CN114681536A

CN114681536A - Improved preparation method of spleen-enlivening pharmaceutical composition

Info

Publication number: CN114681536A
Application number: CN202011576627.3A
Authority: CN
Inventors: 孙小鹦; 廖萍; 廖伟; 廖忠
Original assignee: GUIZHOU JIANXING PHARMACEUTICAL CO Ltd
Current assignee: GUIZHOU JIANXING PHARMACEUTICAL CO Ltd
Priority date: 2020-12-28
Filing date: 2020-12-28
Publication date: 2022-07-01
Anticipated expiration: 2040-12-28
Also published as: CN114681536B

Abstract

The invention relates to an improved preparation method of a spleen-enlivening pharmaceutical composition, which has the advantages of high content of effective components, shortened drying time, low energy consumption, high production efficiency and the like by using preparation methods such as alcohol extraction, water extraction and the like.

Description

Improved preparation method of spleen-enlivening pharmaceutical composition

Technical Field

The invention belongs to the technical field of traditional Chinese medicine pharmacy, and particularly relates to a preparation method of an improved spleen-enlivening pharmaceutical composition.

Background

The spleen-enlivening capsule and the spleen-enlivening and infant-nourishing granule are staple products of Guizhou Jianxing pharmaceutical industry Limited company of the applicant, wherein the spleen-enlivening capsule has the effects of enlivening spleen, appetizing, nourishing blood, soothing nerves, and strengthening intestine to stop diarrhea, and is used for symptoms of loose stool and diarrhea, inappetence and insomnia caused by spleen qi deficiency; the spleen-enlivening and infant-nourishing granules have the effects of enlivening spleen, stimulating appetite, nourishing blood, soothing nerves, securing intestine and stopping diarrhea, and are used for treating children anorexia, diarrhea and loose stool, dysphoria, night sweat and enuresis night cry caused by spleen qi deficiency.

The spleen-enlivening medicine has some defects in the actual production and preparation process, and concretely refers to the following prior art:

1. the applicant, Guizhou Jianxing pharmaceutical industry Co., Ltd, filed 2002 for Chinese invention patents with patent names: a traditional Chinese medicine preparation for activating spleen, stimulating appetite, tonifying qi and reinforcing deficiency (patent number: ZL02127908.X) discloses a preparation method of a spleen-activating medicine, which comprises the following steps: decocting 360g of herba Duchesneae Indicae, 326g of herba Gerberae Piloselloidis, 210g of fructus Gardeniae tea, and 72g of radix Pimpinellae Candolleanae with water to obtain medicinal liquid, concentrating to obtain concentrated solution, adding adjuvants, drying, and grading.

2. The applicant, the chinese patent of invention applied in 2019 by the guizhou jiangxing pharmaceutical industry limited company, has the patent names: the preparation method and the quality control method of the spleen-enlivening and infant-nourishing granules (patent number: ZL201910165531.9) disclose the preparation method of the spleen-enlivening medicine, which comprises the following steps: taking herba Duchesneae Indicae, herba Gerberae Piloselloidis, fructus Gardeniae tea and Valeriana jatamansi jones according to the formula amount, adding warm water of 40-60 ℃, soaking for 0.5 hour, decocting for 2 times, 2 hours for the first time and 1.5 hours for the second time, mixing the decoctions, filtering, concentrating to obtain clear paste with the relative density of 1.15-1.18 (80 ℃), adding a proper amount of sucrose powder, mixing uniformly, preparing into granules, and drying to obtain the traditional Chinese medicine.

3. The execution standard WS-11534(ZD-1534) -2002-2012Z of the spleen-enlivening capsule issued by the State drug administration discloses a preparation method which comprises the following steps: 395g of herba Duchesneae Indicae, 380g of herba Gerberae Piloselloidis, 125g of fructus Gardeniae tea and 93g of valeriana jatamansi jones, 30g of herba Duchesneae Indicae is pulverized into fine powder, and sieved by a 80-mesh sieve for later use. Soaking the rest herba Duchesneae Indicae and other three materials in water for 30 minutes, decocting twice, 2 hours for the first time and 1.5 hours for the second time, mixing decoctions, filtering, concentrating the filtrate to obtain fluid extract with relative density of 1.17-1.20 (80 ℃), adding herba Duchesneae Indicae fine powder, mixing, drying, pulverizing, sieving with 60 mesh sieve, and encapsulating.

