, primary grinding and crushing operation, freeze drying and secondary grinding and crushing operation are adopted, so that the risk of damaging the effective components of the traditional Chinese medicine herbs in the Zhengyuan capsule dry paste powder is reduced under the condition of ensuring that the Zhengyuan capsule dry paste powder has a good dispersion effect.
Drawings
Fig. 1 is a flow chart of the steps of a preparation method of zhengyuan capsule dry paste powder according to an embodiment of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The application provides a preparation method of vital essence capsule dry paste powder, which comprises the following steps: providing the following components in parts by mass: 24 to 48 parts of epimedium, 6 to 10 parts of ginseng, 24 to 48 parts of radix astragali preparata, 16 to 32 parts of glossy privet fruit, 4 to 8 parts of tortoise powder, 8 to 16 parts of turtle powder, 16 to 32 parts of fried bighead atractylodes rhizome and 8 to 16 parts of dried orange peel; crushing the glossy privet fruit to obtain glossy privet fruit fine powder, adding ethanol to perform reflux extraction, and then performing first concentration operation to obtain glossy privet fruit extract; mixing parched Atractylodis rhizoma and pericarpium Citri Tangerinae, adding pure water, decocting with water, and collecting volatile oil, first water extractive solution and first residue; clathrating the volatile oil with hydroxypropyl beta-cyclodextrin to obtain clathrate; mixing the epimedium, the ginseng, the astragalus and the first decoction dregs to obtain a mixture, then carrying out decoction operation, and then carrying out second concentration operation to obtain a mixed extract; mixing the extract, the mixed extract and the inclusion compound of the glossy privet fruit, and then carrying out cutting and crushing operation to obtain a cut crushed product; carrying out low-temperature drying operation on the cut and crushed object, and carrying out primary grinding and crushing operation to obtain a ground and crushed object; freeze drying the ground material, and grinding and pulverizing for the second time to obtain Zhengyuan capsule dry extract powder.
In the preparation method of the vital essence capsule dry paste powder, the low-temperature drying operation, the primary grinding and crushing operation, the freeze drying operation and the secondary grinding and crushing operation are adopted, so that the risk of damaging the effective components of the traditional Chinese medicine herbs in the vital essence capsule dry paste powder is reduced under the condition of ensuring that the vital essence capsule dry paste powder has a good dispersion effect.
In order to better understand the preparation method of the zhengyuan capsule dry extract powder of the present application, the preparation method of the zhengyuan capsule dry extract powder of the present application is further explained below, and referring to fig. 1, the preparation method of the zhengyuan capsule dry extract powder of one embodiment includes the following steps:
s100, providing the following components in parts by mass: 24 to 48 parts of epimedium, 6 to 10 parts of ginseng, 24 to 48 parts of radix astragali preparata, 16 to 32 parts of glossy privet fruit, 4 to 8 parts of tortoise powder, 8 to 16 parts of turtle powder, 16 to 32 parts of fried bighead atractylodes rhizome and 8 to 16 parts of dried orange peel. It can be understood that in the process of preparing the Zhengyuan capsule dry paste powder, the preparation of each component is needed, the omission of substances is avoided, the back-and-forth movement is reduced, and the preparation efficiency of the Zhengyuan capsule dry paste powder is improved.
S200, crushing the wine glossy privet fruit to obtain fine wine glossy privet fruit powder, adding ethanol to perform reflux extraction, and then performing first concentration operation to obtain a wine glossy privet fruit extract. The method has the advantages that the glossy privet fruit is crushed into fine glossy privet fruit powder, so that the leaching of active ingredients is facilitated, the leaching rate of ethanol on the glossy privet fruit is high, the extraction of the active ingredients of the glossy privet fruit is facilitated, and the content of the active ingredients of the glossy privet fruit in the vital capsule dry extract powder is increased.
