CN116139238B - Pharmaceutical composition and preparation method thereof - Google Patents

Pharmaceutical composition and preparation method thereof Download PDF

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CN116139238B
CN116139238B CN202310199844.2A CN202310199844A CN116139238B CN 116139238 B CN116139238 B CN 116139238B CN 202310199844 A CN202310199844 A CN 202310199844A CN 116139238 B CN116139238 B CN 116139238B
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ethanol
mixing
water
tablet
filtering
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CN116139238A (en
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杨华
谭泽云
高慧娟
王西凤
邓坚
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HUNAN HANSEN PHARMACEUTICAL CO Ltd
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HUNAN HANSEN PHARMACEUTICAL CO Ltd
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    • A—HUMAN NECESSITIES
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    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/88—Liliopsida (monocotyledons)
    • A—HUMAN NECESSITIES
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    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
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    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/232—Angelica
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Abstract

The invention relates to a pharmaceutical composition and a preparation method thereof. On one hand, the provided tablet-form traditional Chinese medicine composition is prepared from the following traditional Chinese medicinal materials in parts by weight and a proper amount of auxiliary materials: 24-30 g of pollen typhae, 17-21 g of pulvis Fumi Carbonisatus, 0.1-0.5 ml of fennel oil, 390-475 g of motherwort, 24-30 g of prepared rehmannia root, 24-30 g of common burreed rhizome, 24-30 g of mugwort leaf (charcoal), 73-89 g of rhizoma corydalis, 146-178 g of nutgrass galingale rhizome, 73-89 g of white paeony root, 24-30 g of costustoot, 24-30 g of malaytea scurfpea fruit, 24-30 g of evodia rutaecarpa, 73-89 g of szechuan lovage rhizome, 24-30 g of zedoary and 24-30 g of Chinese angelica. Also provided are methods of preparing the tablets and their pharmaceutical uses. The tablet can be used for regulating menstruation and removing blood stasis clinically, and has excellent treatment effect on qi stagnation, chest and hypochondrium stabbing pain, postpartum blood stasis, lower abdomen pain, dysphoria with feverish sensation in the chest and abdomen and emaciation with yellowish complexion.

Description

Pharmaceutical composition and preparation method thereof
Technical Field
The invention belongs to the technical field of medicines, and relates to an aconite tablet and a preparation method thereof.
Background
Wujin tablet has been received on page 21 of the seventeenth book of Chinese medicinal prescription preparation, standard number WS3-B-3142-98. The prescription of the Wujin tablet is as follows: pollen typhae 30g, pulvis Fumi Carbonisatus 21g, fennel oil 0.15ml, motherwort 480g, prepared rehmannia root 30g, rhizoma sparganii 30g, mugwort leaf (charcoal) 30g, rhizoma corydalis 90g, nutgrass galingale rhizome 180g, white paeony root 90g, costustoot 30g, malaytea scurfpea fruit 30g, evodia rutaecarpa 30g, szechuan lovage rhizome 90g, zedoary 30g and Chinese angelica 30g.
In the above standard, the preparation method of the aconite tablet is described as follows: the sixteen materials are respectively crushed into fine powder and sieved; dissolving oleum Foeniculi in ethanol; decocting herba Leonuri, radix rehmanniae Preparata, and rhizoma Sparganii with water for two times, the first time for 3 hr and the second time for 2 hr; soaking folium Artemisiae Argyi in water at 80deg.C for 2 hr; mixing the above water extractive solutions and warm extract, filtering, concentrating the filtrate into paste (relative density 1.20-1.30, 50-60deg.C); reflux-extracting rhizoma corydalis, rhizoma Cyperi, radix Paeoniae alba, radix aucklandiae, fructus Psoraleae, fructus evodiae, rhizoma Ligustici Chuanxiong and Curcumae rhizoma with 60% ethanol for three times, the first time for 6 hr, the second time for 4 hr, and the third time for 2 hr; extracting radix Angelicae sinensis for three times, reflux-extracting with ethanol for 8 hr, reflux-extracting with 60% ethanol for two times, reflux-extracting for 4 hr, reflux-extracting for 2 hr, mixing the above ethanol extractive solutions, filtering, recovering ethanol, and concentrating into paste; mixing the water and ethanol concentrated extracts, adding fine powder such as pollen Typhae and adjuvant, granulating, drying, cooling, adding oleum Foeniculi solution, mixing, and pressing into 1110 tablets to obtain tablets each weighing 0.6 g.
The formula of the existing quality standard of the Wujin tablet is the same as the formula of the standard WS3-B-3142-98, but the formula is expressed by the amount of 1000 tablets, and the specific formula is as follows: pollen typhae 27.03g, pulvis Fumi Carbonisatus 18.92g, fennel oil 0.135ml, motherwort 432.43g, prepared rehmannia root 27.03g, rhizoma sparganii 27.03g, mugwort leaf (charcoal) 27.03g, rhizoma corydalis 81.08g, nutgrass flatsedge 162.16g, white peony root 81.08g, costustoot 27.03g, psoralea fruit 27.03g, evodia rutaecarpa 27.03g, ligusticum chuanxiong 81.08g, zedoary 27.03g and Chinese angelica 27.03g. The existing quality standard of the Wujin tablet is basically the same as the standard WS3-B-3142-98 method, and is summarized as follows: the sixteen materials are respectively crushed into fine powder and sieved; dissolving oleum Foeniculi in ethanol; decocting herba Leonuri, radix rehmanniae Preparata, and rhizoma Sparganii with water twice, adding 12 times of water for the first time, soaking for 0.5 hr, decocting for 3 hr, adding 8 times of water for the second time, and decocting for 2 hr; soaking folium Artemisiae Argyi in 12 times of water for 0.5 hr, boiling, and soaking at 80deg.C for 2 hr; mixing the above water extractive solutions and the warm extract, filtering, and concentrating the filtrate into paste (relative density of 1.20-1.30, 50-60deg.C); reflux-extracting rhizoma corydalis, rhizoma Cyperi, radix Paeoniae alba, radix aucklandiae, fructus Psoraleae, fructus evodiae, rhizoma Ligustici Chuanxiong and Curcumae rhizoma with 60% ethanol for three times, the first 6 hr, the second 4 hr, and the third 2 hr, with alcohol addition of 8 times, 6 times and 6 times respectively; extracting radix Angelicae sinensis for three times, reflux-extracting with 8 times of ethanol for 8 hr, reflux-extracting with 60% ethanol for two times, the first time for 4 hr, and the second time for 2 hr, wherein the ethanol addition amounts are 6 times and 6 times respectively; mixing the above ethanol extractive solutions, filtering, recovering ethanol, and concentrating into paste; mixing the water and ethanol concentrated extracts, adding fine powder such as pollen Typhae and appropriate amount of starch, dextrin and magnesium stearate, granulating, drying, cooling, adding anisole solution, mixing, and pressing into 1000 tablets to obtain tablet with weight of 0.6 g.
The wujin tablets are orally administered, 4 tablets at a time, which is quite difficult to take for tablets weighing up to 0.6g each. Thus, a new method for preparing an aconite tablet, for example, the administration weight of the finished drug is reduced but the typical active substances of the drug remain substantially unchanged, is highly desired by those skilled in the art.
Disclosure of Invention
The invention aims to provide an aconite tablet which has the effects of regulating menstruation and removing blood stasis and can be clinically used for treating qi stagnation, chest and hypochondrium stabbing pain, postpartum blood stasis, lower abdomen pain, dysphoria with feverish sensation in the chest and hypochondrium and emaciation with yellowish complexion. It has been found that by the process of the present invention, the weight of the final product tablet can be advantageously reduced, allowing the patient to conveniently take it, and the typical chemical active substance of the freshly prepared aconite tablet remains substantially unchanged and/or the biological activity remains substantially unchanged.
For this reason, the first aspect of the present invention relates to a Chinese medicinal composition in the form of a tablet, which may be called as an aconite tablet, and is prepared from the following Chinese medicinal materials in parts by weight and a proper amount of auxiliary materials: 24-30 g of pollen typhae, 17-21 g of pulvis Fumi Carbonisatus, 0.1-0.5 ml of fennel oil, 390-475 g of motherwort, 24-30 g of prepared rehmannia root, 24-30 g of common burreed rhizome, 24-30 g of mugwort leaf (charcoal), 73-89 g of rhizoma corydalis, 146-178 g of nutgrass galingale rhizome, 73-89 g of white paeony root, 24-30 g of costustoot, 24-30 g of malaytea scurfpea fruit, 24-30 g of evodia rutaecarpa, 73-89 g of szechuan lovage rhizome, 24-30 g of zedoary and 24-30 g of Chinese angelica.
The traditional Chinese medicine composition according to the first aspect of the invention is prepared from the following traditional Chinese medicinal materials in parts by weight and a proper amount of auxiliary materials: pollen typhae 27.03g, pulvis Fumi Carbonisatus 18.92g, fennel oil 0.135ml, motherwort 432.43g, prepared rehmannia root 27.03g, rhizoma sparganii 27.03g, mugwort leaf (charcoal) 27.03g, rhizoma corydalis 81.08g, nutgrass flatsedge 162.16g, white peony root 81.08g, costustoot 27.03g, psoralea fruit 27.03g, evodia rutaecarpa 27.03g, ligusticum chuanxiong 81.08g, zedoary 27.03g and Chinese angelica 27.03g.