4. The execution standard WS-10337(ZD-0337) -2002-: soaking the four medicinal materials in water for 30 minutes, decocting for 2 times, the first time lasts for 2 hours, the second time lasts for 1.5 hours, combining the decoctions, filtering, concentrating the filtrate into clear paste with the relative density of 1.15-1.18 (80 ℃), adding sucrose powder, uniformly mixing, granulating, and drying to obtain the traditional Chinese medicine.

The preparation methods of the spleen-enlivening medicine have the technical problems of unclear preparation process parameters, unsatisfactory extract yield, low content of effective components, long extract drying time, low production efficiency and the like.

Disclosure of Invention

In order to overcome the technical problems in the prior art, the existing preparation method of the spleen-enlivening medicament is improved through repeated research and test of company engineers and technicians, and the preparation method of the improved spleen-enlivening medicament composition is provided and is mainly realized through the following technical scheme:

the invention relates to a preparation method of an improved spleen-enlivening medicinal composition, which consists of 360g of tassella herb, 326g of gerbera piloselloides, 210g of gardenia tea and 72g of valeriana jatamansi jones, and the preparation method comprises the following steps:

1) cleaning rhizoma valerianae latifoliae, slicing, oven drying, and pulverizing to obtain fine powder.

2) Cleaning herba Duchesneae Indicae, oven drying, and pulverizing to obtain fine powder.

3) Taking the gardenia tea medicinal material, cleaning, slicing and drying for later use.

4) Taking the gerbera piloselloides medicinal material, cleaning and drying for later use.

5) Adding 6-8 times of the gardenia tea and the gerbera piloselloides processed in the steps 3) and 4) into 45-65 ℃ warm water, soaking for 30 minutes, decocting for 2 times, decocting for 2 hours for the first time and 1.5 hours for the second time, combining the decoctions, filtering, and keeping the filtrate for later use.

6) And (3) combining the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain clear paste with the relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at the drying temperature of 100-130 ℃ and the vacuum degree of-0.085 Mpa for 3-5 hours, crushing to obtain fine powder, sieving, adding auxiliary materials, uniformly mixing, and preparing into pharmaceutically acceptable dosage forms.

7) The preparation method according to claim 1, wherein the ethanol in step 5) is used in an amount and concentration of: 7 times of 70% ethanol.

Preferably, the step 5) of ethanol reflux extraction is performed for 2 times, each time for 2 hours.

Preferably, the temperature of the warm water of the step 6) is 55 ℃.

Preferably, the amount of water added in the step 6) is 7 times.

Preferably, the vacuum belt drying conditions of step 7) are as follows: the drying temperature is 130 ℃, and the drying time is 3 hours.

Preferably, the sieve mesh number of step 7) is: and (4) screening by a 65-100 mesh sieve.

The pharmaceutical dosage form of the invention is a solid preparation or a liquid preparation.

The solid preparation provided by the invention is granules, capsules, tablets, pills and powder.

The liquid preparation of the invention is mixture and oral liquid.

The auxiliary material of the invention refers to a conventional drug carrier in the field of pharmacy, and is selected from one or more of the following fillers, binders, disintegrating agents, lubricants, surfactants or flavoring agents:

the filler is starch, sucrose powder, lactose, mannitol, sorbitol, xylitol, microcrystalline cellulose or glucose.

The adhesive is cellulose derivative, alginate, gelatin or polyvinylpyrrolidone.

The disintegrant is selected from microcrystalline cellulose, sodium carboxymethyl starch, crospolyvinylpyrrolidone, low-substituted hydroxypropyl cellulose or croscarmellose sodium.

The lubricant is selected from stearic acid, polyethylene glycol, calcium carbonate, sodium bicarbonate, superfine silica gel powder, talcum powder or magnesium stearate.