S300, mixing the fried bighead atractylodes rhizome and the dried orange peel, adding pure water to carry out water decoction operation, and collecting volatile oil, a first water extracting solution and first medicine residues. The volatile oil in the fried bighead atractylodes rhizome and the dried orange peel is soluble in water and is volatile after heating, the volatile oil can be fully separated from the residual active ingredients of the fried bighead atractylodes rhizome and the dried orange peel through water decoction, and the volatile oil is volatile after heating, so that the volatile oil is separated and stored firstly, the loss problem of the volatile oil is avoided, and the content of the active ingredients of the fried bighead atractylodes rhizome and the dried orange peel in the vital essence capsule dry paste powder is improved.
S400, performing inclusion operation on the volatile oil by adopting hydroxypropyl beta-cyclodextrin to obtain an inclusion compound. It can be understood that the volatile oil is volatile when heated, even if the volatile oil is stored separately, the volatile oil still volatilizes in the high-temperature drying process, so that the volatile oil is subjected to inclusion operation by adopting hydroxypropyl beta-cyclodextrin to obtain an inclusion compound, the loss of the volatile oil in the high-temperature drying process is reduced, and the contents of the active ingredients of the fried bighead atractylodes rhizome and the dried orange peel in the vital essence capsule dry paste powder are increased. It can also be understood that the hydroxyl group of the hydroxypropyl beta-cyclodextrin and the volatile oil in the fried bighead atractylodes rhizome and the dried orange peel are easy to generate hydrogen bonds, and the inclusion rate and the stability of the volatile oil in the fried bighead atractylodes rhizome and the dried orange peel are improved.
S500, mixing the epimedium herb, the ginseng, the astragalus membranaceus and the first decoction dregs to obtain a mixture, then carrying out decoction operation, and then carrying out second concentration operation to obtain a mixed extract. It can be understood that the first medicine residue also contains a large amount of active ingredients of the fried rhizoma atractylodis macrocephalae and the dried orange peel, so that the first medicine residue is continuously added into the epimedium, the ginseng and the astragalus root for extracting the active ingredients, and the content of the active ingredients in the vital essence capsule dry paste powder is improved.
S600, mixing the wine and glossy privet fruit extract, the mixed extract and the inclusion compound, and then cutting and crushing the mixture to obtain a cut and crushed product. It can be understood that the alcohol glossy privet fruit extract and the mixed extract are sticky substances, the alcohol glossy privet fruit extract, the mixed extract and the inclusion compound are difficult to be uniformly mixed, the cutting and crushing operation is adopted to improve the mixing uniformity and the dispersion degree of the alcohol glossy privet fruit extract, the mixed extract and the inclusion compound, and further improve the quality of the vital essence capsule dry extract powder. It can also be understood that if the dispersion degree of the alcohol glossy privet fruit extract, the mixed extract and the inclusion compound is poor, the alcohol glossy privet fruit extract, the mixed extract and the inclusion compound are difficult to dry, and the condition of local drying or local wetting is formed, so that the problem of poor quality of the vital essence capsule dry extract powder is caused.
And S700, carrying out low-temperature drying operation on the cut crushed material, and carrying out primary grinding and crushing operation to obtain the ground crushed material. It can be understood that the low-temperature drying operation is carried out under the vacuum drying condition, the risk of damaging the effective components of the Chinese herbal medicine raw materials of the vital essence capsule is reduced, the volatilization of part of volatile oil which does not form inclusion compound is reduced, and the content of the effective components of the dry paste powder of the vital essence capsule is further improved. It can also be understood that the purpose of performing low-temperature drying operation before freeze drying is to reduce the moisture in the extract, mixed extract and inclusion compound of glossy privet fruit, and avoid the moisture from being cooled to shoulder height and being frozen at low temperature to form a block, so that the moisture in the block is difficult to volatilize, and the freeze drying efficiency is reduced.
And S800, freeze-drying the ground and crushed material, and then carrying out secondary grinding and crushing operation to obtain the vital essence capsule dry paste powder. It can be understood that the freeze drying is to directly volatilize the frozen ice into water vapor to remove under the vacuum condition, thereby reducing the risk that the effective components of the traditional Chinese medicine herb are easily damaged and avoiding the reduction problem of the volatile oil of the vital essence capsule dry extract powder.
