CN118416120A - Preparation method of semen trichosanthis paste powder and formula granules - Google Patents

Preparation method of semen trichosanthis paste powder and formula granules Download PDF

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CN118416120A
CN118416120A CN202410344646.5A CN202410344646A CN118416120A CN 118416120 A CN118416120 A CN 118416120A CN 202410344646 A CN202410344646 A CN 202410344646A CN 118416120 A CN118416120 A CN 118416120A
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semen trichosanthis
paste powder
semen
trichosanthis
preparing
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李争
廖明丽
李亚楠
张旭
郭天佑
刘良娟
张诗华
高晗
李军山
姜国志
李振江
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Shenwei Pharmaceutical Group Co Ltd
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Shenwei Pharmaceutical Group Co Ltd
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Abstract

The invention provides a preparation method of semen trichosanthis paste powder and formula particles, which belongs to the technical field of traditional Chinese medicine preparations, wherein semen trichosanthis is rolled into semen trichosanthis decoction pieces with the kernel breakage rate of 60-90%, and then the semen trichosanthis paste powder is prepared by circularly extracting, filtering, concentrating, filtering again, adding beta-cyclodextrin into the obtained concentrated solution, mixing uniformly, centrifugally emulsifying, adding an adhesive, mixing uniformly and drying; the semen trichosanthis formula particles are prepared by directly granulating semen trichosanthis paste powder by a dry method. The preparation method provided by the invention has the technical advantages of no need of separate extraction and separation of grease, high extraction rate, simplicity in operation, product stability, good solubility, easiness in granulation and the like, and meanwhile, the prepared semen trichosanthis paste powder and semen trichosanthis formula particles have the advantages of few auxiliary materials, small auxiliary material dosage, high safety, high content retention rate, good efficacy, good stability, long shelf life and the like.

Description

Preparation method of semen trichosanthis paste powder and formula granules
Technical Field
The invention relates to a method for clathrating grease, in particular to a method for preparing semen trichosanthis paste powder and formula particles.
Background
The traditional Chinese medicine formula granule is a traditional Chinese medicine granule for clinical prescription obtained by extracting single medicine with water, concentrating, drying and granulating. Among the common traditional Chinese medicines, few medicinal materials contain nonvolatile oil components, such as fructus cannabis, semen trichosanthis, semen pruni, semen coicis and the like. Semen Trichosanthis is dried mature seed of fructus Trichosanthis Trichosanthes kirilowii maxim or fructus Trichosanthis Trichosanthes rosthornii Harms of Cucurbitaceae, and has effects of moistening lung, resolving phlegm, and relaxing bowels. Semen Trichosanthis contains abundant oil components, and has strong antiinflammatory, anticancer, arteriosclerosis preventing, immunity enhancing, and blood lipid reducing effects. The existing technology for preparing formula particles by extracting and purifying semen trichosanthis oil mainly comprises two steps, namely, extracting and separating oil from semen trichosanthis medicinal materials independently, wherein the method can cause the oil to adhere to equipment in the stages of oil extraction and separation, so that the problem of low extraction rate is caused. The other method is that the conventional water extraction technology is adopted, grease is not separated independently, the obtained liquid medicine has grease floating, the grease is easy to adhere on equipment, the extraction efficiency is low, the influence of the pretreatment crushing degree of medicinal materials is large, the grease cannot be included independently, the difficulty of dry granulation of the obtained fatty oil is large, the finished product after granulation has large oiliness, poor powder chemical property, difficult granulation, poor dissolubility and poor product stability, and the long-term storage of the rancid smell is generated.
