CN105079362A - Huoxiang Zhengqi tablet - Google Patents
Huoxiang Zhengqi tablet Download PDFInfo
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Abstract
The invention relates to a Huoxiang Zhengqi tablet. A preparation method of the medicine disclosed by the invention comprises the following steps: (1) extracting active ingredients of pericarpium arecae, pinellia ternate, radix angelicae and dried orange peel by virtue of a continuous concentration change ethanol extraction method; (2) extracting volatile oil of rhizoma atractylodes and mangnolia officinalis by virtue of a microwave-assisted extraction method; (3) processing poria cocos and mixing a dry extract; and (4) preparing a tablet. By virtue of the preparation method disclosed by the invention, the Huoxiang Zhengqi tablet is rapid to take effect, good in cure effect and low in side effect.
Description
Technical field:
The present invention relates to a kind of HUOXIANG ZHENGQI PIAN, concrete, the present invention relates to a kind of preparation method of HUOXIANG ZHENGQI PIAN.
Technical background:
HUOXIANG ZHENGQI ZHIJI class medicine has removing dampness of inducing sweat, effect of regulating the flow of Qi and the middle Jiao.For summer-heat damp cold, headache heavy sensation of the body is uncomfortable in chest, or fever with aversion to cold, and abdominal distention, vomiting is had loose bowels.In general, mainly be applicable to following several situation: the influenza of common cold of gastrointestinal type, viral influenza and some types, diarrhoea, acute or chronic gastritis, functional gastropathy, catch cold summer the gastrointestinal upset caused, or because of the diarrhoea caused by eating and drinking without temperance, acute or chronic gastritis, functional gastropathy etc.
In prior art, existing HUOXIANG ZHENGQI ZHIJI class drug main will comprise HUOXIANGZHENGQI KOUFUYE, ageratum drop pill, HUOXIANG ZHENGQI WAN, ageratum microemulsion, or the dosage form such as HUOXIANG ZHENGQI WAN.
Chinese patent 20111032193.5 describes a kind of preparation method of HUOXIANGZHENGQI KOUFUYE, it overcomes the deficiencies in the prior art, Cortex Magnoliae Officinalis adds ethanol, reflux, extract, after adjust pH, and after the distillation of Rhizoma Atractylodis, Pericarpium Citri Reticulatae, the Radix Angelicae Dahuricae, medicinal residues secondary back extracts, thus makes product have stronger analgesia, antiinflammatory and antibacterial action.
HUOXIANGZHENGQI KOUFUYE prepared in Chinese patent 2011102448338.5; a kind of method utilizing membrane filter pressing circulation extraction and isolation integrated technique to prepare HUOXIANGZHENGQI KOUFUYE is provided; not only can simplification of flowsheet; significantly shorten the production cycle; energy efficient; be beneficial to environmental conservation and waste residue utilization, and greatly can improve the response rate of effective ingredient.
In addition, Chinese patent 03145667.7 gives a kind of preparation method of ageratum drop pill, is characterized in first, can cover the penetrating odor of Herba Pogostemonis preparation, is easy to be accepted by patient; Secondly, drop pill production process is few, and the cycle is short, and automaticity is high, and production efficiency is high, and advantage of lower cost is easy to industrialization; 3rd, drop pill working condition is easy to control, and pill weight variation is little, and content is comparatively accurate, and quality is guaranteed; 4th, drop pill is convenient to transport, storage, is the form of Chinese drug of country's recommendation at present.Owing to not conforming to ethanol in final products, not only reduce cost economically, and ensureing that " HUOXIANG ZHENGQI SHUI " with States Pharmacopoeia specifications has on the basis of identical function and curative effect, curative effect is in some aspects better than this " HUOXIANG ZHENGQI SHUI ", but reduced side effect aspects such as gastrointestinal stimulations.
For these dosage forms existing in prior art, " Chinese Pharmacopoeia " revises and enlarges prescription and the preparation method that part provides a kind of HUOXIANG ZHENGQI PIAN for 2010.As everyone knows, it is accurate that tablet itself has content, and chemical stability is good, and output is large, mechanization degree high, meanwhile, utilizes HUOXIANG ZHENGQI PIAN prepared by the superiority of tablet, overcome in original dosage form with penetrating odor, the residual of ethanol can be avoided simultaneously, ensure safety.