In the preparation method of the vital essence capsule dry paste powder, the low-temperature drying operation, the primary grinding and crushing operation, the freeze drying operation and the secondary grinding and crushing operation are adopted, so that the risk of damaging the effective components of the traditional Chinese medicine herbs in the vital essence capsule dry paste powder is reduced under the condition of ensuring that the vital essence capsule dry paste powder has a good dispersion effect.
In one embodiment, after the glossy privet fruit is crushed, the glossy privet fruit fine powder is screened by a 24-mesh screen. It can be understood that the glossy privet fruit fine powder obtained by the screening operation of the 24-mesh screen is not easy to generate the condition of dust flying, and is easy to extract to obtain the effective components of the glossy privet fruit, so that the content of the effective components of the glossy privet fruit in the vital essence capsule dry extract powder is improved, and the preparation efficiency of the vital essence capsule dry extract powder is improved.
In one embodiment, the reflux extraction with ethanol comprises the following steps:
adding 10 times (ml/g) of 75% (volume concentration) ethanol into the fine powder of fructus Ligustri Lucidi, reflux extracting for 2 hr, and filtering to obtain first residue and first ethanol extractive solution. It can be understood that in the first reflux extraction, the content of the effective components in the glossy privet fruit fine powder is higher, the content of ethanol needs to be increased to leach the effective components in the glossy privet fruit fine powder, and the leaching time needs to be prolonged, so that 10 times (ml/g) of 75% (volume concentration) ethanol is added into the glossy privet fruit fine powder, the first reflux extraction is carried out for 2 hours, and the leaching efficiency of the effective components in the glossy privet fruit fine powder is improved.
Further, 8 times (ml/g) of 70% (volume concentration) ethanol was added to the primary residue, and the mixture was subjected to secondary reflux extraction for 1.5 hours, followed by secondary filtration to obtain secondary residue and a secondary ethanol extract. It can be understood that in the secondary reflux extraction, the content of the active ingredients in the glossy privet fruit fine powder is relatively low, but the content is still high, the content of ethanol needs to be increased to carry out the active ingredient leaching on the glossy privet fruit fine powder, but the leaching time can be properly reduced, so that 8 times (ml/g) of ethanol with the concentration of 70 percent (volume concentration) is added into the primary medicine residue, the secondary reflux extraction is carried out for 1.5 hours, and the leaching efficiency of the active ingredients of the glossy privet fruit fine powder is improved.
Further, 6 times (ml/g) of 85% (volume concentration) ethanol was added to the second residue, and the mixture was subjected to reflux extraction for three times for 0.5 hour, followed by filtration for three times to obtain the third residue and the third ethanol extract. It can be understood that, in the three times of reflux extraction, the content of the effective components in the glossy privet fruit fine powder is relatively less than that of the effective components in the glossy privet fruit fine powder, and the actual content is also less, so that the content of ethanol needs to be reduced, and the extraction time needs to be reduced, therefore, 6 times (ml/g) of ethanol with the concentration of 85% (volume concentration) is added into the secondary medicine residue, and the three times of reflux extraction is carried out for 0.5 hours, so that the extraction efficiency of the effective components in the glossy privet fruit fine powder is improved.
The first reflux extraction, the second reflux extraction and the third reflux extraction are arranged, so that the leaching efficiency of the effective components in the glossy privet fruit fine powder is improved. If only the first reflux extraction is carried out, or only the first reflux extraction and the second reflux extraction are carried out, the content of the effective components in the glossy privet fruit fine powder is reduced. It can be understood that, during the three-reflux extraction, the residual content of the active ingredients of the glossy privet fruit fine powder is very small, the concentration of the active ingredients of the glossy privet fruit fine powder in the secondary ethanol extraction solution is high, and the residual active ingredients of the glossy privet fruit fine powder are difficult to be continuously leached, so that three-time reflux extraction is needed, the concentration of the active ingredients of the glossy privet fruit fine powder in the three-time ethanol extraction solution is low, the leaching capacity of continuously leaching the residual active ingredients of the glossy privet fruit fine powder is realized, but after the extraction time is 0.5 hour, the content of the active ingredients of the glossy privet fruit fine powder in the three-time ethanol extraction solution is basically not changed, and therefore, the first reflux extraction.