In the existing pretreatment crushing process of semen trichosanthis, the crushing granularity is not specified, which leads to large batch-to-batch difference in the subsequent extraction process, and the operation is performed all through experience. Even if the particle size is specified, no specific pretreatment operation is performed on the portion where the content index component exists. In addition, in the existing inclusion technology after separating grease components separately, the grease mostly adopts ethanol as a cosolvent, beta-cyclodextrin is used as an auxiliary material, a proper amount of water is added, the inclusion is carried out at a set temperature within a certain range, the inclusion liquid is dried at a low temperature, and the whole inclusion process needs ethanol, so that the quality of a finished product is reduced; or beta-cyclodextrin, povidone K30, polyvinylpyrrolidone (PVP), sodium carboxymethyl starch or dextrin are used as auxiliary materials, and the extract paste powder is obtained by independently clathrating and drying oil components, but the method can be adhered to equipment in the oil separation process to cause oil loss, and has the advantages of complex operation, higher equipment requirement and lower clathration rate in the clathration process.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of semen trichosanthis paste powder and formula particles.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method of semen trichosanthis paste powder comprises the steps of taking semen trichosanthis, rolling the semen trichosanthis into semen trichosanthis decoction pieces with kernel breakage rate of 60-90%, circularly extracting, filtering, concentrating, filtering again, adding beta-cyclodextrin into the obtained concentrated solution, mixing uniformly, centrifugally emulsifying, adding an adhesive, mixing uniformly, and drying to obtain the semen trichosanthis paste powder.
Furthermore, the seed coat breaking rate of the semen trichosanthis decoction pieces is 100%.
Further, the centrifugal emulsification is shearing, grinding and high-speed stirring by adopting a colloid mill.
Further, the weight ratio of the semen trichosanthis decoction pieces to the beta-cyclodextrin is 10-20:0.2-0.5.
Further, the weight ratio of the semen trichosanthis decoction pieces to the adhesive is 10-20: 0.25 to 0.7, preferably 10 to 20:0.25 to 0.698.
Further, the temperature of the cyclic extraction is 95-100 ℃ and the time is 0.5-1 h.
Further, after the concentration, the relative density of the obtained concentrated filtrate is 1.02-1.06 at 60 ℃.
Further, the adhesive is at least one of dextrin, povidone K30, polyvinylpyrrolidone and sodium carboxymethyl starch.
Further, in the cyclic extraction process, water is adopted as a solvent, wherein the weight-volume ratio of semen trichosanthis decoction pieces to water is 10-20 kg: 14-18L;
the pore diameters of the two filtering holes are 100-500 meshes.
The semen trichosanthis formula particle is prepared by directly granulating semen trichosanthis paste powder prepared by the preparation method without adding auxiliary materials such as glidants and the like by a dry method.
The preparation method of the semen trichosanthis paste powder and the formula particles has the beneficial effects that:
according to the preparation method, the snakegourd fruit medicinal material is flattened, the specific flattening proportion of the specific part of the snakegourd fruit medicinal material is regulated, and the experiential, standardization and datamation are removed from the pretreatment of the medicinal material, so that the pretreatment process of the snakegourd fruit medicinal material is more similar to the requirement of 'broken when necessary' required in the rule of making Chinese medicinal formula granule standards;
According to the preparation method, the semen trichosanthis medicinal material is flattened, and then the extraction efficiency of the fatty oil is obviously stabilized by a circulating extraction technology, the extraction efficiency of the fatty oil is maintained within a specific range, the condition that the later period is difficult to granulate caused by excessive extraction of the fatty oil in the extraction process is avoided, the different extraction batches are stable and easy to operate, the fatty oil is ensured not to be layered in the extracting solution and the concentrated solution, no oil flowers float, the adhesion of floating oil flowers on equipment caused by excessive extraction is avoided, the total fatty oil loss is small, and the semen trichosanthis paste powder prepared by inclusion of the fatty oil is almost free of oil; the prepared semen trichosanthis paste powder has good grease stability, and can avoid the generation of rancidity oil after long-term placement; the prepared semen trichosanthis paste powder has improved dissolubility, small powder oiliness and good fluidity, avoids paste powder from adhering to the wall of a spraying tower in the spraying process due to the oil passing of the paste powder, reduces the loss in the spraying process, has higher yield and better economic benefit, can be directly subjected to dry granulation, and has high granulation rate;