The surfactant is selected from sodium dodecyl benzene sulfonate, stearic acid, polyoxyethylene-polyoxypropylene copolymer, sorbitan fatty acid or polysorbate (Tween) and the like.

The flavoring agent is selected from crystalline maltitol, sucralose or saccharin sodium.

The invention has the following beneficial effects:

1. the invention extracts the valeriana jatamansi jones and the emilia sonchifolia medicinal material by ethanol, and the average content of the active ingredients of the extract chlorogenic acid is 0.1924mg/g, which is higher than the average content of 0.1555mg/g of the chlorogenic acid in the prior art.

2. The invention adopts warm water to soak the gardenia tea and the gerbera piloselloides medicinal materials, accelerates the precipitation of effective components in the medicinal materials, and realizes the average yield of 20.66 percent of extract which is 19.63 percent higher than the average yield of the extract in the prior art.

3. The invention adopts vacuum belt type drying, reduces the drying time to about 3 hours, obviously saves energy consumption and improves the production efficiency.

Detailed Description

The present invention is described in detail below with reference to specific embodiments, which will help those skilled in the art to further understand the present invention, but not limit the present invention in any way, and those skilled in the art can make various changes and modifications without departing from the spirit of the present invention, which falls into the protection scope of the present invention.

In the following examples, the times are multiple by weight, and the medicinal materials in the preparation process are weighed according to the formula of the spleen-enlivening medicinal composition.

Example 1: preparing into granule

1) Weighing valeriana jatamansi jones according to a formula, cleaning, slicing, drying and crushing to obtain fine powder.

2) Weighing herba Duchesneae Indicae according to formula, cleaning, oven drying, and pulverizing to obtain fine powder.

3) Weighing the gardenia tea medicinal material according to the formula, cleaning, slicing and drying.

4) Weighing the gerbera piloselloides medicinal material according to the formula, cleaning and drying.

5) Adding 70% ethanol in an amount which is 7 times that of the fine powder obtained in the steps 1) and 2) into the fine powder, performing reflux extraction for 2 times, each time for 2 hours, combining the extracting solutions, and filtering to obtain filtrate for later use.

6) Adding the processed gardenia tea and gerbera piloselloides in the steps 3) and 4) into warm water with the temperature of 55 ℃ in an amount of 7 times, soaking for 30 minutes, decocting for 2 times, 2 hours for the first time and 1.5 hours for the second time, combining the decoctions, and filtering to obtain filtrate for later use.

7) And (3) mixing the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain clear paste with the relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt manner at the vacuum degree of-0.085 Mpa and the drying temperature of 130 ℃ for 3 hours, crushing to obtain fine powder, sieving with a 65-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, granulating and bagging to obtain the product.

Example 2: preparing capsule

1) Weighing radix Pimpinellae Candolleanae medicinal materials according to the formula, cleaning, slicing, oven drying, and pulverizing to obtain fine powder.

6) Adding the gardenia tea and the gerbera piloselloides processed in the steps 3) and 4) into warm water with the temperature of 55 ℃ which is 7 times that of the gardenia tea and the gerbera piloselloides, soaking for 30 minutes, decocting for 2 times, 2 hours for the first time and 1.5 hours for the second time, combining the decoctions, filtering, and keeping the filtrate for later use.

7) And (3) combining the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with a relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at a drying temperature of 130 ℃ and a vacuum degree of-0.085 Mpa for 3 hours, crushing to obtain fine powder, sieving with a 65-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, and encapsulating to obtain the product.

Example 3: preparation of tablets

7) And (3) combining the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with a relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at a drying temperature of 130 ℃ and a vacuum degree of-0.085 Mpa for 3 hours, crushing to obtain fine powder, sieving with a 65-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, and tabletting to obtain the product.

Example 4: preparation of the powder

7) And (3) combining the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with a relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at a drying temperature of 130 ℃ and a vacuum degree of-0.085 Mpa for 3 hours, crushing to obtain fine powder, sieving with a 100-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, and bagging to obtain the product.