In one embodiment, the first concentrating operation specifically comprises the following steps:
mixing the primary ethanol extract, the secondary ethanol extract and the tertiary ethanol extract to obtain a mixed ethanol extract.
Further, carrying out reduced pressure distillation and concentration operation on the mixed ethanol extract, and carrying out recovery operation on the volatilized ethanol to obtain the alcohol-treated fructus ligustri lucidi extract, wherein the relative density of the alcohol-treated fructus ligustri lucidi extract is 1.30-1.35 (measured at 50 ℃). It can be understood that the mixed ethanol extract contains a large amount of ethanol, the mixed ethanol extract needs to be subjected to reduced pressure distillation and concentration operation, on one hand, the water content in the alcohol glossy privet fruit extract is reduced, on the other hand, the impurity content of the Zhengyuan capsule dry extract powder is reduced for removing the ethanol, and when the relative density of the alcohol glossy privet fruit extract is 1.30-1.35 (measured at 50 ℃), the alcohol glossy privet fruit extract is favorably mixed with the mixture extract and the clathrate compound.
In one embodiment, in the inclusion operation, the inclusion operation is performed at a temperature of 50 to 60 degrees celsius. It can be understood that the inclusion operation of the volatile oil is carried out at the temperature of 50-60 ℃, so that the inclusion rate of the volatile oil is improved, and the content of effective components of the vital essence capsule dry paste powder is further improved.
In one embodiment, the time for the inclusion operation is 2.5 hours to 3.5 hours. It can be understood that the time of the inclusion operation is 2.5 hours to 3.5 hours, the inclusion rate of the volatile oil is improved, and the content of the effective components of the vital essence capsule dry extract powder is further improved.
In one embodiment, the decoction operation specifically comprises the steps of:
to the mixture was added 8 times (ml/g) the amount of pure water, boiled for 1 hour, and then subjected to a first filtration operation to obtain a second residue and a second aqueous extract. It can be understood that the content of each effective component in the mixture is high, the content of pure water needs to be increased for effective component leaching, and the leaching time needs to be prolonged, so that the leaching efficiency of the effective components is improved by adding 8 times (ml/g) of pure water to the mixture and boiling for 1 hour.
Further, 6 times (ml/g) of pure water was added to the second residue, and the mixture was decocted at 60 to 75 ℃ for 5 hours, followed by a second filtration operation to obtain a third residue and a third aqueous extract. It can be understood that in the secondary reflux extraction, the content of the active ingredients in the second herb residue is relatively low, but still high, and the content of the pure water needs to be increased for leaching the active ingredients, but the leaching time can be properly reduced, so that the leaching efficiency of the active ingredients is improved by adding 6 times (ml/g) of the pure water into the second herb residue and decocting the mixture for 5 hours at the temperature of between 60 and 75 ℃.
Further, 2 times (ml/g) of pure water was added to the third residue, and the mixture was decocted at 35 to 50 ℃ for 2 hours, followed by a third filtration operation to obtain a fourth residue and a fourth aqueous extract. It can be understood that the content of the effective components in the third herb residue is relatively low, the actual content is also low, so that the content of pure water needs to be reduced, and the extraction time needs to be reduced, so that 2 times (ml/g) of pure water is added into the third herb residue, and the third herb residue is decocted for 2 hours at the temperature of 35-50 ℃, so that the extraction efficiency of the effective components in the wine glossy privet fruit fine powder is improved.
It is noted that the extraction efficiency of the effective components of the mixture is improved by decocting the mixture for three times to extract the effective components. If only one or two times of decoction is carried out, the content of the effective components of the mixture is reduced. It can be understood that, during the third decoction extraction, the residual content of the effective components of the mixture is very small, and at the moment, the concentration of the effective components of the mixture in the three-water extracting solution is high, and the residual effective components of the mixture are difficult to be leached continuously, so that the three decoction extractions are needed, the concentration of the effective components of the mixture in the third decoction extraction is low, and the mixture has the capability of continuously leaching the effective components of the mixture, but after the extraction time is 5 hours, the content of the effective components of the mixture in the third decoction extraction solution is basically not changed, so that the three decoction extractions are arranged, and the leaching efficiency of the effective components of the mixture is favorably.