In " pharmacopeia ", the prescription of HUOXIANG ZHENGQI PIAN is Rhizoma Atractylodis 86g, Pericarpium Citri Reticulatae 86g, Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 86g, Radix Angelicae Dahuricae 130g, Poria 130g, Pericarpium Arecae 130g, Rhizoma Pinelliae 86g, Radix Glycyrrhizae extractum 11g, patchouli oil 0.9ml, Folium perillae acutae oil 0.4ml; Preparation method is: above ten tastes, and Radix Angelicae Dahuricae 81g is ground into fine powder, for subsequent use; Pericarpium Citri Reticulatae extracts after volatile oil mixes with patchouli oil, Folium perillae acutae oil and dissolves with appropriate amount of ethanol, for subsequent use; Carry the aqueous solution after oil to continue to employ, medicinal residues decoct with water 1 hour, and filter, filtrate is for subsequent use; Pericarpium Arecae, Poria decoct with water secondary, 2 hours first times, second time 1 hour, and filter, merging filtrate, adds the aqueous solution after carrying oil and above-mentioned filtrate, and filter, filtrate is for subsequent use; Rhizoma Pinelliae cold water soak, does not have within 8 hours, change water once, separately adds Rhizoma Zingiberis 7.3g, decoct with water secondary after the brewed heart, and filter, merging filtrate, adds above-mentioned filtrate and Radix Glycyrrhizae extractum, is concentrated into the clear paste that relative density is 1.2-1.3 (55 DEG C); Radix Angelicae Dahuricae 49g, Rhizoma Atractylodis, Cortex Magnoliae Officinalis 60% alcohol reflux three times, 6 hours first times, second time 4 hours, 2 hours third times, merges above-mentioned ethanol extract, and filter, filtrate recycling ethanol, is condensed into cream; Merge water, alcohol condensed cream, add Radix Angelicae Dahuricae fine powder and right amount of auxiliary materials, mixed pelletization is dry, is blended into the alcoholic solution of patchouli oil, Folium perillae acutae oil and Oleum Citri Reticulatae, and mixing is pressed into 1000, or is pressed into 1000 film coatings.
Ageratum opiates commercially available at present, it inevitably remains certain ethanol, and wherein effective ingredient cannot improve further, causes its slow problem that takes effect.
Summary of the invention:
In order to overcome HUOXIANG ZHENGQI PIAN ethanol residual in preparation process, improving wherein effective ingredient simultaneously, increasing drug effect, specially propose the present invention.
One of them object of the present invention is to provide a kind of HUOXIANG ZHENGQI PIAN;
Another object of the present invention is to provide a kind of preparation method of HUOXIANG ZHENGQI PIAN.
In order to realize object of the present invention, technical scheme of the present invention is as follows:
Prescription:
Rhizoma Atractylodis 160g, Pericarpium Citri Reticulatae 160g, Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 160g, Radix Angelicae Dahuricae 240g, Poria 240g, Pericarpium Arecae 240g, Rhizoma Pinelliae 160g, Radix Glycyrrhizae extractum 20g, patchouli oil 1.6ml, Folium perillae acutae oil 0.8ml,
Adjuvant: magnesium stearate 3g, Icing Sugar 1.2g
Its preparation method is:
1) dynamically concentration change alcoholic solution extracts Pericarpium Arecae, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae effective ingredient continuously
The alcoholic solution of 95% is added in Chinese medicament extracting device, mixed after the Pericarpium Arecae of recipe quantity, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae are pulverized 50-150 mesh sieve, from the dog-house of extractor, material is dropped into after infiltration, after feeding intake, heated and stirred is carried out to extractor, and to control final temperature be 65-75 DEG C;
Extractor top connects a water tank, makes it and extractor UNICOM, is provided with valve switch and effusion meter between water tank and extractor, and wherein effusion meter can control water in water tank and flow into the speed of extractor; While extractor is heated, also water in water tank is heated, make Water in Water Tanks temperature consistent with temperature in extractor;
After temperature stabilization in water tank and extractor, open the valve switch of water tank, by controlling the flow velocity of water in water tank, the water in water tank slowly being instilled in extractor, ensureing that in extractor, concentration of alcohol rate of change is that also control temperature is constant in 0.3-0.5%/min continuation stirring.After reaction 1.5-2.5h, when in extractor, concentration of alcohol is about 40-60%, stopped reaction;
Extractor bottoms can folding be provided with filter screen, and after first set reaction terminates, extractor bottoms is opened, and medicinal residues are extracted device bottom screen and intercept, and extracting solution flows down along extractor bottoms and filters after condensation and collect;