Example 5: preparing pills

7) And (3) mixing the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain clear paste with the relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at the vacuum degree of-0.085 Mpa and the drying temperature of 130 ℃ for 3 hours, crushing to obtain fine powder, sieving with a 65-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, extruding and preparing pills.

Example 6: preparing oral liquid

7) And (3) combining the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with a relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at a vacuum degree of-0.085 Mpa and a drying temperature of 130 ℃ for 3 hours, crushing to obtain fine powder, sieving with a 100-mesh sieve, adding a proper amount of crystalline maltitol, stirring for dissolving, adding purified water to a constant volume, controlling the pH value to be 6, and bottling to obtain the product.

Example 7: preparing into granule

5) Adding 60% ethanol 6 times the amount of the fine powder obtained in the steps 1) and 2) into the fine powder, performing reflux extraction for 3 times, each time for 2 hours, combining the extracting solutions, and filtering to obtain filtrate for later use.

6) Adding the gardenia tea and the gerbera piloselloides processed in the steps 3) and 4) into 6 times of warm water at 45 ℃, soaking for 30 minutes, decocting for 2 times, 2 hours for the first time and 1.5 hours for the second time, combining the decoctions, and filtering to obtain filtrate for later use.

7) And (3) combining the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with a relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at a drying temperature of 100 ℃ and a vacuum degree of-0.085 Mpa for 5 hours, crushing to obtain fine powder, sieving with a 65-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, granulating and bagging to obtain the product.

Example 8: preparing capsule

7) And (3) mixing the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain clear paste with the relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at the vacuum degree of-0.085 Mpa and the drying temperature of 100 ℃ for 5 hours, crushing to obtain fine powder, sieving with a 65-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, and encapsulating to obtain the product.

Example 9: preparation of tablets

7) And (3) mixing the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain clear paste with the relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at the vacuum degree of-0.085 Mpa and the drying temperature of 100 ℃ for 5 hours, crushing to obtain fine powder, sieving with a 65-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, and tabletting to obtain the product.

Example 10: preparation of the powder

7) And (3) combining the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with a relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at a drying temperature of 100 ℃ and a vacuum degree of-0.085 Mpa for 5 hours, crushing to obtain fine powder, sieving with a 100-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, and bagging to obtain the product.

Example 11: preparing pills

7) And (3) combining the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with a relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at a drying temperature of 100 ℃ and a vacuum degree of-0.085 Mpa for 5 hours, crushing to obtain fine powder, sieving with a 65-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, and making pills.

Example 12: preparing oral liquid

7) And (3) combining the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with a relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at a vacuum degree of-0.085 Mpa and a drying temperature of 100 ℃ for 5 hours, crushing to obtain fine powder, sieving with a 100-mesh sieve, adding crystalline maltitol, stirring for dissolving, adding purified water to a constant volume, controlling the pH value to be 6, and bottling to obtain the product.

Example 13: preparing into granule

5) Adding 8 times of 80% ethanol into the fine powder obtained in the steps 1) and 2), reflux-extracting for 3 times, each time for 1 hour, combining the extracting solutions, and filtering to obtain filtrate for later use.

6) Adding the gardenia tea and the gerbera piloselloides processed in the steps 3) and 4) into 8 times of warm water with the temperature of 65 ℃, soaking for 30 minutes, decocting for 2 times, 2 hours for the first time and 1.5 hours for the second time, combining the decoctions, and filtering to obtain filtrate for later use.

7) And (3) combining the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with a relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at a vacuum degree of-0.085 Mpa and a drying temperature of 115 ℃ for 4 hours, crushing to obtain fine powder, sieving with a 65-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, and granulating to obtain the product.

Example 14: preparing capsule

7) And (3) combining the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with a relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at a drying temperature of 115 ℃ under-0.085 Mpa for 4 hours, crushing to obtain fine powder, sieving with a 65-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, and encapsulating to obtain the product.