The traditional Chinese medicine composition according to the first aspect of the invention is prepared from the following traditional Chinese medicinal materials and proper amount of auxiliary materials in parts by weight: 24-30 g of pollen typhae, 17-21 g of pulvis Fumi Carbonisatus, 0.1-0.5 ml of fennel oil, 390-475 g of motherwort, 24-30 g of prepared rehmannia root, 24-30 g of common burreed rhizome, 24-30 g of mugwort leaf (charcoal), 73-89 g of rhizoma corydalis, 146-178 g of nutgrass galingale rhizome, 73-89 g of white paeony root, 24-30 g of costustoot, 24-30 g of malaytea scurfpea fruit, 24-30 g of evodia rutaecarpa, 73-89 g of szechuan lovage rhizome, 24-30 g of zedoary and 24-30 g of Chinese angelica.
The traditional Chinese medicine composition according to the first aspect of the invention is prepared from the following traditional Chinese medicinal materials and proper amount of auxiliary materials in parts by weight: pollen typhae 27.03g, pulvis Fumi Carbonisatus 18.92g, fennel oil 0.135ml, motherwort 432.43g, prepared rehmannia root 27.03g, rhizoma sparganii 27.03g, mugwort leaf (charcoal) 27.03g, rhizoma corydalis 81.08g, nutgrass flatsedge 162.16g, white peony root 81.08g, costustoot 27.03g, psoralea fruit 27.03g, evodia rutaecarpa 27.03g, ligusticum chuanxiong 81.08g, zedoary 27.03g and Chinese angelica 27.03g.
The weight of each tablet of the traditional Chinese medicine composition according to the first aspect of the invention is 300-600 mg.
The weight of each tablet of the traditional Chinese medicine composition according to the first aspect of the invention is 300-500 mg.
The weight of each tablet of the traditional Chinese medicine composition according to the first aspect of the invention is 300-400 mg.
The Chinese medicinal composition according to the first aspect of the invention has a tablet weight of 350mg per tablet.
The traditional Chinese medicine composition according to the first aspect of the invention, wherein the auxiliary materials comprise a lubricant and a filler. For example, the lubricant is selected from: stearic acid, magnesium stearate, calcium stearate, or combinations thereof. For example, the filler is selected from: starch, dextrin, sucrose, lactose, or a combination thereof.
The Chinese medicinal composition according to the first aspect of the present invention contains 0.5 to 1.5% of magnesium stearate, for example, 1% of magnesium stearate.
The traditional Chinese medicine composition according to the first aspect of the invention comprises starch and dextrin, for example, the weight ratio of the starch to the dextrin is 1:2, for example, in an amount such that the tablet weight reaches a prescribed tablet weight.
The traditional Chinese medicine composition according to the first aspect of the invention is prepared according to a method comprising the following steps:
(1) Pulverizing pollen Typhae and pulvis Fumi Carbonisatus respectively into fine powder, sieving, and mixing to obtain medicinal powder;
(2) Dissolving oleum Foeniculi in ethanol (for example, 10-20 times volume of oleum Foeniculi such as about 15 times volume) for use;
(3) Decocting herba Leonuri, radix rehmanniae Preparata, and rhizoma Sparganii with water twice (for example, adding 12 times of water for the first time, soaking for 0.5 hr, decocting for 3 hr, adding 8 times of water for the second time, decocting for 2 hr), and filtering to obtain water extract; soaking folium Artemisiae Argyi in water at 80deg.C (for example, 12 times of water for 0.5 hr, boiling, soaking at 80deg.C for 2 hr), and filtering to obtain soaking solution; mixing the above water extractive solutions and the warm extract, filtering, and concentrating the filtrate into paste;
(4) Reflux-extracting rhizoma corydalis, rhizoma Cyperi, radix Paeoniae alba, radix aucklandiae, fructus Psoraleae, fructus evodiae, rhizoma Ligustici Chuanxiong, and Curcumae rhizoma with 60% ethanol for three times (for example, 6 hr for the first time, 4 hr for the second time, and 2 hr for the third time, with ethanol addition of 8 times, 6 times, and 6 times respectively), mixing the three extractive solutions, and filtering to obtain ethanol extractive solution; reflux-extracting radix Angelicae sinensis with ethanol for three times (for example, reflux-extracting with 8 times of ethanol for 8 hr for the first time, reflux-extracting with 60% ethanol for two times, reflux-extracting for 4 hr for the first time and reflux-extracting for 2 hr for the second time, adding 6 times of ethanol and 6 times of ethanol respectively), mixing the three extractive solutions, and filtering to obtain ethanol extractive solution; mixing the above ethanol extractive solutions, filtering, recovering ethanol, and concentrating into paste;
(5) Mixing the water and ethanol concentrated extracts, adding pollen Typhae and pulvis Fumi Carbonisatus fine powder, starch, dextrin, and magnesium stearate, granulating, drying, cooling, adding oleum Foeniculi solution, mixing, and tabletting.
Further, the second aspect of the present invention provides a method for preparing the Chinese medicinal composition in the form of a tablet according to any one of the first aspect of the present invention, comprising the steps of:
(1) Pulverizing pollen Typhae and pulvis Fumi Carbonisatus respectively into fine powder, sieving, and mixing to obtain medicinal powder;
(2) Dissolving oleum Foeniculi in ethanol (for example, 10-20 times volume of oleum Foeniculi such as about 15 times volume) for use;
(3) Decocting herba Leonuri, radix rehmanniae Preparata, and rhizoma Sparganii with water twice (for example, adding 12 times of water for the first time, soaking for 0.5 hr, decocting for 3 hr, adding 8 times of water for the second time, decocting for 2 hr), and filtering to obtain water extract; soaking folium Artemisiae Argyi in water at 80deg.C (for example, 12 times of water for 0.5 hr, boiling, soaking at 80deg.C for 2 hr), and filtering to obtain soaking solution; mixing the above water extractive solutions and the warm extract, filtering, and concentrating the filtrate into paste;
(4) Reflux-extracting rhizoma corydalis, rhizoma Cyperi, radix Paeoniae alba, radix aucklandiae, fructus Psoraleae, fructus evodiae, rhizoma Ligustici Chuanxiong, and Curcumae rhizoma with 60% ethanol for three times (for example, 6 hr for the first time, 4 hr for the second time, and 2 hr for the third time, with ethanol addition of 8 times, 6 times, and 6 times respectively), mixing the three extractive solutions, and filtering to obtain ethanol extractive solution; reflux-extracting radix Angelicae sinensis with ethanol for three times (for example, reflux-extracting with 8 times of ethanol for 8 hr for the first time, reflux-extracting with 60% ethanol for two times, reflux-extracting for 4 hr for the first time and reflux-extracting for 2 hr for the second time, adding 6 times of ethanol and 6 times of ethanol respectively), mixing the three extractive solutions, and filtering to obtain ethanol extractive solution; mixing the above ethanol extractive solutions, filtering, recovering ethanol, and concentrating into paste;
(5) Mixing the water and ethanol concentrated extracts, adding pollen Typhae and pulvis Fumi Carbonisatus fine powder, starch, dextrin, and magnesium stearate, granulating, drying, cooling, adding oleum Foeniculi solution, mixing, and tabletting.
In any one of the embodiments according to any one of the aspects of the present invention, in preparing the Chinese medicinal composition in the form of a tablet, after filtering the combined aqueous extract and warm immersion liquid in step (3), citric acid and kaolin are added to the filtrate, uniformly mixed, and then concentrated into a paste; for example, each 432.43g of the motherwort is added with 2 to 2.5g of citric acid; for example, the amount of kaolin added to each 432.43g of motherwort herb is 8-9 g.
Further, the third aspect of the present invention provides the use of the tablet-form Chinese medicinal composition according to any one of the first aspect of the present invention for preparing a medicament for regulating menstruation and removing blood stasis; for example, in the preparation of medicaments for treating qi stagnation, chest and hypochondrium pain, postpartum blood stasis, lower abdomen pain, dysphoria with feverish sensation in the chest and abdomen and emaciation with yellowish complexion.
The prepared aconite gold slice has excellent effects as described above and below.
Detailed Description
The invention provides the following specific examples to further illustrate various aspects of the invention.
In the following specific examples, tablets were compressed by selecting a round die of a suitable size for the designed tablet weight, compressing the tablets with a force of 6.5 to 8kg, and sealing and packaging the compressed tablets with an aluminum plastic blister after the compressed tablets were left for 4 to 5 hours.
