Preparation method of pollen extract preparation

Abstract

The invention provides a preparation method of a pollen extract preparation, and relates to the technical field of preparation processes. The preparation method comprises the following steps: (1) dissolving a pollen extract EA10 with 95% ethanol to obtain a solution I; (2) dissolving the pollen extract P5 in water to obtain a solution II; (3) paving auxiliary material powder colloidal silicon dioxide, microcrystalline cellulose and croscarmellose sodium on a boiling bed for preheating; and (4) spraying the solution I and the solution II into a boiling bed, mixing with the auxiliary material powder, and granulating. According to the preparation method, a one-step granulation forming process is adopted, conditions are mild, degradation of related medicine components in the forming process cannot be caused, the disintegration and tablet weight differences of tablets prepared by pressing prepared particles meet pharmacopoeia standards under the condition that auxiliary materials are in a certain composition proportion, a long-time melting process is not needed in the granulation process, and the operation time is shortened.

Description

Technical Field

[0001] The invention belongs to the technical field of preparation technology, and specifically relates to a method for preparing a pollen extract preparation. Background Art

[0002] Prostatitis refers to a prostate disease caused by a variety of complex reasons, with urethral irritation symptoms and chronic pelvic pain as the main clinical manifestations. Prostatitis is a common disease in urology, ranking first among male patients under 50 years old in urology. Prostatitis can usually be treated with Pushitai tablets. The current preparation process of Pushitai tablet compositions is relatively complicated, and it is difficult to produce in large quantities, resulting in high production costs. For example, Chinese invention patent application CN111419884A discloses a preparation process for a Sheniton tablet composition, and the specific preparation steps are as follows: Step 1, preparation of GBX Premix: EA10 (66g) is placed in a white plastic container, and the temperature is controlled at 35°C in a heating cabinet for 20h to melt EA10, and the melted EA10 is mixed with microcrystalline cellulose (462g) in a mixing device for 8min, and then anhydrous silicon dioxide (70g) is added. However, the melting time in the above patent application is as long as 20h. It takes a long time.

[0003] Therefore, there is an urgent need to develop a method for preparing a pollen extract preparation that does not require a long melting process, shortens the operation time, and prevents drug degradation according to the characteristics of the pollen extract. Summary of the invention

[0004] The present invention aims at the problems existing in the prior art and provides a method for preparing a pollen extract preparation. Through a one-step granulation molding process, the conditions are mild, the drug degradation will not be caused during the molding process, and the disintegration and tablet weight difference of the tablets pressed from the prepared granules meet the pharmacopoeia standards under a certain composition ratio of the excipients, and a long melting process is not required during the granulation process, thus shortening the operation time.

[0005] One of the purposes of the present invention is to provide a method for preparing a pollen extract preparation, the pollen extract preparation comprising pollen extract EA10, pollen extract P5 and auxiliary materials, the preparation method comprising the following steps: (1) dissolving pollen extract EA10 in 95% ethanol to obtain solution I; (2) dissolving pollen extract P5 in water to obtain solution II; (3) spreading auxiliary materials such as colloidal silicon dioxide, microcrystalline cellulose and cross-linked sodium carboxymethyl cellulose on a fluidized bed for preheating; (4) mixing solution I and solution II, spraying them into a fluidized bed for mixing and granulating with the auxiliary materials, the granulation time being 0.5-1h, to obtain the product.

[0006] Preferably, in step (1), the mass ratio of the pollen extract EA10 to 95% ethanol is 1:4-6.

[0007] Preferably, in step (2), the mass ratio of the pollen extract P5 to water is 1:1-3.

[0008] Preferably, in step (3), the mass ratio of colloidal silicon dioxide, microcrystalline cellulose and cross-linked sodium carboxymethyl cellulose is 1:20-50:1-2.

[0009] Preferably, the mass ratio of the pollen extract EA10 to the pollen extract P5 is 1:15-25.

[0010] Preferably, the mass ratio of the pollen extract EA10 to the auxiliary material is 1:30-40.

[0011] Preferably, during the granulation process in step (4), the air inlet temperature is controlled at 100-105° C., the material temperature is 50-70° C., and the atomization pressure is 0.45-0.6 MPa.

[0012] Preferably, the pollen extract preparation is a tablet, which is obtained by tableting and coating after a one-step granulation.