Example 15: preparation of tablets

5) Adding 8 times of 80% ethanol into the fine powder obtained in the step 1) and the step 2), reflux-extracting for 3 times, each time for 1 hour, combining the extracting solutions, and filtering to obtain filtrate for later use.

7) And (3) combining the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with a relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at a vacuum degree of-0.085 Mpa and a drying temperature of 115 ℃ for 4 hours, crushing to obtain fine powder, sieving with a 65-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, and tabletting to obtain the product.

Example 16: preparation of the powder

7) And (3) combining the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with a relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at a vacuum degree of-0.085 Mpa and a drying temperature of 115 ℃ for 4 hours, crushing to obtain fine powder, sieving with a 100-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, and bagging to obtain the product.

Example 17: preparing pills

7) And (3) combining the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with a relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at a vacuum degree of-0.085 Mpa and a drying temperature of 115 ℃ for 4 hours, crushing to obtain fine powder, sieving with a 100-mesh sieve, adding a proper amount of sucrose powder, uniformly mixing, extruding and making into pills.

Example 18: preparing oral liquid

7) And (3) mixing the filtrates obtained in the steps 5) and 6), uniformly mixing, concentrating under reduced pressure to obtain clear paste with the relative density of 1.15-1.18 (80 ℃), drying in a vacuum belt type at the vacuum degree of-0.085 Mpa and the drying temperature of 115 ℃ for 4 hours, crushing to obtain fine powder, sieving with a 100-mesh sieve, adding crystalline maltitol, stirring for dissolving, adding purified water for fixing the volume, controlling the pH value to be 6, and bottling to obtain the finished product.

To further illustrate the beneficial effects of the present invention, the applicant conducted a series of experimental studies of the preparation method and provided the following experimental data:

first, investigation of preparation process

The formula is as follows: 360g of herba Duchesneae Indicae, 326g of herba Gerberae Piloselloidis, 210g of fructus Gardeniae tea and 72g of radix Pimpinellae Candolleanae.

The process comprises the following steps: the original preparation process adopts the four medicinal materials to carry out simple water decoction, the content of active ingredients is lower, the improvement is that the valeriana jatamansi jones and the emilia sonchifolia are extracted by ethanol after being crushed, and the extraction solvent, the amount, the extraction times and the extraction time are examined. Decocting fructus Gardeniae tea and herba Gerberae Piloselloidis in water, mixing the extractive solution with radix Pimpinellae Candolleanae and herba Duchesneae Indicae ethanol extractive solution, concentrating, and inspecting the extract yield and total solid.

The investigation method comprises the following steps: chlorogenic acid content determination method

1) Instruments and reagents: high performance liquid chromatograph: agilent, USA; the chlorogenic acid reference substance is provided by China food and drug testing institute, and the batch number is 110753-once 201314; reagent: acetonitrile is chromatographic alcohol, and water is deionized water.

2) Chromatographic conditions are as follows: chromatographic column Dikma C with octadecylsilane chemically bonded silica as filler₁₈(4.6 mm. times.250 mm,5 μm); mobile phase: acetonitrile-0.4% phosphoric acid aqueous solution (12:88) at a flow rate of 1.0 ml/min; the detection wavelength is 327 nm; the number of theoretical plates is not less than 1000 calculated according to chlorogenic acid peak.

3) Preparation of control solutions: precisely weighing appropriate amount of chlorogenic acid reference substance, adding 50% methanol to obtain 200 μ g/ml solution.

4) Preparation of a test solution: taking 0.5g of the extract of the following example, placing the extract in a conical flask with a plug, adding 50ml of 50% methanol solution, sealing the plug, shaking up, and weighing the extract to determine the mass; ultrasonic extracting for 40min, cooling, adding 50% methanol solution to reduce weight loss, shaking, filtering, collecting filtrate 0.2ml, adding 50% methanol to dilute, and diluting to constant volume of 10 ml.

5) And (3) determination: precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.