Example 1: preparing a Chinese medicinal composition in the form of tablet (i.e. Wujin tablet)
To prepare the formula and the amount of 1000 tablets:
27.03g of pollen typhae, 18.92g of pulvis Fumi Carbonisatus, 0.135ml of fennel oil,
432.43g of motherwort herb, 27.03g of prepared rehmannia root, 27.03g of common burreed rhizome, 27.03g of Chinese mugwort leaf (charcoal),
81.08g of rhizoma corydalis, 162.16g of rhizoma cyperi, 81.08g of radix paeoniae alba, 27.03g of radix aucklandiae, 27.03g of fructus psoraleae, 27.03g of fructus evodiae, 81.08g of rhizoma ligustici wallichii, 27.03g of rhizoma curcumae and 27.03g of angelica,
starch, dextrin and magnesium stearate are added in the amounts shown in the following preparation methods.
The preparation method comprises the following steps:
pulverizing pollen Typhae and pulvis Fumi Carbonisatus respectively into fine powder, sieving, and mixing to obtain 45.95g of medicinal powder;
dissolving oleum Foeniculi (0.135 ml) with appropriate amount of ethanol (2 ml) for use;
decocting herba Leonuri, radix rehmanniae Preparata, and rhizoma Sparganii (486.49 g in total) with water twice, adding 12 times of water for the first time, soaking for 0.5 hr, decocting for 3 hr, adding 8 times of water for the second time, decocting for 2 hr, and filtering to obtain water extractive solution (73.94 g if it is concentrated and dried to water content of less than 5%);
Soaking folium Artemisiae Argyi (27.03 g) in 12 times of water for 0.5 hr, boiling, soaking at 80deg.C for 2 hr, filtering to obtain a warm soaking solution (if it is concentrated and dried to water content less than 5%, the weight of the obtained dry granule is 3.67 g);
mixing the above water extractive solutions and the warm extract, filtering, and concentrating the filtrate into paste (relative density of 1.20-1.30, 50-60deg.C);
reflux-extracting rhizoma corydalis, rhizoma Cyperi, radix Paeoniae alba, radix aucklandiae, fructus Psoraleae, fructus evodiae, rhizoma Ligustici Chuanxiong, and Curcumae rhizoma (513.51 g in total) with 60% ethanol for three times (6 hr for the first time, 4 hr for the second time, and 2 hr for the third time), adding 8 times, 6 times, and 6 times of ethanol respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution (59.47 g dry granule weight if concentrated and dried to water content less than 5%);
extracting radix Angelicae sinensis (27.03 g) for three times, reflux-extracting with 8 times of ethanol for 8 hr for two times with 60% ethanol for 4 hr, reflux-extracting for 2 hr for 6 times and 6 times of ethanol respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution (the weight of the obtained dry granule is 2.82g if it is concentrated and dried to water content of less than 5%);
mixing the above ethanol extractive solutions, filtering, recovering ethanol, and concentrating into paste;
Mixing the water and ethanol concentrated extracts, adding pollen Typhae fine powder, starch, dextrin, and magnesium stearate, granulating, drying, cooling, adding oleum Foeniculi solution, mixing, and pressing into 1000 tablets to obtain 600mg tablet.
The above magnesium stearate was added in an amount of 1% by weight of the tablet (about 6 mg/tablet added in this example), and the weight ratio of starch to dextrin was 1:2 and an appropriate amount to a total weight of 600mg per tablet (the total amount of both added starch and dextrin in this example is about 408 mg/tablet).
The water extract of motherwort, the mugwort leaf warm extract, the tetrahydropalmatine and the angelica alcohol extract are all fed in an amount which is 2 times (namely 2000 tablets), the obtained extract is divided into 2 parts, one part is used for continuously preparing 1000 tablets, and the other part is used for measuring the dry matter mass in the extract; for example, as shown in the water extract of leonurus, the dried particles obtained by concentrating and drying the water extract until the water content is less than 5% have a weight of 73.94g (72.38 g to 76.34 g); the remaining embodiments of the present invention can similarly yield dry matter weights in different extraction steps; for example, the dry matter weights of the extracts of the mugwort leaf, the corydalis tuber and the angelica are respectively 3.67g (3.5 g-3.67 g), 59.47g (57.03 g-60.12 g) and 2.82g (2.82 g-2.94 g) which are also measured by a similar method. Of course, 73.94g of the above water extract such as leonurus can also be measured by the following method: precisely measuring the right amount of the obtained water extract such as motherwort, removing the solvent by a proper method such as a volatilizing solvent method to obtain a dry matter with the water content less than 5%, thereby converting the measured water extract into the subsequent dry particle amount, and adding the dry matter obtained by volatilizing the solvent back into the water extract, so that the method can dispense with 2000 tablets.
Example 2: preparing a Chinese medicinal composition in the form of tablet (i.e. Wujin tablet)
To prepare the formula and the amount of 1000 tablets:
27.03g of pollen typhae, 18.92g of pulvis Fumi Carbonisatus, 0.135ml of fennel oil,
432.43g of motherwort herb, 27.03g of prepared rehmannia root, 27.03g of common burreed rhizome, 27.03g of Chinese mugwort leaf (charcoal),
81.08g of rhizoma corydalis, 162.16g of rhizoma cyperi, 81.08g of radix paeoniae alba, 27.03g of radix aucklandiae, 27.03g of fructus psoraleae, 27.03g of fructus evodiae, 81.08g of rhizoma ligustici wallichii, 27.03g of rhizoma curcumae and 27.03g of angelica,
starch, dextrin and magnesium stearate are added in the amounts shown in the following preparation methods.
The preparation method comprises the following steps:
pulverizing pollen Typhae and pulvis Fumi Carbonisatus respectively into fine powder, sieving, and mixing to obtain 45.95g of medicinal powder;
dissolving oleum Foeniculi (0.135 ml) with appropriate amount of ethanol (2 ml) for use;
decocting herba Leonuri, radix rehmanniae Preparata, and rhizoma Sparganii (486.49 g in total) with water twice, adding 12 times of water for the first time, soaking for 0.5 hr, decocting for 3 hr, adding 8 times of water for the second time, decocting for 2 hr, and filtering to obtain water extractive solution (76.34 g if it is concentrated and dried to water content less than 5%);
soaking folium Artemisiae Argyi (27.03 g) in 12 times of water for 0.5 hr, boiling, soaking at 80deg.C for 2 hr, filtering to obtain a warm soaking solution (if it is concentrated and dried to water content less than 5%, the weight of the obtained dry granule is 3.5 g);
Mixing the above water extractive solutions and the warm extract, filtering, and concentrating the filtrate into paste (relative density of 1.20-1.30, 50-60deg.C);
reflux-extracting rhizoma corydalis, rhizoma Cyperi, radix Paeoniae alba, radix aucklandiae, fructus Psoraleae, fructus evodiae, rhizoma Ligustici Chuanxiong, and Curcumae rhizoma (513.51 g in total) with 60% ethanol for three times (6 hr for the first time, 4 hr for the second time, and 2 hr for the third time), adding 8 times, 6 times, and 6 times of ethanol respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution (60.12 g dry granule weight if concentrated and dried to water content less than 5%);
extracting radix Angelicae sinensis (27.03 g) for three times, reflux-extracting with 8 times of ethanol for 8 hr for two times with 60% ethanol for 4 hr, reflux-extracting for 2 hr for 6 times and 6 times of ethanol respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution (the weight of the obtained dry granule is 2.94g if it is concentrated and dried to water content of less than 5%);
mixing the above ethanol extractive solutions, filtering, recovering ethanol, and concentrating into paste;
mixing the water and ethanol concentrated extracts, adding pollen Typhae fine powder, starch, dextrin, and magnesium stearate, granulating, drying, cooling, adding oleum Foeniculi solution, mixing, and pressing into 1000 tablets to obtain 600mg tablet.
The above magnesium stearate was added in an amount of 1% by weight of the tablet (about 6 mg/tablet added in this example), and the weight ratio of starch to dextrin was 1:2 and an appropriate amount to a total weight of 600mg per tablet (the total amount of added starch and dextrin in this example is about 405 mg/tablet).
Example 3: preparing a Chinese medicinal composition in the form of tablet (i.e. Wujin tablet)
To prepare the formula and the amount of 1000 tablets:
27.03g of pollen typhae, 18.92g of pulvis Fumi Carbonisatus, 0.135ml of fennel oil,
432.43g of motherwort herb, 27.03g of prepared rehmannia root, 27.03g of common burreed rhizome, 27.03g of Chinese mugwort leaf (charcoal),
81.08g of rhizoma corydalis, 162.16g of rhizoma cyperi, 81.08g of radix paeoniae alba, 27.03g of radix aucklandiae, 27.03g of fructus psoraleae, 27.03g of fructus evodiae, 81.08g of rhizoma ligustici wallichii, 27.03g of rhizoma curcumae and 27.03g of angelica,
starch, dextrin and magnesium stearate are added in the amounts shown in the following preparation methods.