Again closed extractor bottoms, the ethanol that concentration is 40-60% is added in medicinal residues after first set reaction terminates, and slowly add water according to the step of the first reaction, ensure that in extractor, concentration of alcohol rate of change is 0.2-1.3%/min, in reaction 0.5-1.5h to extractor, concentration of alcohol becomes 5-15%, the filtrate of collecting with first time after collecting filtrate cold filtration merges, and collects filtering residue; Collected filtrate is condensed into thick paste;
2) Rhizoma Atractylodis, Cortex Magnoliae Officinalis volatile oil constituents extraction
The Rhizoma Atractylodis magnolia obovata of recipe quantity, crosses 50-200 mesh sieve after pulverizing, carries out microwave extracting, wherein microwave extracting power is 300-450w, solid-liquid ratio 1:30-1:45, Extraction solvent is the alcoholic solution of 60-85%, extracts 10-25min, after repeating extraction 3 times, filter, merging filtrate, by filtrate reduced in volume, obtain Mixed chaotic sequences, and collect filtering residue;
3) process of preparing Chinese medicine of Poria and the mixing of thick paste
After simply being washed by the Poria raw material of recipe quantity, be cut into the lamellar of thickness equalization, and the thick paste of positive and negative uniform application step (1) gained repeatedly in Indian buead tablet, steaming and decocting 15-45min in steamer, controls steamer temperature and is no more than 70 DEG C;
After first time steaming and decocting terminates, again smear remaining thick paste, carry out steaming and decocting; So steaming and decocting is infiltrated in Indian buead tablet completely to thick paste for 3 times repeatedly, is dried by Poria and wears into fine powder, for subsequent use;
4) preparation of tablet
By the Radix Glycyrrhizae extractum mix homogeneously of the dried cream powder in step (3) and recipe quantity, add the sucrose of recipe quantity and appropriate water, mix soft material granulation processed, dry after crossing 14 mesh sieves;
After the Folium perillae acutae oil of the Mixed chaotic sequences of step (2) and recipe quantity, patchouli oil being mixed homogeneously, add granule dry after sieving, and add magnesium stearate mixing, be pressed into 500, every more than sheet 0.5g.
Preferably, the preparation method of described HUOXIANG ZHENGQI PIAN is:
1) dynamically concentration ethanol extracts Pericarpium Arecae, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae effective ingredient continuously
The alcoholic solution of 95% is added in Chinese medicament extracting device, mixed after the Pericarpium Arecae of recipe quantity, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae are pulverized 100 mesh sieves, from the dog-house of extractor, dropped into material after infiltration, after feeding intake, heated and stirred is carried out to extractor, and to control final temperature be 68 DEG C;
Extractor top connects a water tank, makes it and extractor UNICOM, is provided with valve switch and effusion meter between water tank and extractor, and wherein effusion meter can control water in water tank and flow into the speed of extractor.While extractor is heated, also water in water tank is heated, make Water in Water Tanks temperature consistent with temperature in extractor;
After temperature stabilization in water tank and extractor, opening the valve switch of water tank, by controlling the flow velocity of water in water tank, the water in water tank slowly being instilled in extractor, ensure that in extractor, concentration of alcohol rate of change is 0.42%/min, continuing to stir also, control temperature is constant.After reaction 2h, when concentration of alcohol in extractor is 50%, stopped reaction;
Extractor bottoms can folding be provided with filter screen, and after first set reaction terminates, extractor bottoms is opened, and medicinal residues are extracted device bottom screen and intercept, and extracting solution flows down along extractor bottoms and filters after condensation and collect;
Again closed extractor bottoms, the ethanol that concentration is 50% is added in medicinal residues after first set reaction terminates, and slowly add water according to the step of the first reaction, concentration of alcohol rate of change in extractor is kept to be 0.68%/min, in reaction 1h to extractor, concentration of alcohol becomes 10%, the filtrate of collecting with first time after collecting filtrate cold filtration merges, and collects filtering residue; Collected filtrate is condensed into thick paste;
2) Rhizoma Atractylodis, Cortex Magnoliae Officinalis volatile oil constituents extraction