First) inspection of the extraction method of valeriana jatamansi jones and emilia sonchifolia

1. Investigation of ethanol extraction Process

Mixing dried and pulverized Valeriana jatamansi Jones and herba Duchesneae Indicae fine powder, adding 6, 7, 8 times of 60%, 70%, 80% ethanol respectively, reflux extracting for 2 times, each for 2 hr, drying the filtrate, and pulverizing to obtain ethanol extract.

Preparing corresponding test solution according to the method for measuring the content of the chlorogenic acid, and measuring the content of the chlorogenic acid in each part of the extract. The results are shown in tables 1-3:

table 1: influence of 60% ethanol dosage on effective component content

Table 2: influence of 70% ethanol dosage on effective component content

Table 3: influence of 80% ethanol dosage on effective component content

And (3) test results: from the above test results, it can be seen that the chlorogenic acid content of the extract obtained by using 7 times and 8 times of 70% ethanol and 80% ethanol is equivalent, and from the aspects of cost saving, energy consumption and the like, 7 times of 70% ethanol is selected as a preferred parameter of the ethanol extraction process.

2. Examination of number of ethanol extractions and extraction time

Mixing dried and pulverized Valeriana jatamansi Jones and herba Duchesneae Indicae fine powder, adding 7 times of 70% ethanol, reflux extracting for 2, 3, and 4 times respectively for 1, 2, and 3 hr each time, drying the filtrate, and pulverizing to obtain ethanol extract.

According to the content determination method, 5g of ethanol extract is prepared into a test solution, and the content of chlorogenic acid in each part of extract is determined. The results are shown in tables 4-6:

table 4: influence of extraction times on the content of effective components (1 hour each time)

Table 5: influence of extraction times on the content of effective components (2 hours each time)

Table 6: influence of extraction times on the content of effective components (3 hours each time)

And (3) test results: from the above table 4-6, it can be seen that, when 2 hours and 3 hours are extracted each time, the extraction times are 2 times, 3 times and 4 times, and when 1 hour is extracted each time, 4 times are extracted each time, the content of the effective components of the obtained extract is equivalent, and the extraction times are 2 times selected and 2 hours are extracted each time as the optimal extraction parameters in consideration of the factors of saving energy consumption, cost, reducing process steps and the like.

And (4) conclusion: through the experimental design of the alcohol extraction process parameters, the preferable ethanol extraction method obtained by screening comprises the following steps: mixing dried and pulverized Valeriana jatamansi Jones and herba Duchesneae Indicae fine powder, adding 7 times of 70% ethanol, and reflux-extracting for 2 times (each for 2 hr) to obtain ethanol extractive solution.

Second) research on extraction method of gardenia tea and gerbera piloselloides

1. Investigation of Water extraction Process

Taking cut and dried gardenia tea and gerbera piloselloides, respectively adding warm water with the temperature of 45 ℃, 55 ℃ and 65 ℃ in an amount of 6, 7 and 8 times of the amount of the warm water, soaking for 30 minutes, decocting for 2 times, decocting for 2 hours for the first time and decocting for 1.5 hours for the second time, combining the decoctions, filtering, combining the filtrate with the ethanol extracting solution, mixing uniformly, concentrating the filtrate to obtain clear paste with the relative density of 1.15-1.18 (80 ℃), calculating the yield of the extract, and detecting the total solid. The results are shown in tables 7-9:

table 7: influence of the amount of water added on the yield of extract and the total solid (Water temperature 45 ℃ C.)

Table 8: influence of the amount of water added on the yield of extract and the total solid (Water temperature 55 ℃ C.)

Table 9: influence of the amount of water added on the yield of the extract and the total solid (water temperature 65 ℃ C.)

And (3) test results: from the above table 7-9, it can be seen that when the water addition temperature is 55 ℃ and 65 ℃, the extract yield and total solid content of 7 times and 8 times of water are similar, and from the consideration of saving energy consumption and cost, the water addition temperature of 55 ℃ and the water addition amount of 7 times are preferred as the optimal extraction process parameters.