The preparation method comprises the following steps:
pulverizing pollen Typhae and pulvis Fumi Carbonisatus respectively into fine powder, sieving, and mixing to obtain 45.95g of medicinal powder;
dissolving oleum Foeniculi (0.135 ml) with appropriate amount of ethanol (2 ml) for use;
decocting herba Leonuri, radix rehmanniae Preparata, and rhizoma Sparganii (486.49 g in total) with water twice, adding 12 times of water for the first time, soaking for 0.5 hr, decocting for 3 hr, adding 8 times of water for the second time, decocting for 2 hr, and filtering to obtain water extractive solution (72.38 g if it is concentrated and dried to water content of less than 5%);
Soaking folium Artemisiae Argyi (27.03 g) in 12 times of water for 0.5 hr, boiling, soaking at 80deg.C for 2 hr, filtering to obtain a warm soaking solution (if it is concentrated and dried to water content less than 5%, the weight of the obtained dry granule is 3.56 g);
mixing the above water extractive solutions and the warm extract, filtering, and concentrating the filtrate into paste (relative density of 1.20-1.30, 50-60deg.C);
reflux-extracting rhizoma corydalis, rhizoma Cyperi, radix Paeoniae alba, radix aucklandiae, fructus Psoraleae, fructus evodiae, rhizoma Ligustici Chuanxiong, and Curcumae rhizoma (513.51 g in total) with 60% ethanol for three times (6 hr for the first time, 4 hr for the second time, and 2 hr for the third time), adding 8 times, 6 times, and 6 times of ethanol respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution (57.03 g dry granule weight if concentrated and dried to water content less than 5%);
extracting radix Angelicae sinensis (27.03 g) for three times, reflux-extracting with 8 times of ethanol for 8 hr for two times with 60% ethanol for 4 hr, reflux-extracting for 2 hr for 6 times and 6 times of ethanol respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution (the weight of the obtained dry granule is 2.93g if it is concentrated and dried to water content of less than 5%);
mixing the above ethanol extractive solutions, filtering, recovering ethanol, and concentrating into paste;
Mixing the water and ethanol concentrated extracts, adding pollen Typhae fine powder, starch, dextrin, and magnesium stearate, granulating, drying, cooling, adding oleum Foeniculi solution, mixing, and pressing into 1000 tablets to obtain 600mg tablet.
The above magnesium stearate was added in an amount of 1% by weight of the tablet (about 6 mg/tablet added in this example), and the weight ratio of starch to dextrin was 1:2 and an appropriate amount to a total weight of 600mg per tablet (the total amount of both added starch and dextrin in this example is about 412 mg/tablet).
Examples 1-3 above were prepared essentially according to the calendar version of the drug standard, each tablet weighing 600mg, containing more than two-thirds of the adjuvant, the tablet weight being very large and 4 tablets each time, being very uncomfortable to take, reducing the tablet weight being very significant for the patient. In the following examples, the inventors tried to reduce the amount of auxiliary materials without changing the basic preparation process of the drug, i.e., the process of the extraction stage of the drug, in order to reduce the tablet weight.
Example 4: preparing a Chinese medicinal composition in the form of tablet (i.e. Wujin tablet)
To prepare the formula and the amount of 1000 tablets:
27.03g of pollen typhae, 18.92g of pulvis Fumi Carbonisatus, 0.135ml of fennel oil,
432.43g of motherwort herb, 27.03g of prepared rehmannia root, 27.03g of common burreed rhizome, 27.03g of Chinese mugwort leaf (charcoal),
81.08g of rhizoma corydalis, 162.16g of nutgrass galingale rhizome, 81.08g of white peony root, 27.03g of costustoot, 27.03g of malaytea scurfpea fruit, 27.03g of evodia rutaecarpa, 81.08g of szechuan lovage rhizome, 27.03g of zedoary, 27.03g of Chinese angelica, and the following components of starch, dextrin and magnesium stearate are added according to the amounts shown in the following preparation methods.
The preparation method comprises the following steps:
pulverizing pollen Typhae and pulvis Fumi Carbonisatus respectively into fine powder, sieving, and mixing to obtain 45.95g of medicinal powder;
dissolving oleum Foeniculi (0.135 ml) with appropriate amount of ethanol (2 ml) for use;
decocting herba Leonuri, radix rehmanniae Preparata, and rhizoma Sparganii with water twice, adding 12 times of water for soaking for 0.5 hr, decocting for 3 hr, adding 8 times of water for 2 hr, and filtering to obtain water extractive solution;
soaking folium Artemisiae Argyi in 12 times of water for 0.5 hr, boiling, soaking at 80deg.C for 2 hr, and filtering to obtain a warm soaking solution;
mixing the above water extract and the warm extract, filtering, adding 2.3g of citric acid and 8.5g of Kaolin to the filtrate (which contains about 77.2g of solid matters by sampling and measuring, and is consistent with the solid matters in the water extract and the warm extract of examples 1-3), uniformly mixing, and concentrating to obtain paste (the relative density is 1.20-1.30, 50-60 ℃).
Reflux-extracting rhizoma corydalis, rhizoma Cyperi, radix Paeoniae alba, radix aucklandiae, fructus Psoraleae, fructus evodiae, rhizoma Ligustici Chuanxiong and Curcumae rhizoma with 60% ethanol for three times, the first time for 6 hr, the second time for 4 hr, and the third time for 2 hr, with ethanol addition amounts of 8 times, 6 times and 6 times respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution;
Extracting radix Angelicae sinensis for three times, reflux-extracting with 8 times of ethanol for 8 hr, reflux-extracting with 60% ethanol for two times, reflux-extracting for 4 hr, reflux-extracting for 2 hr, adding 6 times of ethanol and 6 times of ethanol respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution;
mixing the above ethanol extracts (containing about 61.3g of solids, which is consistent with the amount of solids in the mixed ethanol extracts of examples 1-3, by sampling measurement), filtering, recovering ethanol, and concentrating into paste;
mixing the water and ethanol concentrated extracts, adding pollen Typhae fine powder, starch, dextrin, and magnesium stearate, granulating, drying, cooling, adding oleum Foeniculi solution, mixing, and pressing into 1000 tablets. The above magnesium stearate was added in an amount of 1% by weight of the tablet (about 3.5 mg/tablet added in this example), and the weight ratio of starch to dextrin was 1:2 and an appropriate amount to the total weight of 350mg per tablet (the total amount of both added starch and dextrin in this example is about 151.1 mg/tablet).
Example 5: preparing a Chinese medicinal composition in the form of tablet (i.e. Wujin tablet)
To prepare the formula and the amount of 1000 tablets:
27.03g of pollen typhae, 18.92g of pulvis Fumi Carbonisatus, 0.135ml of fennel oil,
432.43g of motherwort herb, 27.03g of prepared rehmannia root, 27.03g of common burreed rhizome, 27.03g of Chinese mugwort leaf (charcoal),
81.08g of rhizoma corydalis, 162.16g of nutgrass galingale rhizome, 81.08g of white peony root, 27.03g of costustoot, 27.03g of malaytea scurfpea fruit, 27.03g of evodia rutaecarpa, 81.08g of szechuan lovage rhizome, 27.03g of zedoary, 27.03g of Chinese angelica, and the following components of starch, dextrin and magnesium stearate are added according to the amounts shown in the following preparation methods.
The preparation method comprises the following steps:
pulverizing pollen Typhae and pulvis Fumi Carbonisatus respectively into fine powder, sieving, and mixing to obtain 45.95g of medicinal powder;
dissolving oleum Foeniculi (0.135 ml) with appropriate amount of ethanol (2 ml) for use;
decocting herba Leonuri, radix rehmanniae Preparata, and rhizoma Sparganii with water twice, adding 12 times of water for soaking for 0.5 hr, decocting for 3 hr, adding 8 times of water for 2 hr, and filtering to obtain water extractive solution;
soaking folium Artemisiae Argyi in 12 times of water for 0.5 hr, boiling, soaking at 80deg.C for 2 hr, and filtering to obtain a warm soaking solution;
mixing the above water extractive solutions and the warm extract, filtering, adding citric acid 2g and Kaolin 9g into filtrate (containing solid matter about 76.4g by sampling measurement), mixing, and concentrating into paste (relative density 1.20-1.30, 50-60deg.C).
Reflux-extracting rhizoma corydalis, rhizoma Cyperi, radix Paeoniae alba, radix aucklandiae, fructus Psoraleae, fructus evodiae, rhizoma Ligustici Chuanxiong and Curcumae rhizoma with 60% ethanol for three times, the first time for 6 hr, the second time for 4 hr, and the third time for 2 hr, with ethanol addition amounts of 8 times, 6 times and 6 times respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution;
Extracting radix Angelicae sinensis for three times, reflux-extracting with 8 times of ethanol for 8 hr, reflux-extracting with 60% ethanol for two times, reflux-extracting for 4 hr, reflux-extracting for 2 hr, adding 6 times of ethanol and 6 times of ethanol respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution;
mixing the above ethanol extractive solutions (containing about 62.5g of solid matters by sampling measurement), filtering, recovering ethanol, and concentrating into paste;
mixing the water and ethanol concentrated extracts, adding pollen Typhae fine powder, starch, dextrin, and magnesium stearate, granulating, drying, cooling, adding oleum Foeniculi solution, mixing, and pressing into 1000 tablets. The above magnesium stearate was added in an amount of 1% by weight of the tablet (about 3.5 mg/tablet added in this example), and the weight ratio of starch to dextrin was 1:2 and an appropriate amount to the total weight of 350mg per tablet (the total amount of both added starch and dextrin in this example is about 150.5 mg/tablet).