The Rhizoma Atractylodis magnolia obovata of recipe quantity, crosses 150 mesh sieves after pulverizing, carries out microwave extracting, wherein microwave extracting power is 400w, solid-liquid ratio 1:40, Extraction solvent is the alcoholic solution of 80%, extracts 15min, after repeating extraction 3 times, filter, merging filtrate, by filtrate reduced in volume, obtain Mixed chaotic sequences, and collect filtering residue;
3) process of preparing Chinese medicine of Poria and the mixing of thick paste
After simply being washed by the Poria raw material of recipe quantity, be cut into the lamellar of thickness equalization, and the thick paste of positive and negative uniform application step (1) gained repeatedly in Indian buead tablet, steaming and decocting 30min in steamer, controls steamer temperature and is no more than 70 DEG C;
After first time steaming and decocting terminates, again smear remaining thick paste, carry out steaming and decocting; Steaming and decocting is coated with most to thick paste and infiltrates in Indian buead tablet completely for 3 times so repeatedly, is dried by Poria and wears into fine powder, for subsequent use;
4) preparation of tablet
By the Radix Glycyrrhizae extractum mix homogeneously of the dried cream powder in step (3) and recipe quantity, add the sucrose of recipe quantity and appropriate water, mix soft material granulation processed, dry after crossing 14 mesh sieves;
After the Folium perillae acutae oil of the Mixed chaotic sequences of step (2) and recipe quantity, patchouli oil being mixed homogeneously, add granule dry after sieving, and add magnesium stearate mixing, be pressed into 500, every sheet 0.62g.
Preferred, in the present invention, adjuvant available starches slurry, also can add microcrystalline Cellulose.
The invention has the beneficial effects as follows:
1. in the extraction to Pericarpium Arecae, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae effective ingredient, adopt the ethanol extraction apparatus and method of " continuous concentration change ", ensure that in medical material, extracts active ingredients is complete, improves the extraction ratio of effective ingredient, ensure that the final drug effect of product; Save extraction time and resource simultaneously, achieve energy-efficient object.
2., in the extraction to Rhizoma Atractylodis magnolia obovata volatile oil, adopting microwave to help lifting manipulation to extract Mixed chaotic sequences, by changing extraction conditions, improve the yield of volatile oil.
3. in the preparation process of Tablets, starch is replaced with starch slurry as binding agent, use microcrystalline Cellulose as diluent and disintegrating agent, improve stability and the disintegration of tablet.
4. by studying process for preparing medicine of the present invention, carrying out zoopery to medicine of the present invention, can draw, gained HUOXIANG ZHENGQI PIAN medicine of the present invention, has instant effect, good drug efficacy, the effects such as side effect is low.
5. although it is simple replacement to existing extracting method that some steps in preparation method of the present invention seem, or limit is changed to experiment condition, or the improvement utilizing known principle of the prior art to carry out production equipment, but Chinese medicine is because the factor such as the complexity of its composition and uncertainty, its whole preparation method should be regarded as an overall technical scheme, consider its technological means, technical purpose and technique effect, its one step contrary can not solve technical problem of the present invention, also its technique effect cannot be expected, thus should by not separated for its single preparation process.Therefore, consider the general idea of preparation method of the present invention, can determine that the bioavailability existed in the prior art that the present invention solves is low, the problems such as efficient energy-saving, and reach corresponding technique effect, there is substantial feature and significant progress.
Detailed description of the invention
Embodiment 1
Prescription:
Rhizoma Atractylodis 160g, Pericarpium Citri Reticulatae 160g, Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 160g, Radix Angelicae Dahuricae 240g, Poria 240g, Pericarpium Arecae 240g, Rhizoma Pinelliae 160g, Radix Glycyrrhizae extractum 20g, patchouli oil 1.6ml, Folium perillae acutae oil 0.8ml,
Adjuvant: magnesium stearate 3g, Icing Sugar 1.2g
Preparation method:
(1) dynamically concentration ethanol extracts Pericarpium Arecae, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae effective ingredient continuously
The alcoholic solution of 95% is added in Chinese medicament extracting device, mixed after the Pericarpium Arecae of recipe quantity, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae are pulverized 100 mesh sieves, from the dog-house of extractor, dropped into material after infiltration, after feeding intake, heated and stirred is carried out to extractor, and to control final temperature be 68 DEG C.