According to the preparation method, oil is not required to be squeezed independently, oil is not required to be extracted and separated independently, the oil is always in the liquid medicine through a circulating extraction technology, the obtained extracting solution and the concentrated solution are not layered, beta-cyclodextrin can be directly added into the concentrated solution for inclusion, the inclusion rate is high, the process operation is simple, the steps with large operation difficulty are omitted, and the requirement on equipment is low; meanwhile, the beta-cyclodextrin is added to effectively protect the content index component 3, 29-dibenzoyl trichosanthes kirilowii Maxim kernel triol, so that the content index component loss in the production process is reduced, the addition amount of granulating auxiliary materials is reduced, and the content of the content index component in the finished product is improved;
The preparation method provided by the invention has the technical advantages of no need of separate extraction and separation of grease, high extraction rate, simplicity in operation, product stability, good solubility, easiness in granulation and the like, and meanwhile, the prepared semen trichosanthis paste powder and semen trichosanthis formula particles also have the advantages of few auxiliary materials, small auxiliary material dosage, high safety, high content retention rate, good efficacy, good stability, long shelf life and the like;
the preparation method of the invention can directly add beta-cyclodextrin into the concentrated solution to pass through a colloid mill without separately adding inclusion operation.
Detailed Description
The following description of the technical solution in the embodiments of the present invention is clear and complete. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Example 1 preparation method of semen Trichosanthis paste powder and formulation granule
The embodiment is a preparation method of semen trichosanthis paste powder and formula particles, and the specific preparation process comprises the following steps:
s1, adjusting the distance between compression rollers at two sides of a flattening machine to be 0.1-0.3 cm (the distance between the compression rollers at two sides is 0.2cm in the embodiment), taking a proper amount of semen trichosanthis, passing through the flattening machine, rolling for 1-3 times, and rolling into semen trichosanthis decoction pieces with a seed coat breaking rate of 100% and a seed kernel breaking rate of 60%;
S2, adding 10-20 kg of semen trichosanthis decoction pieces with the skin breaking rate of 100% and the kernel breaking rate of 60% into a multifunctional extraction tank, adding 10kg of semen trichosanthis decoction pieces and 15L of drinking water in the embodiment, starting circulation, circularly extracting for 0.5-1 h at 95-100 ℃ (the temperature of the multifunctional extraction in the embodiment is 100 ℃ and the time is 1 h), filtering the obtained extract, sieving with a 100-500 mesh sieve (marked as a first sieving, sieving with a 200-mesh sieve in the embodiment), concentrating until the relative density of the obtained concentrated filtrate is 1.02-1.06 at 60 ℃ (the relative density of the obtained concentrated filtrate is 1.04 at 60 ℃ in the embodiment), and sieving with a 100-500-mesh sieve (marked as a second sieving, sieving with a 200-mesh sieve in the embodiment) to obtain the concentrated solution.
S3, adding 0.2-0.5 kg of beta-cyclodextrin (0.2 kg of beta-cyclodextrin is added in the embodiment) into the concentrated solution, stirring and mixing uniformly at room temperature (the stirring speed is 30-60 r/min and the stirring time is 7-15 min, the stirring speed is 40r/min and the stirring time is 7min in the embodiment), and performing centrifugal emulsification through a colloid mill by shearing, grinding and high-speed stirring to obtain a liquid medicine;
wherein the rotation speed of the colloid mill is 2200-3200 r/min, the emulsification fineness is 30-50 mu m, and the rotation speed of the colloid mill is 2530r/min and the emulsification fineness is 30 mu m in the embodiment.