Example 6: preparing a Chinese medicinal composition in the form of tablet (i.e. Wujin tablet)
To prepare the formula and the amount of 1000 tablets:
27.03g of pollen typhae, 18.92g of pulvis Fumi Carbonisatus, 0.135ml of fennel oil,
432.43g of motherwort herb, 27.03g of prepared rehmannia root, 27.03g of common burreed rhizome, 27.03g of Chinese mugwort leaf (charcoal),
81.08g of rhizoma corydalis, 162.16g of nutgrass galingale rhizome, 81.08g of white peony root, 27.03g of costustoot, 27.03g of malaytea scurfpea fruit, 27.03g of evodia rutaecarpa, 81.08g of szechuan lovage rhizome, 27.03g of zedoary, 27.03g of Chinese angelica, and the following components of starch, dextrin and magnesium stearate are added according to the amounts shown in the following preparation methods.
The preparation method comprises the following steps:
pulverizing pollen Typhae and pulvis Fumi Carbonisatus respectively into fine powder, sieving, and mixing to obtain 45.95g of medicinal powder;
dissolving oleum Foeniculi (0.135 ml) with appropriate amount of ethanol (2 ml) for use;
decocting herba Leonuri, radix rehmanniae Preparata, and rhizoma Sparganii with water twice, adding 12 times of water for soaking for 0.5 hr, decocting for 3 hr, adding 8 times of water for 2 hr, and filtering to obtain water extractive solution;
soaking folium Artemisiae Argyi in 12 times of water for 0.5 hr, boiling, soaking at 80deg.C for 2 hr, and filtering to obtain a warm soaking solution;
mixing the above water extractive solutions and the warm extract, filtering, adding citric acid 2.5g and Kaolinitum 8g into filtrate (containing solid matter about 78.3g by sampling measurement), mixing, and concentrating into paste (relative density 1.20-1.30, 50-60deg.C).
Reflux-extracting rhizoma corydalis, rhizoma Cyperi, radix Paeoniae alba, radix aucklandiae, fructus Psoraleae, fructus evodiae, rhizoma Ligustici Chuanxiong and Curcumae rhizoma with 60% ethanol for three times, the first time for 6 hr, the second time for 4 hr, and the third time for 2 hr, with ethanol addition amounts of 8 times, 6 times and 6 times respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution;
extracting radix Angelicae sinensis for three times, reflux-extracting with 8 times of ethanol for 8 hr, reflux-extracting with 60% ethanol for two times, reflux-extracting for 4 hr, reflux-extracting for 2 hr, adding 6 times of ethanol and 6 times of ethanol respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution;
Mixing the above ethanol extractive solutions (containing about 60.6g of solid matters by sampling measurement), filtering, recovering ethanol, and concentrating into paste;
mixing the water and ethanol concentrated extracts, adding pollen Typhae fine powder, starch, dextrin, and magnesium stearate, granulating, drying, cooling, adding oleum Foeniculi solution, mixing, and pressing into 1000 tablets. The above magnesium stearate was added in an amount of 1% by weight of the tablet (about 3.5 mg/tablet added in this example), and the weight ratio of starch to dextrin was 1:2 and an appropriate amount to the total weight of 350mg per tablet (the total amount of both added starch and dextrin in this example is about 151 mg/tablet).
Example 7: preparing a Chinese medicinal composition in the form of tablet (i.e. Wujin tablet)
To prepare the formula and the amount of 1000 tablets:
27.03g of pollen typhae, 18.92g of pulvis Fumi Carbonisatus, 0.135ml of fennel oil,
432.43g of motherwort herb, 27.03g of prepared rehmannia root, 27.03g of common burreed rhizome, 27.03g of Chinese mugwort leaf (charcoal),
81.08g of rhizoma corydalis, 162.16g of nutgrass galingale rhizome, 81.08g of white peony root, 27.03g of costustoot, 27.03g of malaytea scurfpea fruit, 27.03g of evodia rutaecarpa, 81.08g of szechuan lovage rhizome, 27.03g of zedoary, 27.03g of Chinese angelica, and the following components of starch, dextrin and magnesium stearate are added according to the amounts shown in the following preparation methods.
The preparation method comprises the following steps:
pulverizing pollen Typhae and pulvis Fumi Carbonisatus respectively into fine powder, sieving, and mixing to obtain 45.95g of medicinal powder;
Dissolving oleum Foeniculi (0.135 ml) with appropriate amount of ethanol (2 ml) for use;
decocting herba Leonuri, radix rehmanniae Preparata, and rhizoma Sparganii with water twice, adding 12 times of water for soaking for 0.5 hr, decocting for 3 hr, adding 8 times of water for 2 hr, and filtering to obtain water extractive solution;
soaking folium Artemisiae Argyi in 12 times of water for 0.5 hr, boiling, soaking at 80deg.C for 2 hr, and filtering to obtain a warm soaking solution;
mixing the above water extractive solutions and the warm extract, filtering, adding citric acid 2.3g and Kaolinitum 8.5g into filtrate (containing solid matter about 79.1g by sampling measurement), mixing, and concentrating into paste (relative density 1.20-1.30, 50-60deg.C);
reflux-extracting rhizoma corydalis, rhizoma Cyperi, radix Paeoniae alba, radix aucklandiae, fructus Psoraleae, fructus evodiae, rhizoma Ligustici Chuanxiong and Curcumae rhizoma with 60% ethanol for three times, the first time for 6 hr, the second time for 4 hr, and the third time for 2 hr, with ethanol addition amounts of 8 times, 6 times and 6 times respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution;
extracting radix Angelicae sinensis for three times, reflux-extracting with 8 times of ethanol for 8 hr, reflux-extracting with 60% ethanol for two times, reflux-extracting for 4 hr, reflux-extracting for 2 hr, adding 6 times of ethanol and 6 times of ethanol respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution;
Mixing the above ethanol extractive solutions (containing about 61.6g of solid matters by sampling measurement), filtering, recovering ethanol, and concentrating into paste;
mixing the water and ethanol concentrated extracts, adding pollen Typhae fine powder, starch, dextrin, and magnesium stearate, granulating, drying, cooling, adding oleum Foeniculi solution, mixing, and pressing into 1000 tablets. The above magnesium stearate was added in an amount of 1% by weight of the tablet (about 3 mg/tablet added in this example), and the weight ratio of starch to dextrin was 1:2 and an appropriate amount to a total weight of 300mg per tablet (the total amount of both added starch and dextrin in this example is about 99.4 mg/tablet).
Example 8: preparing a Chinese medicinal composition in the form of tablet (i.e. Wujin tablet)
To prepare the formula and the amount of 1000 tablets:
27.03g of pollen typhae, 18.92g of pulvis Fumi Carbonisatus, 0.135ml of fennel oil,
432.43g of motherwort herb, 27.03g of prepared rehmannia root, 27.03g of common burreed rhizome, 27.03g of Chinese mugwort leaf (charcoal),
81.08g of rhizoma corydalis, 162.16g of nutgrass galingale rhizome, 81.08g of white peony root, 27.03g of costustoot, 27.03g of malaytea scurfpea fruit, 27.03g of evodia rutaecarpa, 81.08g of szechuan lovage rhizome, 27.03g of zedoary, 27.03g of Chinese angelica, and the following components of starch, dextrin and magnesium stearate are added according to the amounts shown in the following preparation methods.
The preparation method comprises the following steps:
pulverizing pollen Typhae and pulvis Fumi Carbonisatus respectively into fine powder, sieving, and mixing to obtain 45.95g of medicinal powder;
Dissolving oleum Foeniculi (0.135 ml) with appropriate amount of ethanol (2 ml) for use;
decocting herba Leonuri, radix rehmanniae Preparata, and rhizoma Sparganii with water twice, adding 12 times of water for soaking for 0.5 hr, decocting for 3 hr, adding 8 times of water for 2 hr, and filtering to obtain water extractive solution;
soaking folium Artemisiae Argyi in 12 times of water for 0.5 hr, boiling, soaking at 80deg.C for 2 hr, and filtering to obtain a warm soaking solution;
mixing the above water extractive solutions and the warm extract, filtering, adding citric acid 2.3g and Kaolinitum 8.5g into filtrate (containing solid matter 77.8g by sampling measurement), mixing, and concentrating into paste (relative density 1.20-1.30, 50-60deg.C);
reflux-extracting rhizoma corydalis, rhizoma Cyperi, radix Paeoniae alba, radix aucklandiae, fructus Psoraleae, fructus evodiae, rhizoma Ligustici Chuanxiong and Curcumae rhizoma with 60% ethanol for three times, the first time for 6 hr, the second time for 4 hr, and the third time for 2 hr, with ethanol addition amounts of 8 times, 6 times and 6 times respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution;
extracting radix Angelicae sinensis for three times, reflux-extracting with 8 times of ethanol for 8 hr, reflux-extracting with 60% ethanol for two times, reflux-extracting for 4 hr, reflux-extracting for 2 hr, adding 6 times of ethanol and 6 times of ethanol respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution;
Mixing the above ethanol extractive solutions (containing about 62.2g of solid matters by sampling measurement), filtering, recovering ethanol, and concentrating into paste;
mixing the water and ethanol concentrated extracts, adding pollen Typhae fine powder, starch, dextrin, and magnesium stearate, granulating, drying, cooling, adding oleum Foeniculi solution, mixing, and pressing into 1000 tablets. The above magnesium stearate was added in an amount of 1% by weight of the tablet (about 4 mg/tablet added in this example), and the weight ratio of starch to dextrin was 1:2 and an appropriate amount to a total weight of 400mg per tablet (the total amount of both added starch and dextrin in this example is about 199.1 mg/tablet).