Extractor top connects a water tank, makes it and extractor UNICOM, is provided with valve switch and effusion meter between water tank and extractor, and wherein effusion meter can control water in water tank and flow into the speed of extractor.While extractor is heated, also water in water tank is heated, make Water in Water Tanks temperature consistent with temperature in extractor.
After temperature stabilization in water tank and extractor, opening the valve switch of water tank, by controlling the flow velocity of water in water tank, the water in water tank slowly being instilled in extractor, ensure that in extractor, concentration of alcohol rate of change is 0.42%/min, continuing to stir also, control temperature is constant.After reaction 2h, when concentration of alcohol in extractor is 50%, stopped reaction.
Extractor bottoms can folding be provided with filter screen, and after first set reaction terminates, extractor bottoms is opened, and medicinal residues are extracted device bottom screen and intercept, and extracting solution flows down along extractor bottoms and filters after condensation and collect.
Again closed extractor bottoms, the ethanol that concentration is 50% is added in medicinal residues after first set reaction terminates, and slowly add water according to the step of the first reaction, concentration of alcohol rate of change in extractor is kept to be 0.68%/min, in reaction 1h to extractor, concentration of alcohol becomes 10%, the filtrate of collecting with first time after collecting filtrate cold filtration merges, and collects filtering residue.
Collected filtrate is condensed into thick paste.
(2) Rhizoma Atractylodis, Cortex Magnoliae Officinalis volatile oil constituents extraction
The Rhizoma Atractylodis magnolia obovata of recipe quantity, crosses 150 mesh sieves after pulverizing, carries out microwave extracting, wherein microwave extracting power is 400w, solid-liquid ratio 1:40, Extraction solvent is the alcoholic solution of 80%, extracts 15min, after repeating extraction 3 times, filter, merging filtrate, by filtrate reduced in volume, obtain Mixed chaotic sequences, and collect filtering residue.
(3) process of preparing Chinese medicine of Poria and the mixing of thick paste
After simply being washed by the Poria raw material of recipe quantity, be cut into the lamellar of thickness equalization, and the thick paste of positive and negative uniform application step (1) gained repeatedly in Indian buead tablet, steaming and decocting 30min in steamer, controls steamer temperature and is no more than 70 DEG C.
After first time steaming and decocting terminates, again smear remaining thick paste, carry out steaming and decocting; Steaming and decocting is coated with most to thick paste and infiltrates in Indian buead tablet completely for 3 times so repeatedly, is dried by Poria and wears into fine powder, for subsequent use.
(4) preparation of tablet
By the Radix Glycyrrhizae extractum mix homogeneously of the dried cream powder in step (3) and recipe quantity, add the sucrose of recipe quantity and appropriate water, mix soft material granulation processed, dry after crossing 14 mesh sieves.
After the Folium perillae acutae oil of the Mixed chaotic sequences of step (2) and recipe quantity, patchouli oil being mixed homogeneously, add granule dry after sieving, and add magnesium stearate mixing, be pressed into 925, every sheet 0.62g.
Embodiment 2
Prescription:
Rhizoma Atractylodis 160g, Pericarpium Citri Reticulatae 160g, Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 160g, Radix Angelicae Dahuricae 240g, Poria 240g, Pericarpium Arecae 240g, Rhizoma Pinelliae 160g, Radix Glycyrrhizae extractum 20g, patchouli oil 1.6ml, Folium perillae acutae oil 0.8ml,
Adjuvant: magnesium stearate 3g, Icing Sugar 1.2g
(1) concentration continually varying alcoholic solution extracts Pericarpium Arecae, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae effective ingredient
The alcoholic solution of 95% is added in Chinese medicament extracting device, after the Pericarpium Arecae of recipe quantity, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and tangerine peel powder being broken into 50 mesh sieves, mixing was closed, and dropped into material, after feeding intake after infiltration from the dog-house of extractor, heated and stirred is carried out to extractor, and to control final temperature be 65 DEG C.
Extractor top connects a water tank, and water tank and extractor UNICOM, be provided with valve switch and effusion meter between water tank and extractor, and wherein effusion meter can control water in water tank and flow into the speed of extractor.While extractor is heated, also water in water tank is heated, make Water in Water Tanks temperature consistent with temperature in extractor.