[0013] Further preferably, the coating is specifically: using 6% Opadry coating agent in 85% ethanol solution, continuously spraying with air flow until the coating layer weight is 1-6% of the tablet core weight, and drying. Preferably, the coating layer weight is 2%-4% of the tablet core weight.

[0014] Compared with the prior art, the present invention has the following beneficial effects: through a one-step granulation molding process, the conditions are mild, and the drug degradation will not be caused during the molding process. Moreover, when the auxiliary materials are in a certain composition ratio, the disintegration and tablet weight difference of the tablets pressed from the prepared granules meet the pharmacopoeia standards, and there is no need for a long melting process during the granulation process, thereby shortening the operation time. DETAILED DESCRIPTION

[0015] The following non-limiting examples can enable those skilled in the art to more fully understand the present invention, but do not limit the present invention in any way. The following content is merely an exemplary description of the scope of the present invention, and those skilled in the art can make various changes and modifications to the present invention based on the disclosed content, which should also fall within the scope of the present invention.

[0016] In the examples of the present invention, the sources and batch numbers of the relevant substances are shown in Table 1.

[0017] Table 1: Sources and batch numbers of related substances

[0018]

[0019]

[0020] Example 1

[0021] The preparation method of the pollen extract preparation comprises the following steps:

[0022] (1) dissolving 66 g of pollen extract EA10 in 5 times the volume fraction of 95% ethanol aqueous solution to obtain solution I;

[0023] (2) Dissolve 1.2 kg of pollen extract P5 in 2 times the amount of water to obtain solution II;

[0024] (3) Spread 70 g of colloidal silicon dioxide, 2130 g of microcrystalline cellulose, and 90 g of cross-linked sodium carboxymethyl cellulose on a fluidized bed for preheating;

[0025] (4) Solution I and Solution II are mixed, sprayed into a fluidized bed for mixing and granulation with the auxiliary materials, the inlet air temperature is controlled at 100° C., the material temperature is 60° C., the atomization pressure is 0.5 MPa, and the granulation is performed for 0.5 h.

[0026] Comparative Example 1:

[0027] The amounts of pollen extract EA10, pollen extract P5 and auxiliary materials such as colloidal silicon dioxide, microcrystalline cellulose and cross-linked carboxymethyl cellulose in Example 1 remain unchanged and are prepared by a conventional wet granulation method.

[0028] (1) Dissolve 66 g of EA10 in 5 times the volume fraction of 50% ethanol aqueous solution;

[0029] (2) Add 2130 g of microcrystalline cellulose and 90 g of cross-linked sodium carboxymethyl cellulose to a wet granulator, mix well, add the solution to make granules, dry at 50° C., and pass through an 80-mesh sieve after drying;

[0030] (3) Add 1.2 kg of pollen extract P5 and 70 g of colloidal silicon dioxide to the above particles and mix well to obtain the product.

[0031] Comparative Example 2:

[0032] The preparation method of the pollen extract preparation comprises the following steps:

[0033] (1) Dissolve 66 g of EA10 in 5 times the volume fraction of 95% ethanol aqueous solution to obtain solution I;

[0034] (2) Dissolve 1.2 kg of P5 in 2 times the amount of water to obtain solution II;

[0035] (3) Spread 70 g of colloidal silicon dioxide, 1970 g of microcrystalline cellulose, and 250 g of cross-linked sodium carboxymethyl cellulose on a fluidized bed for preheating;

[0036] (4) Solution I and Solution II are mixed, sprayed into a fluidized bed for mixing and granulation with the auxiliary materials, the inlet air temperature is controlled at 100° C., the material temperature is 60° C., the atomization pressure is 0.5 MPa, and the granulation is performed for 0.5 h.

[0037] The difference from Example 1 is that in step (3), the amount of microcrystalline cellulose is reduced to 1970 g, and the amount of cross-linked sodium carboxymethyl cellulose is increased to 250 g. The rest is the same as Example 1.

[0038] Comparative Example 3:

[0039] The preparation method of the pollen extract preparation comprises the following steps:

[0040] (1) Dissolve 66 g of EA10 in 5 times the volume fraction of 95% ethanol aqueous solution to obtain solution I;

[0041] (2) Dissolve 1.2 kg of P5 in 2 times the amount of water to obtain solution II;

[0042] (3) Spread 30 g of colloidal silicon dioxide, 2170 g of microcrystalline cellulose, and 90 g of cross-linked sodium carboxymethyl cellulose on a fluidized bed for preheating;

[0043] (4) Solution I and Solution II are mixed, sprayed into a fluidized bed for mixing and granulation with the auxiliary materials, the inlet air temperature is controlled at 100° C., the material temperature is 60° C., the atomization pressure is 0.5 MPa, and the granulation is performed for 0.5 h.