Example 11:referring to the formulation and preparation method of example 4, however, only 8.5g of Kaolinitum was added without adding citric acid to the filtrate obtained by mixing the water extract such as herba Leonuri with the folium Artemisiae Argyi warm extract, the other operations and the material addition amounts were the same, and finally precipitation was carried outThe powder and dextrin are added in proper amounts to the total weight of each tablet of 350mg and pressed into tablets.
Example 12:referring to the formulation and the preparation method of example 4, however, the filtrate obtained by mixing the water extract of motherwort and the like and the mugwort leaf warming extract was not added with kaolin, but only with 2.3g of citric acid, the rest of the operations and the material addition amounts were the same, and finally starch and dextrin were added in an appropriate amount to the total weight of each tablet of 350mg, and compressed into tablets.
Example 13:referring to the formulation and the preparation method of example 4, however, the filtrate obtained by mixing the water extract of motherwort and the like and the mugwort leaf warming extract was not added with kaolin nor citric acid, the rest of the operations and the material addition amounts were the same, and finally starch and dextrin were added in an appropriate amount to 350mg per total weight of tablet, and compressed into tablets.
Example 14:with reference to the formulation and process of example 4, but at the end stage, citric acid and kaolin are added together with the fine powder of pollen Typhae, etc., and finally starch and dextrin are added in an appropriate amount to the total weight of each tablet of 350mg, and compressed into tablets.
Example 15:with reference to the formulations and the preparation methods of examples 4 to 6, but at the end, a proper amount of starch and dextrin was added to the total weight of each tablet of 600mg, and compressed into tablets.
Example 16:referring to the formulas and the preparation methods of examples 4 to 6, citric acid and kaolin were added after mixing the combined alcohol extracts of corydalis tuber and the like and angelica sinensis, before concentrating the recovered ethanol, the rest of the operations and the material addition amounts were the same, and finally starch and dextrin were added in an appropriate amount to 350mg of total weight of each tablet, and compressed into tablets.
Test example 1: examination of tablet Properties
As described above, in preparing the tablets of each example, round dies of appropriate size are selected for the designed tablet weight, the tablets are pressed with a force of 6.5 to 8kg in a unified manner, the pressed tablets are left at room temperature for 4 to 5 hours, and then subjected to an aluminum plastic blister seal package, which is also a process normally required to be experienced in production. After the tablets were left at room temperature for 4 to 5 hours (4.5 hours), the friability of the tablets obtained herein was measured according to the "0923 tablet friability test" by the fourth edition of the pharmacopoeia 2020, which is a common important parameter for reflecting the tablet forming performance, which is commonly used in the art. The friability test of the present invention is as follows: 6.5g of tablets are taken, powder falling off from the tablets is blown off by a blower, the tablets are precisely weighed, placed in a cylinder and rotated for 10 times. Taking out, removing powder by the same method, precisely weighing, and calculating the weight loss, wherein the weight loss is expressed as a percentage. The art generally prescribes that the tablet friability is not reduced by more than 1% by weight and that broken, cracked and crushed tablets are not detected. The weight loss was averaged 5 times per batch of tablets, and the percentage of tablets tested was calculated for the case of broken, cracked and crushed tablets.
The weight loss of each batch of tablets of examples 1 to 3 was measured to be 0.66%, 0.48% and 0.57%, respectively, and no broken, cracked and crushed tablets were detected;
the weight loss of each batch of tablets of examples 4-8 was 0.41%, 0.39%, 0.32%, 0.62%, 0.44%, and no broken, cracked and crushed tablets were detected, the slightly higher weight loss of the tablets of example 7 may be related to slightly less starch/dextrin addition as an adjunct but the tablets still meet the general requirements;
the weight loss of the tablets of example 11 was 2.37% and the breaking (4.3%, 4/93) and cracking (7.5%, 7/93) chips were detected;
the weight loss of the tablets of example 12 was 3.43% and the breaking (6.6%, 6/91) and cracking (9.9%, 9/91) chips were detected;
the weight loss of the tablets of example 13 was 3.63% and the breaking (5.4%, 5/92) and cracking (10.9%, 10/92) chips were detected;
the weight loss of the tablets of example 14 was 2.74% and the breaking (5.4%, 5/93) and cracking (6.5%, 6/93) chips were detected;
the weight loss of the three batches of tablets of example 15 was 0.47%, 0.36%, 0.52%, respectively, and no broken, cracked, and crushed tablets were detected;
the weight loss of the three batches of tablets of example 16 was 3.26%, 3.52% and 3.13%, respectively, and an unequal number of broken pieces (breaking rates of 5.1%, 3.9% and 4.6%) and cracked pieces (cracking rates of 8.3%, 11.3% and 9.2%) were detected.
From the above results, it can be seen that the 600mg tablets of examples 1 to 3 prepared with reference to the original standard are excellent in moldability and have excellent friability;
when the auxiliary material (starch/dextrin) was reduced to a tablet weight of about 350mg, as described in example 13, the tablet formability was unacceptable and the friability was unacceptable;
when a proper amount of citric acid and kaolin were added to the combined aqueous extract and warm extract and the weight of the tablet was reduced to about 350mg of the auxiliary material (starch/dextrin), as shown in examples 4 to 8, the tablet was excellent in moldability and had excellent friability; in the case of adding a proper amount of citric acid and kaolin to the aqueous extract and the warming extract, a small amount of auxiliary material (starch/dextrin) was still added in sufficient amount to a tablet weight of about 600mg, as described in example 15, at which time the obtained tablet was still excellent in moldability and had excellent friability;
however, when the timing of adding only either or both of citric acid and kaolin was changed, as shown in examples 11, 12, 14, 16, in the case of reducing the auxiliary material (starch/dextrin) to about 350mg of tablet weight, the tablet moldability was unacceptable and the friability was unacceptable.
Based on the above results, the inventors have unexpectedly found that the addition of only small amounts of both citric acid and kaolin at specific process stages, while greatly reducing the filling adjuvant, produces tablets of approximately half the weight of the prior art, such tablets exhibiting excellent formability, which was not anticipated at all by the prior art.
Those skilled in the art will appreciate that the examples 11-14 and example 16 may exhibit problems such as cracking during subsequent packaging, transportation, storage and use of the tablets, which is not acceptable at all, due to the significantly poor friability results. Whereas the small weight tablets of examples 4-8 are significantly better than the tablets of examples 1-3 and example 15 in terms of patient compliance; of course, although the tablets of examples 4 to 8 were significantly reduced in weight, their active drug preparation process, i.e., the operation of the extraction stage of the Chinese medicinal materials, was not changed, so that it was expected that the biological activity of these small-weight tablets was not different from that of the large-weight tablets.
Test example 2: tablet quality detection
Quality inspection of some of the Uygur tablets prepared herein with reference to current quality standards
1. Traits: generally, the aconite root tablet should be a tan tablet, fragrant and bitter. Through observation, all the prepared aconite gold slices in examples 1-16 are tan slices, fragrant and bitter in taste, and all meet the requirements.
2. And (3) identification: taking 20 pieces of a batch of aconite sheets, grinding, adding 50ml of water, heating in water bath, centrifuging, filtering, extracting the filtrate with ethyl acetate three times, 30ml each time, mixing the extracting solutions, recovering ethyl acetate, and concentrating to 2ml to obtain a sample solution; and adding ethanol into paeoniflorin reference substance to obtain a solution containing 1mg per 1ml of paeoniflorin reference substance solution. According to a thin layer chromatography (rule 0502 of four Chinese pharmacopoeia 2020 edition), sucking 10 μl of each of the above two solutions, respectively spotting on the same silica gel G thin layer plate, spreading with chloroform-methanol-water (7:3:1) lower layer solution as developing agent, taking out, air drying, spraying sulfuric acid ethanol solution (1:1) (V/V), and baking at 105deg.C until the spot color is clear; in general, the sample chromatogram will show spots of the same color at positions corresponding to the control chromatogram. All of the U-gold tablets prepared in examples 1 to 16 showed spots of the same color at the positions corresponding to the control chromatogram in the sample chromatograms.