After temperature stabilization in water tank and extractor, opening the valve switch of water tank, by controlling the flow velocity of water in water tank, the water in water tank slowly being entered in extractor, ensure that in extractor, concentration of alcohol rate of change is 0.5%/min, continuing to stir also, control temperature is constant.After reaction 1.5h, when concentration of alcohol in extractor is about 40%, stopped reaction.
Extractor bottoms can folding be provided with filter screen, and after first set reaction terminates, extractor bottoms is opened, and medicinal residues are extracted device bottom screen and intercept, extracting solution flow down along extractor bottoms and after condensation collecting by filtration.
Again closed extractor bottoms, the ethanol that concentration is 40% is added in medicinal residues after first set reaction terminates, and slowly add water according to the step of the first reaction, ensure that in extractor, concentration of alcohol rate of change is 1.16%/min, in reaction 0.5h to extractor, concentration of alcohol becomes 5%, the filtrate of collecting with first time after collecting filtrate cold filtration merges, and collects filtering residue.
Collected filtrate is condensed into thick paste.
(2) Rhizoma Atractylodis, Cortex Magnoliae Officinalis volatile oil constituents extraction
The Rhizoma Atractylodis magnolia obovata of recipe quantity, crosses 100 mesh sieves after pulverizing, carries out microwave extracting, wherein microwave extracting power is 300w, solid-liquid ratio 1:30, Extraction solvent is the alcoholic solution of 60%, extracts 25min, after repeating extraction 3 times, filter, merging filtrate, by filtrate reduced in volume, obtain Mixed chaotic sequences, and collect filtering residue.
(3) process of preparing Chinese medicine of Poria
After simply being washed by the Poria raw material of recipe quantity, be cut into the lamellar of thickness equalization, and the thick paste of positive and negative uniform application step (1) gained repeatedly in Indian buead tablet, steaming and decocting 15min in steamer, controls steamer temperature and is no more than 70 DEG C.
After first time steaming and decocting terminates, again smear remaining thick paste, carry out steaming and decocting; Steaming and decocting is coated with most to thick paste and infiltrates in Indian buead tablet completely for 3 times so repeatedly, is dried by Poria and wears into fine powder, for subsequent use.
(4) preparation of tablet
By the Radix Glycyrrhizae extractum mix homogeneously of the dried cream powder in step (3) and recipe quantity, add the sucrose of recipe quantity and appropriate water, mix soft material granulation processed, dry after crossing 14 mesh sieves.
After the Folium perillae acutae oil of the Mixed chaotic sequences of step (2) and recipe quantity, patchouli oil being mixed homogeneously, add granule dry after sieving, and add magnesium stearate mixing, be pressed into 500, every sheet 0.5g.
Embodiment 3
Prescription:
Rhizoma Atractylodis 160g, Pericarpium Citri Reticulatae 160g, Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 160g, Radix Angelicae Dahuricae 240g, Poria 240g, Pericarpium Arecae 240g, Rhizoma Pinelliae 160g, Radix Glycyrrhizae extractum 20g, patchouli oil 1.6ml, Folium perillae acutae oil 0.8ml,
Adjuvant: magnesium stearate 3g, Icing Sugar 1.2g
(1) concentration continually varying alcoholic solution extracts Pericarpium Arecae, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae effective ingredient
The alcoholic solution of 95% is added in Chinese medicament extracting device, mixed after the Pericarpium Arecae of recipe quantity, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae are pulverized 150 mesh sieves, from the dog-house of extractor, dropped into material after infiltration, after feeding intake, heated and stirred is carried out to extractor, and to control final temperature be 70 DEG C.
Extractor top connects a water tank, and water tank and extractor UNICOM, be provided with valve switch and effusion meter between water tank and extractor, and wherein effusion meter can control water in water tank and flow into the speed of extractor.While extractor is heated, also water in water tank is heated, make Water in Water Tanks temperature consistent with temperature in extractor.
After temperature stabilization in water tank and extractor, opening the valve switch of water tank, by controlling the flow velocity of water in water tank, the water in water tank slowly being entered in extractor, ensure that in extractor, concentration of alcohol rate of change is 0.2%/min, continuing to stir also, control temperature is constant.After reaction 2.5h, when concentration of alcohol in extractor is about 60%, stopped reaction.