And (4) conclusion: through the experimental design of the water extraction process parameters, the optimal water extraction method obtained by screening comprises the following steps: taking the gardenia tea and the gerbera piloselloides, adding 7 times of warm water with the temperature of 55 ℃, soaking for 30 minutes, decocting for 2 times, decocting for 2 hours for the first time, decocting for 1.5 hours for the second time, combining the decoction, filtering to obtain an extracting solution, combining the extracting solution with the ethanol extracting solution, mixing uniformly, concentrating the filtrate to obtain clear paste with the relative density of 1.15-1.18 (80 ℃), drying, crushing, and adding auxiliary materials to obtain the gardenia tea.

Third) study of drying Process

And (3) carrying out vacuum belt type drying, wherein the vacuum degree is-0.085 Mpa, the drying temperature is 100-130 ℃, drying is carried out for 3-5 hours, the following 3 drying methods are respectively set, and the influence of different drying temperatures and different drying times on the moisture content of the extract is investigated.

1. The drying method 1: and (3) vacuum belt drying: the vacuum degree is-0.085 Mpa, the drying temperature is 130 ℃, and the drying time is 3 hours.

2. The drying method 2: and (3) vacuum belt drying: the vacuum degree is-0.085 Mpa, the drying temperature is 115 ℃, and the drying time is 4 hours.

3. The drying method 3: and (3) vacuum belt drying: the vacuum degree is-0.085 Mpa, the drying temperature is 100 ℃, and the drying time is 5 hours. The results are shown in Table 10:

table 10: influence of different drying temperatures and time on water content of extract

And (3) test results: according to the above table, the vacuum belt drying method is adopted, so that the drying time is obviously shortened, the moisture content of the extract is reduced, and the method 1 is preferably selected from the factors of saving energy consumption and the like, namely the vacuum degree is-0.085 Mpa, the drying temperature is 130 ℃, and the drying time is 3 hours as a preferable drying process parameter.

And (4) conclusion: the vacuum belt type drying process is carried out under the conditions that the vacuum degree is-0.085 Mpa, the drying temperature is 130 ℃ and the drying time is 3 hours.

Comparative test

Comparative example 1:

the invention has the following patent: a traditional Chinese medicine preparation for activating spleen, stimulating appetite, tonifying qi and tonifying deficiency (patent number: ZL02127908.X) is prepared by the following steps: decocting 360g of herba Emiliae, 326g of herba Gerberae Piloselloidis, 210g of fructus Gardeniae tea, and 72g of radix Pimpinellae Candolleanae with water to obtain decoction, concentrating to obtain concentrated solution, adding adjuvants, drying, and grading.

Comparative example 2:

the invention has the following patent: the preparation method and the quality control method of the spleen-enlivening and infant-nourishing granules (patent number: ZL201910165531.9) disclose the preparation method of the spleen-enlivening medicine, which comprises the following steps: taking herba Duchesneae Indicae, herba Gerberae Piloselloidis, fructus Gardeniae tea and Valeriana jatamansi jones according to the formula amount, adding warm water of 40-60 ℃, soaking for 0.5 hour, decocting for 2 times, 2 hours for the first time and 1.5 hours for the second time, mixing the decoctions, filtering, concentrating to obtain clear paste with the relative density of 1.15-1.18 (80 ℃), adding a proper amount of sucrose powder, mixing uniformly, preparing into granules, and drying to obtain the traditional Chinese medicine.

Comparative example 3:

the execution standard WS-11534(ZD-1534) -2002-2012Z of the spleen-enlivening capsule issued by the State drug administration discloses a preparation method which comprises the following steps: 395g of herba Duchesneae Indicae, 380g of herba Gerberae Piloselloidis, 125g of fructus Gardeniae tea and 93g of valeriana jatamansi jones, 30g of herba Duchesneae Indicae is pulverized into fine powder, and sieved by a 80-mesh sieve for later use. Soaking the rest herba Duchesneae Indicae and other three materials in water for 30 minutes, decocting twice, 2 hours for the first time and 1.5 hours for the second time, mixing decoctions, filtering, concentrating the filtrate to obtain fluid extract with relative density of 1.17-1.20 (80 ℃), adding herba Duchesneae Indicae fine powder, mixing, drying, pulverizing, sieving with 60 mesh sieve, and encapsulating.