In one embodiment, the second concentration operation specifically comprises the following steps:
and mixing the first water extracting solution, the second water extracting solution and the third water extracting solution to obtain a mixed water extracting solution.
Further, carrying out reduced pressure distillation and concentration operation on the mixed water extract to obtain a mixture extract, wherein the relative density of the mixture extract is 1.04-1.08 (measured at 50 ℃). And (3) carrying out reduced pressure distillation and concentration operation on the mixed water extract, reducing the water content of the mixture extract, and when the relative density of the mixture extract is 1.04-1.08 (measured at 50 ℃), being beneficial to mixing the mixture extract with the alcohol glossy privet fruit extract and the inclusion compound.
In one embodiment, the low-temperature drying operation is carried out at the temperature of 35-50 ℃;
and the low-temperature drying operation is carried out in a closed environment. It will be appreciated that the low temperature drying operation is conducted in a closed environment to facilitate a reduction in the amount of volatile oils that are not included.
In one embodiment, the mass ratio of the volatile oil to the hydroxypropyl beta-cyclodextrin is 1: (7-9). It can be understood that the mass ratio of the volatile oil to the hydroxypropyl beta-cyclodextrin is 1: (7-9), the inclusion rate of the volatile oil is improved, and the content of effective components in the vital essence capsule dry paste powder is further improved.
In one embodiment, the water content of the vital capsules is 3% to 5%. It can be understood that when the water content of the vital essence capsule dry powder paste is 3% -5%, the vital essence capsule dry powder paste has relatively uniform particle size distribution, and the moisture absorption of the vital essence capsule dry powder paste is relatively poor.
Compared with the prior art, the application at least comprises the following advantages:
in the preparation method of the Zhengyuan capsule dry paste powder, low-temperature drying operation, primary grinding and crushing operation, freeze drying and secondary grinding and crushing operation are adopted, so that the risk of damaging the effective components of the traditional Chinese medicine herbs in the Zhengyuan capsule dry paste powder is reduced under the condition of ensuring that the Zhengyuan capsule dry paste powder has a good dispersion effect.
The following examples are given by way of illustration, and it is noted that the following examples are not intended to be exhaustive of all possible and that the materials used in the following examples are commercially available without specific recitation.
Example 1
A preparation method of Zhengyuan capsule dry paste powder comprises the following steps:
providing the following components in parts by mass: 48kg of epimedium, 10kg of ginseng, 48kg of radix astragali preparata, 32kg of wine-processed glossy privet fruit, 8kg of tortoise powder, 16kg of turtle powder, 32kg of fried bighead atractylodes rhizome and 16kg of dried orange peel;
crushing the glossy privet fruit to obtain glossy privet fruit fine powder, adding ethanol to perform reflux extraction, and then performing first concentration operation to obtain glossy privet fruit extract;
mixing parched Atractylodis rhizoma and pericarpium Citri Tangerinae, adding pure water, decocting with water, and collecting volatile oil, first water extractive solution and first residue;
clathrating the volatile oil with hydroxypropyl beta-cyclodextrin at 60 deg.C for 3.5 hr to obtain clathrate;
mixing the epimedium, the ginseng, the astragalus and the first decoction dregs to obtain a mixture, then carrying out decoction operation, and then carrying out second concentration operation to obtain a mixed extract;
mixing the extract, the mixed extract and the inclusion compound of the glossy privet fruit, and then carrying out cutting and crushing operation to obtain a cut crushed product;
carrying out low-temperature drying operation on the cut crushed material at the temperature of 50 ℃, and carrying out primary grinding and crushing operation to obtain ground crushed material; and
freeze drying the ground material, and grinding and pulverizing for the second time to obtain Zhengyuan capsule dry extract powder.