S4, pumping the medicine liquid into a liquid preparation tank of a spray drying tower, adding 0.25-0.698 kg of dextrin as an adhesive (in the embodiment, adding 0.698kg of dextrin), stirring uniformly at room temperature (the stirring speed is 40-80 r/min and the stirring time is 1-3 h, the stirring speed is 50r/min and the stirring time is 1h in the embodiment), and performing spray drying granulation on the obtained paste powder aqueous solution to obtain 1.20kg of semen trichosanthis paste powder, wherein the mark is Y1.
S5, adopting semen trichosanthis paste powder Y1, directly granulating by a dry method without adding auxiliary materials such as a glidant and the like, and obtaining semen trichosanthis formula granules, wherein the granules are marked as G1, and the granulating rate is 99.2%.
In the present invention, the method for drying the aqueous solution of the paste powder is not particularly limited, and conventional methods for drying the aqueous solution may be selected, including but not limited to vacuum drying, spray drying, freeze drying, and the like, and will not be described herein.
Examples 2-5 preparation method of semen Trichosanthis paste powder and formulation granule
Examples 2 to 5 are the preparation methods of semen Trichosanthis paste powder and formulation granule, which have the same steps as example 1, except for the differences of the raw material amount and the technological parameters, and the specific details are shown in table 1:
Table 1 list of process parameters in examples 2 to 5
The contents of the other parts of examples 2 to 5 are the same as those of example 1, and will not be described again here.
The binder may be at least one of dextrin, povidone K30, polyvinylpyrrolidone (PVP) and sodium carboxymethyl starch, and is not limited to the above examples, but is not limited to the ratio in the above examples.
Experimental example 1 Experimental determination
Comparative examples 1 to 6 are comparative experiments of the preparation methods of the semen Trichosanthis paste powder and the formulation granule in example 1, and the same batch of semen Trichosanthis as the raw material in example 1, and the steps are basically the same as those in example 1, except that the raw material amounts and the process parameters are different, and the specific details are shown in table 2:
table 2 lists of Process parameters for comparative examples 1 to 6
Comparative example 7 is a comparative test of the preparation method of the semen Trichosanthis paste powder and the formulation granule in example 1, and the same batch of semen Trichosanthis as the raw material as in example 1 is adopted, except that dynamic extraction is adopted instead of cyclic extraction in comparative example 7, to obtain 1.766kg semen Trichosanthis paste powder, and marked as DY7. The semen trichosanthis formula particles are prepared by directly granulating semen trichosanthis paste powder DY7 in a dry method without adding auxiliary materials such as glidants, and the granulating rate is 95.2 percent, wherein the particles are marked as DG 7.
From the above comparative examples, it can be seen that varying the rate of kernel breakage, the amount of beta-cyclodextrin, the extraction mode and temperature and the relative density of the concentrated filtrate at 60 ℃ resulted in a different degree of granulation rate reduction.
Further, the content transfer rate and the repose angle of the 3, 29-dibenzoyl trichosanthes kirilowii kernel are measured as follows:
The 3, 29-dibenzoyl trichosanthes kirilowii Maxim kernel triol content, the content transfer rate and the repose angle in the trichosanthes kirilowii Maxim paste powder are respectively measured by taking the trichosanthes kirilowii Maxim formula particles Y1-Y5 and DY 1-DY 7 prepared in examples 1-5 and comparative examples 1-7.
The content determination method of 3, 29-dibenzoyl trichosanthes kirilowii Maxim kernel triol in the semen trichosanthis formula particles is determined according to the method recorded in semen trichosanthis of a part of medicinal materials and decoction pieces in Chinese pharmacopoeia (2020 edition); the repose angle is measured by adopting a fixed funnel method;
The content transfer rate is calculated by the following method, and the calculation formula is as follows:
Content transfer rate (%) =content of finished product (g/g) ×extract rate/medicinal material content×100%;
wherein, the paste yield of the above examples and comparative examples is calculated according to the national standard after the equivalent is complemented, the paste yield is 14.08%, and the medicinal material content is calculated according to the pharmacopoeia requirement of 0.08%.