3. And (3) identification: taking 10 pieces of a batch, grinding, adding 50ml of ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, concentrating the filtrate to 10ml on a water bath, adding the filtrate on an activated carbon-alumina column (0.5 g of activated carbon, 100-200 meshes of neutral alumina, 5g and 10mm in inner diameter), eluting with 50ml of ethanol, collecting eluent, evaporating to dryness, and adding 1ml of ethanol into residues to dissolve the residues to obtain a sample solution. And adding ethanol into the stachydrine hydrochloride reference substance to prepare a solution containing 5mg per 1ml as a reference substance solution. According to thin layer chromatography (rule 0502 of four Chinese pharmacopoeia 2020 edition), 10 μl of each of the above two solutions is absorbed, respectively spotted on the same silica gel G thin layer plate, and developed with n-butanol-hydrochloric acid-water (4:1:0.5) as developing agent, taken out, air dried, and sprayed with dilute bismuth potassium iodide test solution. Generally, spots of the same color appear on the sample chromatogram at positions corresponding to those on the control chromatogram. All of the U-gold tablets prepared in examples 1 to 16 showed spots of the same color at the positions corresponding to the chromatogram of the control sample in the chromatogram of the test sample.
4. And (3) identification: taking 10 pieces of a batch, grinding, wetting with ammonia water, standing for 1 hour, adding 50ml of chloroform, performing ultrasonic treatment for 30 minutes, separating chloroform layer, filtering, evaporating filtrate to dryness, and adding 2ml of ethanol into residue to dissolve, thereby obtaining a sample solution. And adding ethanol into tetrahydropalmatine reference substance to obtain a solution containing 1mg per 1m as reference substance solution. According to thin layer chromatography (rule 0502 of four edition of Chinese pharmacopoeia 2020), sucking 5 μl of each of the above two solutions, respectively spotting on the same silica gel G thin layer plate, spreading with cyclohexane-acetone (7:3) as developing agent, taking out, air drying, developing with iodine vapor until the spot color is clear, taking out, standing, and inspecting under ultraviolet lamp (365 nm) after the spot is faded. In general, the sample chromatogram will show fluorescent spots of the same color at positions corresponding to those of the control chromatogram. All of the U-gold tablets prepared in examples 1 to 16 showed fluorescent spots of the same color at the positions corresponding to the chromatogram of the control sample in the chromatogram of the test sample.
5. And (3) identification: taking 5 pieces of a batch, grinding, adding 30ml of diethyl ether, carrying out ultrasonic treatment for 5 minutes, filtering, evaporating the filtrate to dryness, and adding 2ml of ethyl acetate into the residue to dissolve the residue to obtain a test solution. Otherwise, 1g of rhizoma ligustici wallichii and angelica are respectively taken as reference medicinal materials, and the reference medicinal materials are respectively prepared into reference medicinal material solutions by the same method. According to thin layer chromatography (rule 0502 of four edition of Chinese pharmacopoeia 2020), sucking 5 μl of each of the above three solutions, respectively spotting on the same silica gel G thin layer plate, spreading with n-hexane-ethyl acetate (9:1) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp (365 nm). In general, the sample chromatogram will show fluorescent spots of the same color at positions corresponding to those of the control chromatogram. All of the U-gold tablets prepared in examples 1 to 16 showed fluorescent spots of the same color at the positions corresponding to the chromatogram of the control sample in the chromatogram of the test sample.
6. Weight difference checking: taking 20 pieces of the sample, precisely weighing the total weight, respectively precisely weighing each piece after the average piece weight is obtained, and comparing each piece of weight with the weight of the marking piece, wherein the weight difference limit is generally regulated to be +/-5 percent in the field. All of the tablets prepared in examples 1 to 16 were tested to have a weight difference limit in the range of.+ -. 1.9% to.+ -. 3.3%, for example, the tablet in example 4 had a weight difference limit of.+ -. 2.36%.
7. Checking disintegration time limit: the disintegration time test (the disintegration time test of tablets according to the rule 0921 of the fourth edition of the pharmacopoeia of China, 2020) generally specifies that when all of the tablets in each batch should disintegrate within 1 hour, the tablets are considered to be compliant with the specification. The disintegration time of all the tablets prepared in examples 1 to 16 was examined to be in the range of 26 to 42min, for example, 31min.
8. And (3) content measurement: measuring by high performance liquid chromatography (China pharmacopoeia 2020 edition four general rules 0512); chromatographic conditions and system suitability test: octadecylsilane chemically bonded silica is used as a filler (Thermo ScientificTMHypersilTMODS C HPLC chromatographic column, 4.6mm multiplied by 250mm and 5 μm in this example), acetonitrile-0.1% phosphoric acid solution (17:83) is used as a mobile phase, the detection wavelength is 230nm, and the theoretical plate number is not lower than 2000 calculated according to paeoniflorin peaks; preparation of a control solution: precisely weighing paeoniflorin reference substance, and adding methanol to obtain solution containing 0.02mg per 1 ml; preparation of test solution: mixing the above materials under different weight, grinding, precisely weighing about 2 pieces of Uygur autonomous region, placing into a conical flask with plug, precisely adding 50ml of 50% ethanol, weighing, ultrasonic treating (power 250W, frequency 45 KHz) for 40 min, cooling to room temperature, weighing again, supplementing the reduced weight with 50% ethanol, shaking, filtering, discarding the primary filtrate, precisely measuring 25ml of the secondary filtrate, evaporating to dryness on water bath, adding 20ml of water to dissolve the residue, transferring to a separating funnel, shaking and extracting four times (30 ml, 20 ml) with water saturated n-butanol solution, mixing n-butanol extractive solutions, washing twice with ammonia test solution, 20ml each time, discarding Washing ammonia-removed test solution with water saturated with n-butanol twice, each time 20ml, separating n-butanol extract, evaporating in water bath, dissolving residue with methanol, transferring to 50ml measuring flask, adding methanol to scale, shaking, filtering before sampling, and collecting filtrate; assay: respectively precisely sucking 10 μl of the reference solution and the sample solution, and injecting into a liquid chromatograph for measurement. The art generally prescribes that each 1 tablet of Wujin tablet contains white peony root and paeoniflorin (C 23 H 28 O 11 ) And not less than 0.30mg. In order to make the results consistent, the content measurement work referred to herein was performed by the same analyst, and all of the aconite sheets prepared in examples 1 to 16 were measured to contain paeoniflorin (C 23 H 28 O 11 ) The total content is in the range of 0.94-1.17 mg/tablet, for example, the white peony root of the tablets of example 1 and example 4 is compounded with paeoniflorin (C 23 H 28 O 11 ) The total of the total is 1.073 mg/tablet and 1.026 mg/tablet.
Test example 3: examination of tablet stability
The tablets of examples 4 to 8 were placed in a light-shielding manner at 40℃for 6 months (a condition simulating a long-term standing at room temperature for 2 years or more) in an aluminum-plastic composite blister pack simulating a commercially available pack, and samples were taken at 0 month and 6 months, respectively, and the respective properties of the tablets were measured as in test example 1 and test example 2 herein. The 0 month results are as described above, and the 6 month results are as follows: examples 4 to 8 each had a weight loss of 0.45%, 0.37%, 0.36%, 0.59%, and 0.42% by weight loss in the 6-month friability test, and no broken, cracked, and crushed tablets were detected; examples 4 to 8 each batch of tablets showed a 6 month character of tan tablets, a smell of gas, and a bitter taste; examples 4-8 each batch of tablets was identified for 6 months using paeoniflorin as a control, and spots of the same color were displayed at the positions corresponding to the control chromatogram; examples 4-8 each batch of tablets was identified for 6 months using stachydrine hydrochloride as a control, and spots of the same color were displayed at the positions corresponding to the chromatogram of the control; examples 4-8 each batch of tablets was identified for 6 months using tetrahydropalmatine as a control, and all showed fluorescent spots of the same color at the positions corresponding to the chromatogram of the control; examples 4-8 tablets of each batch for 6 months were prepared from Ligusticum wallichii and swertia Japonica Makino Identifying the reference medicinal materials, and displaying fluorescent spots with the same color at the positions corresponding to the chromatogram of the reference medicinal materials; examples 4 to 8 each batch of tablets were examined for 6 months of disintegration time, the disintegration time was in the range of 23 to 44 minutes, for example, the disintegration time of the tablets of example 4 was 29 minutes; examples 4 to 8 each batch of tablets was measured for 6 months content, and white peony root was contained in paeoniflorin (C 23 H 28 O 11 ) The content of paeoniflorin (C) is 0.98-1.09 mg/tablet, such as radix Paeoniae alba of example 4 tablet 23 H 28 O 11 ) Each 1.023 mg/tablet.
The stability results show that some of the aconite tablets prepared by the invention have excellent stability.