Example 2
A preparation method of Zhengyuan capsule dry paste powder comprises the following steps:
providing the following components in parts by mass: 36kg of epimedium, 8kg of ginseng, 36kg of radix astragali preparata, 24kg of wine-processed glossy privet fruit, 6kg of tortoise powder, 12kg of turtle powder, 24kg of fried bighead atractylodes rhizome and 12kg of dried orange peel;
crushing the glossy privet fruit to obtain glossy privet fruit fine powder, adding ethanol to perform reflux extraction, and then performing first concentration operation to obtain glossy privet fruit extract;
mixing parched Atractylodis rhizoma and pericarpium Citri Tangerinae, adding pure water, decocting with water, and collecting volatile oil, first water extractive solution and first residue;
clathrating the volatile oil with hydroxypropyl beta-cyclodextrin at 55 deg.C for 3 hr to obtain clathrate;
mixing the epimedium, the ginseng, the astragalus and the first decoction dregs to obtain a mixture, then carrying out decoction operation, and then carrying out second concentration operation to obtain a mixed extract;
mixing the extract, the mixed extract and the inclusion compound of the glossy privet fruit, and then carrying out cutting and crushing operation to obtain a cut crushed product;
carrying out low-temperature drying operation on the cut crushed material at 42 ℃, and carrying out primary grinding and crushing operation to obtain ground crushed material; and
freeze drying the ground material, and grinding and pulverizing for the second time to obtain Zhengyuan capsule dry extract powder.
Example 3
A preparation method of Zhengyuan capsule dry paste powder comprises the following steps:
providing the following components in parts by mass: 24kg of epimedium, 6kg of ginseng, 24kg of radix astragali preparata, 16kg of wine-processed glossy privet fruit, 4kg of tortoise powder, 8kg of turtle powder, 16kg of fried bighead atractylodes rhizome and 8kg of dried orange peel;
crushing the glossy privet fruit to obtain glossy privet fruit fine powder, adding ethanol to perform reflux extraction, and then performing first concentration operation to obtain glossy privet fruit extract;
mixing parched Atractylodis rhizoma and pericarpium Citri Tangerinae, adding pure water, decocting with water, and collecting volatile oil, first water extractive solution and first residue;
clathrating the volatile oil with hydroxypropyl beta-cyclodextrin at 50 deg.C for 2.5 hr to obtain clathrate;
mixing the epimedium, the ginseng, the astragalus and the first decoction dregs to obtain a mixture, then carrying out decoction operation, and then carrying out second concentration operation to obtain a mixed extract;
mixing the extract, the mixed extract and the inclusion compound of the glossy privet fruit, and then carrying out cutting and crushing operation to obtain a cut crushed product;
carrying out low-temperature drying operation on the cut crushed material at 35 ℃, and carrying out primary grinding and crushing operation to obtain ground crushed material; and
freeze drying the ground material, and grinding and pulverizing for the second time to obtain Zhengyuan capsule dry extract powder.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of vital essence capsule dry paste powder is characterized by comprising the following steps:
providing the following components in parts by mass: 24 to 48 parts of epimedium, 6 to 10 parts of ginseng, 24 to 48 parts of radix astragali preparata, 16 to 32 parts of glossy privet fruit, 4 to 8 parts of tortoise powder, 8 to 16 parts of turtle powder, 16 to 32 parts of fried bighead atractylodes rhizome and 8 to 16 parts of dried orange peel;
crushing the glossy privet fruit to obtain glossy privet fruit fine powder, adding ethanol to perform reflux extraction, and then performing first concentration operation to obtain glossy privet fruit extract;
mixing parched Atractylodis rhizoma and pericarpium Citri Tangerinae, adding pure water, decocting with water, and collecting volatile oil, first water extractive solution and first residue;
clathrating the volatile oil with hydroxypropyl beta-cyclodextrin to obtain clathrate;
mixing the epimedium, the ginseng, the astragalus and the first decoction dregs to obtain a mixture, then carrying out decoction operation, and then carrying out second concentration operation to obtain a mixed extract;
mixing the extract of glossy privet fruit, the mixed extract and the inclusion compound, and then cutting and crushing the mixture to obtain cut and crushed materials;
carrying out low-temperature drying operation on the cut and crushed object, and carrying out primary grinding and crushing operation to obtain a ground and crushed object; and
and (3) freeze-drying the ground and crushed material, and then carrying out secondary grinding and crushing operation to obtain the vital essence capsule dry paste powder.