[0044] The difference from Example 1 is that in step (3), the amount of colloidal silicon dioxide is reduced to 30 g, and the amount of microcrystalline cellulose is increased to 2170 g. The rest is the same as Example 1.

[0045] Test Example 1:

[0046] The contents of the main drug components EA10 and P5 in the granules after the preparation process were determined by HPLC, and the degradation rate was calculated by the following formula:

[0047]

[0048] Wherein, M1 is the input amount of EA10 or P5 before preparation, and M2 is the mass of EA10 or P5 in the particles after preparation.

[0049] The degradation rates of EA10 and P5 in three different batches of particles prepared in Example 1 and Comparative Example 1 are shown in Table 2.

[0050] Table 2: Degradation rates of EA10 and P5 in three different batches of particles prepared in Example 1 and Comparative Example 1

[0051]

[0052] According to the data in the table, the present invention adopts a one-step granulation method with mild conditions, which will not cause degradation of the components pollen extract EA10 and pollen extract P5 during the molding process. However, the traditional wet granulation will cause serious degradation of the components EA10 and P5 during the drying process, affecting the effect of the drug.

[0053] Test Example 2:

[0054] The granules obtained in Example 1, Comparative Example 2 and Comparative Example 3 were respectively tableted and coated under the same experimental conditions to obtain tablets of about 0.36 g / tablet. The coating was specifically: 85% ethanol solution of 6% Opadry coating agent was continuously sprayed with air flow until the weight of the coating layer was 3% of the weight of the tablet core, and then dried. The tablet disintegration and tablet weight difference were determined according to the method of "Chinese Pharmacopoeia". Relevant data are shown in Table 3.

[0055] Table 3: Performance test results of the tablets prepared from the granules of Example 1, Comparative Example 2 and Comparative Example 3

[0056]

[0057] The one-step granulation material provided in Example 1 of the present invention has good fluidity, and the disintegration and tablet weight difference of the prepared tablets meet the pharmacopoeia standards, while the disintegration of the tablets of Comparative Examples 2-3 deteriorates, and the tablet weight difference does not meet the pharmacopoeia standards.

[0058] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, rather than to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions of the technical solution of the present invention by ordinary technicians in this field do not deviate from the essence and scope of the technical solution of the present invention.

Claims

1. A method for preparing a pollen extract preparation, the pollen extract preparation comprising pollen extract EA10, pollen extract P5 and excipients, characterized in that: The preparation method comprises the following steps: (1) dissolving pollen extract EA10 in 95% ethanol to obtain solution I; (2) dissolving pollen extract P5 in water to obtain solution II; (3) spreading auxiliary materials such as colloidal silicon dioxide, microcrystalline cellulose and cross-linked sodium carboxymethyl cellulose on a fluidized bed for preheating; (4) mixing solution I and solution II, spraying them into a fluidized bed for mixing and granulating with the auxiliary materials, and the granulation time is 0.5-1h to obtain the product.

2. The preparation method according to claim 1, characterized in that: In the step (1), the mass ratio of the pollen extract EA10 to 95% ethanol is 1:4-6.

3. The preparation method according to claim 1, characterized in that: In the step (2), the mass ratio of the pollen extract P5 to water is 1:1-3.

4. The preparation method according to claim 1, characterized in that: In the step (3), the mass ratio of colloidal silicon dioxide, microcrystalline cellulose and cross-linked sodium carboxymethyl cellulose is 1:20-50:1-2.

5. The preparation method according to claim 1, characterized in that: The mass ratio of the pollen extract EA10 to the pollen extract P5 is 1:15-25.

6. The preparation method according to claim 1, characterized in that: The mass ratio of the pollen extract EA10 to the auxiliary material is 1:30-40.

7. The preparation method according to claim 1, characterized in that: In the granulation process in step (4), the air inlet temperature is controlled at 100-105° C., the material temperature is 50-70° C., and the atomization pressure is 0.45-0.6 MPa.

8. The preparation method according to claim 1, characterized in that: The pollen extract preparation is a tablet, which is obtained by tableting and coating after one-step granulation.

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