The prepared aconite tablet has the effects of regulating menstruation and removing blood stasis, and can be clinically used for qi stagnation, thoracorib stinging, postpartum blood stasis, lower abdomen pain, dysphoria with feverish sensation in the chest and abdomen and emaciation with yellowish complexion; generally, the aconite tablet of the present invention can be orally administered, and generally, the dosage of 4 tablets per time and 2 times per day can be adopted. The 300-400 mg/tablet prepared according to certain embodiments of the present invention provides significantly better patient compliance when taken than the 600 mg/tablet product commercially available.
While the invention has been described in detail in the general context and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.

Claims (10)

1. The 1000 tablets of the traditional Chinese medicine composition in the form of tablets are prepared from the following traditional Chinese medicine materials in parts by weight and a proper amount of auxiliary materials: 24-30 g of pollen typhae, 17-21 g of grass cream, 0.1-0.5 ml of fennel oil, 390-470 g of motherwort, 24-30 g of prepared rehmannia root, 24-30 g of rhizoma sparganii, 24-30 g of carbonized mugwort leaf, 73-89 g of rhizoma corydalis, 146-178 g of nutgrass galingale rhizome, 73-89 g of white paeony root, 24-30 g of costustoot, 24-30 g of fructus psoraleae, 24-30 g of fructus evodiae, 73-89 g of rhizoma ligustici wallichii, 24-30 g of rhizoma curcumae and 24-30 g of Chinese angelica; the traditional Chinese medicine composition in the form of a tablet is prepared according to the following steps:
(1) Pulverizing pollen Typhae and pulvis Fumi Carbonisatus respectively into fine powder, sieving, and mixing to obtain medicinal powder;
(2) Dissolving oleum Foeniculi in ethanol;
(3) Decocting herba Leonuri, radix rehmanniae Preparata, and rhizoma Sparganii with water twice, and filtering to obtain water extractive solution; soaking folium Artemisiae Argyi in water at 80deg.C, and filtering to obtain a warm soaking solution; mixing the above water extractive solutions and the warm extract, filtering, adding citric acid and Kaolinitum into the filtrate, mixing, and concentrating to obtain paste; wherein each 432.43g of motherwort is added with 2-2.5 g of citric acid and 8-9 g of kaolin;
(4) Reflux-extracting rhizoma corydalis, rhizoma Cyperi, radix Paeoniae alba, radix aucklandiae, fructus Psoraleae, fructus evodiae, rhizoma Ligustici Chuanxiong and Curcumae rhizoma with 60% ethanol for three times, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution; reflux-extracting radix Angelicae sinensis with ethanol for three times, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution; mixing the above ethanol extractive solutions, filtering, recovering ethanol, and concentrating into paste;
(5) Mixing the water and alcohol concentrated paste, adding fine powder of pollen typhae and pulvis Fumi Carbonisatus, starch, dextrin and magnesium stearate, mixing, granulating, drying, cooling, adding the common fennel oil alcohol solution, mixing, and pressing into tablets, wherein the tablet weight of each tablet is 300-400 mg; wherein the content of magnesium stearate in the tablet is 0.5% -1.5%, and the weight ratio of starch to dextrin is 1:2 and the amount of the two is such that the weight of each tablet reaches the prescribed tablet weight.
2. The traditional Chinese medicine composition according to claim 1, which is prepared from 1000 Chinese medicinal materials in the following weight proportion: pollen typhae 27.03g, pulvis Fumi Carbonisatus 18.92g, fennel oil 0.135ml, motherwort 432.43g, prepared rehmannia root 27.03g, rhizoma sparganii 27.03g, carbonized mugwort leaf 27.03g, rhizoma corydalis 81.08g, nutgrass galingale rhizome 162.16g, white paeony root 81.08g, costustoot 27.03g, malaytea scurfpea fruit 27.03g, evodia rutaecarpa 27.03g, szechuan lovage rhizome 81.08g, zedoary 27.03g and Chinese angelica 27.03g.
3. The Chinese medicinal composition according to claim 1, wherein each tablet has a tablet weight of 350mg.
4. The traditional Chinese medicine composition according to claim 1, wherein the content of magnesium stearate in the tablet is 1%.
5. The Chinese medicinal composition according to claim 1, wherein in the step (2), the fennel oil is dissolved with 10 to 20 times of ethanol by volume.
6. The Chinese medicinal composition according to claim 1, wherein in the step (3), the motherwort, the prepared rehmannia root and the common burreed rhizome are decocted with water twice, the water added for 12 times is soaked for 0.5 hour, the decoction is carried out for 3 hours, the water added for 8 times is decocted for 2 hours, and the water extract is obtained by filtering; soaking folium Artemisiae Argyi in 12 times of water for 0.5 hr, boiling, soaking at 80deg.C for 2 hr, and filtering to obtain a warm soaking solution; mixing the above water extractive solutions and the warm extract, filtering, adding citric acid and Kaolinitum into the filtrate, mixing, and concentrating to obtain paste; wherein, each 432.43g of motherwort herb is added with 2-2.5 g of citric acid and 8-9 g of kaolin.
7. The Chinese medicinal composition according to claim 1, wherein in the step (4), the rhizoma corydalis, the rhizoma cyperi, the white paeony root, the costustoot, the fructus psoraleae, the fructus evodiae, the ligusticum wallichii and the rhizoma curcumae are extracted by reflux with 60% ethanol for three times, the first time is 6 hours, the second time is 4 hours, the third time is 2 hours, the alcohol addition amounts are 8 times, 6 times and 6 times respectively, and the three extracts are combined and filtered to obtain an alcohol extract; reflux-extracting radix Angelicae sinensis with ethanol for three times, reflux-extracting with 8 times of ethanol for 8 hr, reflux-extracting with 60% ethanol for two times, reflux-extracting for 4 hr, reflux-extracting with 6 times and 6 times of ethanol for 2 hr, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution; mixing the above ethanol extractive solutions, filtering, recovering ethanol, and concentrating into paste.
8. The method for preparing the traditional Chinese medicine composition according to any one of claims 1-7, comprising the following steps:
(1) Pulverizing pollen Typhae and pulvis Fumi Carbonisatus respectively into fine powder, sieving, and mixing to obtain medicinal powder;
(2) Dissolving the fennel oil with 10-20 times of ethanol for standby;
(3) Decocting herba Leonuri, radix rehmanniae Preparata, and rhizoma Sparganii with water twice, adding 12 times of water for soaking for 0.5 hr, decocting for 3 hr, adding 8 times of water for 2 hr, and filtering to obtain water extractive solution; soaking folium Artemisiae Argyi in 12 times of water for 0.5 hr, boiling, soaking at 80deg.C for 2 hr, and filtering to obtain a warm soaking solution; mixing the above water extractive solutions and the warm extract, filtering, adding citric acid and Kaolinitum into the filtrate, mixing, and concentrating to obtain paste; wherein each 432.43g of motherwort is added with 2-2.5 g of citric acid and 8-9 g of kaolin;
(4) Reflux-extracting rhizoma corydalis, rhizoma Cyperi, radix Paeoniae alba, radix aucklandiae, fructus Psoraleae, fructus evodiae, rhizoma Ligustici Chuanxiong and Curcumae rhizoma with 60% ethanol for three times, the first time for 6 hr, the second time for 4 hr, and the third time for 2 hr, with ethanol addition amounts of 8 times, 6 times and 6 times respectively, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution; reflux-extracting radix Angelicae sinensis with ethanol for three times, reflux-extracting with 8 times of ethanol for 8 hr, reflux-extracting with 60% ethanol for two times, reflux-extracting for 4 hr, reflux-extracting with 6 times and 6 times of ethanol for 2 hr, mixing the three extractive solutions, and filtering to obtain ethanol extractive solution; mixing the above ethanol extractive solutions, filtering, recovering ethanol, and concentrating into paste;
(5) Mixing the water and alcohol concentrated paste, adding fine powder of pollen typhae and pulvis Fumi Carbonisatus, starch, dextrin and magnesium stearate, granulating, drying, cooling, adding the common fennel oil alcohol solution, mixing, and tabletting, wherein the tablet weight of each tablet is 300-400 mg.
9. The use of the traditional Chinese medicine composition according to any one of claims 1-7 in preparing a medicament for regulating menstruation and removing blood stasis.
10. The use of the traditional Chinese medicine composition according to any one of claims 1-7 in preparing medicines for treating qi stagnation, chest and hypochondrium stabbing pain, postpartum blood stasis, lower abdomen pain, dysphoria with smothery sensation in the chest and chest, and emaciation with yellowish complexion.
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Citations (2)

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Publication number Priority date Publication date Assignee Title
CN101278917A (en) * 2008-02-28 2008-10-08 王世锋 Method for preparing povidone iodine vaginal tablet
CN102824614A (en) * 2012-09-20 2012-12-19 南京正亮医药科技有限公司 Application of Wujin tablets for preparing medicines for suppressing PC-3 cell proliferation

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101278917A (en) * 2008-02-28 2008-10-08 王世锋 Method for preparing povidone iodine vaginal tablet
CN102824614A (en) * 2012-09-20 2012-12-19 南京正亮医药科技有限公司 Application of Wujin tablets for preparing medicines for suppressing PC-3 cell proliferation

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