Therefore, the transfer rate (%) of the content of 3, 29-dibenzoyl trichosanthes kirilowii Maxim in the trichosanthes kirilowii Maxim formulation granule of the present invention is =the content of 3, 29-dibenzoyl trichosanthes kirilowii Maxim (mg/g) ×14.08%/(0.08% ×1000) ×100%.
The specific results are shown in the following table:
TABLE 3 Table of the results of the measurements of the semen Trichosanthis extract powder
As can be seen from Table 3, when the seed kernel breakage rate of the semen Trichosanthis is low, the dosage of beta-cyclodextrin is too large or the extraction temperature is too low, the content and the content transfer rate of 3, 29-dibenzoyl trichosanthes kirilowii Maxim can be reduced; when the kernel breakage rate is high, the dosage of beta-cyclodextrin is too small, the relative density of the concentrated filtrate is too high at 60 ℃ or dynamic extraction is carried out, the content and the content transfer rate of 3, 29-dibenzoyl trichosanthes kirilowii kernel triol are improved, but the repose angle is too high, so that the preparation method is not suitable for granulating or preparing tablets.
The specific kernel breaking rate, the beta-cyclodextrin dosage, the extraction mode and the temperature and the relative density of the concentrated filtrate at 60 ℃ are selected, so that the higher content and the content transfer rate of the 3, 29-dibenzoyl trichosanthes kirilowii Maxim can be effectively obtained, and the obtained trichosanthes kirilowii Maxim particles have a better repose angle.
It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

Claims (10)

1. A preparation method of semen trichosanthis paste powder is characterized in that semen trichosanthis is rolled into semen trichosanthis decoction pieces with kernel breakage rate of 60-90%, and then the semen trichosanthis paste powder is obtained by circularly extracting, filtering, concentrating, filtering again, adding beta-cyclodextrin into the obtained concentrated solution, mixing uniformly, centrifugally emulsifying, adding an adhesive, mixing uniformly, and drying.
2. The method for preparing the semen trichosanthis paste powder according to claim 1, wherein the seed coat breakage rate of the semen trichosanthis decoction pieces is 100%.
3. The method for preparing semen trichosanthis paste powder according to claim 1 or 2, wherein the centrifugal emulsification is shearing, grinding and high-speed stirring by a colloid mill.
4. The method for preparing the semen trichosanthis paste powder according to claim 1 or 2, wherein the weight ratio of semen trichosanthis decoction pieces to beta-cyclodextrin is 10-20:0.2-0.5.
5. The method for preparing the semen trichosanthis paste powder according to claim 1 or 2, wherein the weight ratio of semen trichosanthis decoction pieces to the adhesive is 10-20:0.25-0.7.
6. The method for preparing semen trichosanthis paste powder according to claim 1 or 2, wherein the temperature of the cyclic extraction is 95-100 ℃ and the time is 0.5-1 h.
7. The method for preparing semen trichosanthis paste powder according to claim 1 or 2, wherein the relative density of the obtained concentrated filtrate after concentration is 1.02-1.06 at 60 ℃.
8. The method for preparing semen trichosanthis paste powder according to claim 1 or 2, wherein the adhesive is at least one of dextrin, povidone K30, polyvinylpyrrolidone and sodium carboxymethyl starch.
9. The method for preparing semen trichosanthis paste powder according to claim 1 or 2, wherein the solvent adopted in the cyclic extraction process is water, and the weight-volume ratio of semen trichosanthis decoction pieces to water is 1kg: 14-18L;
the pore diameters of the two filtering holes are 100-500 meshes.
10. A method for preparing semen trichosanthis formula particles, which is characterized in that the semen trichosanthis formula particles are prepared by directly granulating semen trichosanthis paste powder prepared by the method according to any one of claims 1-9 by a dry method.
CN202410344646.5A 2024-03-25 2024-03-25 Preparation method of semen trichosanthis paste powder and formula granules Pending CN118416120A (en)

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