2. The method for preparing Zhengyuan capsule dry extract powder as claimed in claim 1, wherein the above-mentioned pulverizing process is followed by a 24 mesh sieve screening process.
3. The preparation method of the Zhengyuan capsule dry paste powder as claimed in claim 1, wherein the reflux extraction operation by adding ethanol specifically comprises the following steps:
adding 10 times (ml/g) of 75% (volume concentration) ethanol into the glossy privet fruit fine powder, carrying out first reflux extraction for 2 hours, and then carrying out first filtration operation to obtain first medicine residues and a first ethanol extracting solution;
adding 8 times (ml/g) of 70% (volume concentration) ethanol into the primary medicine residue, performing secondary reflux extraction for 1.5 hours, and performing secondary filtration operation to obtain secondary medicine residue and secondary ethanol extract;
adding 6 times (ml/g) of 85% (volume concentration) ethanol into the secondary residue, reflux-extracting for three times for 0.5 hr, and filtering for three times to obtain tertiary residue and tertiary ethanol extractive solution.
4. The method for preparing zheng yuan capsule dry paste powder as claimed in claim 3, wherein the first concentrating operation comprises the following steps:
mixing the primary ethanol extract, the secondary ethanol extract and the tertiary ethanol extract to obtain a mixed ethanol extract;
and carrying out reduced pressure distillation and concentration operation on the mixed ethanol extract, and carrying out recovery operation on the volatilized ethanol to obtain the wine glossy privet fruit extract, wherein the relative density of the wine glossy privet fruit extract is 1.30-1.35 (measured at 50 ℃).
5. The preparation method of Zhengyuan capsule dry paste powder according to claim 1, wherein in the inclusion operation, the inclusion operation is performed at a temperature of 50-60 ℃;
the time of the inclusion operation is 2.5 to 3.5 hours.
6. The preparation method of Zhengyuan capsule dry extract powder as claimed in claim 1, wherein the decoction specifically comprises the following steps:
adding 8 times (ml/g) of pure water to the mixture, boiling for 1 hour, and performing a first filtration operation to obtain a second residue and a second water extract;
adding 6 times (ml/g) of pure water into the second decoction dregs, decocting for 5 hours at the temperature of 60-75 ℃, and then carrying out second filtering operation to obtain third decoction dregs and a third water extracting solution;
adding 2 times (ml/g) of pure water into the third decoction dregs, decocting for 2 hours at the temperature of 35-50 ℃, and then carrying out third filtration operation to obtain a fourth decoction dregs and a fourth water extracting solution.
7. The method for preparing zheng yuan capsule dry paste powder as claimed in claim 6, wherein the second concentrating operation comprises the following steps:
mixing the first water extracting solution, the second water extracting solution, the third water extracting solution and the fourth water extracting solution to obtain mixed water extracting solution;
and carrying out reduced pressure distillation and concentration operation on the mixed water extract to obtain a mixture extract, wherein the relative density of the mixture extract is 1.04-1.08 (measured at 50 ℃).
8. The preparation method of Zhengyuan capsule dry paste powder according to claim 1, wherein the low-temperature drying operation is performed at 35-50 ℃;
and the low-temperature drying operation is carried out in a closed environment.
9. The preparation method of the vital essence capsule dry paste powder according to claim 1, wherein the mass ratio of the volatile oil to the hydroxypropyl beta-cyclodextrin is 1: (7-9).
10. The preparation method of the Zhengyuan capsule dry paste powder as claimed in claim 1, wherein the water content of the Zhengyuan capsule dry paste powder is 3-5%.
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