Comparative example 4:

the execution standard WS-10337(ZD-0337) -2002-: soaking the four medicinal materials in water for 30 minutes, decocting for 2 times, the first time lasts for 2 hours, the second time lasts for 1.5 hours, combining the decoctions, filtering, concentrating the filtrate into clear paste with the relative density of 1.15-1.18 (80 ℃), adding sucrose powder, uniformly mixing, granulating, and drying to obtain the traditional Chinese medicine.

The contents of the effective components of chlorogenic acid in the examples 1, 7 and 15 of the invention and the comparative examples 1, 2, 3 and 4 are compared according to the content determination method of the chlorogenic acid, and the extract and solid yields of each group are counted and compared, and the results are shown in tables 11 to 13 in sequence.

Table 11: chlorogenic acid contents of examples and comparative examples

Table 12: extract and solid yield of examples and comparative examples

Table 13: extract and solid yield of examples and comparative examples

And (3) test results: from the above table, the content of the average effective ingredient chlorogenic acid in the examples is much higher than that of the comparative example; the average extractum and total solid yield of the examples are higher than those of the comparative example.

And (4) conclusion: by combining the series of examples and the process investigation and comparative tests, the content of the effective components of the composition prepared by the preparation method of the improved spleen-enlivening medicinal composition provided by the invention is verified to be higher than the content of the effective components of the extract prepared by the preparation method in the prior art.

By the preparation method of the spleen-enlivening pharmaceutical composition, the content of active ingredients in the pharmaceutical composition is improved, the extraction rate of composition extract is improved, and the quality of the medicine is further improved; meanwhile, through the research on the extract drying process, the time of the drying process is reduced, the energy consumption is saved, and the production efficiency is improved.

Claims

1. An improved preparation method of a spleen-enlivening medicinal composition is characterized in that the spleen-enlivening medicinal composition consists of 360g of poinsettia, 326g of gerbera pilosula, 210g of gardenia tea and 72g of valeriana jatamansi jones, and the preparation method comprises the following steps:

1) cleaning rhizoma valerianae latifoliae, slicing, oven drying, and pulverizing to obtain fine powder;

2) cleaning herba Duchesneae Indicae, oven drying, and pulverizing to obtain fine powder;

3) cleaning a gardenia tea medicinal material, slicing and drying for later use;

4) taking a gerbera piloselloides medicinal material, cleaning and drying for later use;

5) adding 60-80% ethanol in an amount which is 6-8 times that of the fine powder obtained in the step 1) and the step 2), performing reflux extraction for 2-4 times, each time for 1-3 hours, combining the extracting solutions, and filtering to obtain a filtrate for later use; adding 6-8 times of the gardenia tea and the gerbera piloselloides processed in the steps 3) and 4) into 45-65 ℃ warm water, soaking for 30 minutes, decocting for 2 times, decocting for 2 hours for the first time and 1.5 hours for the second time, combining the decoctions, and filtering to obtain a filtrate for later use;

2. The preparation method according to claim 1, wherein the ethanol in step 5) is used in an amount and concentration of: 7 times of 70% ethanol.

3. The method according to claim 1, wherein the ethanol reflux extraction of step 5) is performed 2 times for 2 hours.

4. The method according to claim 1, wherein the warm water of step 6) has a temperature of 55 ℃.

5. The method according to claim 1, wherein the amount of water added in step 6) is 7 times the amount of water.

6. The method of claim 1, wherein the vacuum belt drying conditions of step 7) are: drying temperature 130 deg.C, drying for 3 hr.

7. The method of claim 1, wherein the step 7) has a sieve mesh number of: and (4) screening by a 65-100 mesh sieve.

8. The method of claim 1, wherein the dosage form is a solid formulation or a liquid formulation.

9. The preparation method according to claim 8, wherein the solid preparation is granules, capsules, tablets, pills or powder, and the liquid preparation is mixture or oral liquid.

10. The method according to claim 1, wherein the excipient is starch, crystalline maltitol, or sucrose powder.