Extractor bottoms can folding be provided with filter screen, and after first set reaction terminates, extractor bottoms is opened, and medicinal residues are extracted device bottom screen and intercept, extracting solution flow down along extractor bottoms and after condensation collecting by filtration.
Again closed extractor bottoms, the ethanol that concentration is 60% is added in medicinal residues after first set reaction terminates, and slowly add water according to the step of the first reaction, ensure that in extractor, concentration of alcohol rate of change is 0.3%/min, in reaction 1.5h to extractor, concentration of alcohol becomes 15%, the filtrate of collecting with first time after collecting filtrate cold filtration merges, and collects filtering residue.
Collected filtrate is condensed into thick paste.
(2) Rhizoma Atractylodis, Cortex Magnoliae Officinalis volatile oil constituents extraction
The Rhizoma Atractylodis magnolia obovata of recipe quantity, crosses 200 mesh sieves after pulverizing, carries out microwave extracting, wherein microwave extracting power is 450w, solid-liquid ratio 1:45, Extraction solvent is the alcoholic solution of 85%, extracts 10min, after repeating extraction 3 times, filter, merging filtrate, by filtrate reduced in volume, obtain Mixed chaotic sequences, and collect filtering residue.
(3) process of preparing Chinese medicine of Poria
After simply being washed by the Poria raw material of recipe quantity, be cut into the lamellar of thickness equalization, and the thick paste of positive and negative uniform application step (1) gained repeatedly in Indian buead tablet, steaming and decocting 45min in steamer, controls steamer temperature and is no more than 70 DEG C.
After first time steaming and decocting terminates, again smear remaining thick paste, carry out steaming and decocting; Steaming and decocting is coated with most to thick paste and infiltrates in Indian buead tablet completely for 3 times so repeatedly, is dried by Poria and wears into fine powder, for subsequent use.
(4) preparation of tablet
By the Radix Glycyrrhizae extractum mix homogeneously of the dried cream powder in step (3) and recipe quantity, add the sucrose of recipe quantity and appropriate water, mix soft material granulation processed, dry after crossing 14 mesh sieves.
After the Folium perillae acutae oil of the Mixed chaotic sequences of step (2) and recipe quantity, patchouli oil being mixed homogeneously, add granule dry after sieving, and add magnesium stearate mixing, be pressed into 500, every sheet 0.6g.
Embodiment 4
Prescription:
Rhizoma Atractylodis 160g, Pericarpium Citri Reticulatae 160g, Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 160g, Radix Angelicae Dahuricae 240g, Poria 240g, Pericarpium Arecae 240g, Rhizoma Pinelliae 160g, Radix Glycyrrhizae extractum 20g, patchouli oil 1.6ml, Folium perillae acutae oil 0.8ml,
Adjuvant: magnesium stearate 3g, sucrose 1.2g, the starch slurry of 10%
(1) concentration continually varying alcoholic solution extracts Pericarpium Arecae, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae effective ingredient
The alcoholic solution of 95% is added in Chinese medicament extracting device, mixed after the Pericarpium Arecae of recipe quantity, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae are pulverized 90 mesh sieves, from the dog-house of extractor, dropped into material after infiltration, after feeding intake, heated and stirred is carried out to extractor, and to control final temperature be 75 DEG C.
Extractor top connects a water tank, and water tank and extractor UNICOM, be provided with valve switch and effusion meter between water tank and extractor, and wherein effusion meter can control water in water tank and flow into the speed of extractor.While extractor is heated, also water in water tank is heated, make Water in Water Tanks temperature consistent with temperature in extractor.
After temperature stabilization in water tank and extractor, opening the valve switch of water tank, by controlling the flow velocity of water in water tank, the water in water tank slowly being entered in extractor, ensure that in extractor, concentration of alcohol rate of change is 0.46%/min, continuing to stir also, control temperature is constant.After reaction 2h, when concentration of alcohol in extractor is about 55%, stopped reaction.
Extractor bottoms can folding be provided with filter screen, and after first set reaction terminates, extractor bottoms is opened, and medicinal residues are extracted device bottom screen and intercept, extracting solution flow down along extractor bottoms and after condensation collecting by filtration.
Again closed extractor bottoms, the ethanol that concentration is 55% is added in medicinal residues after first set reaction terminates, and slowly add water according to the step of the first reaction, ensure that in extractor, concentration of alcohol rate of change is 0.5%/min, in reaction 1.5h to extractor, concentration of alcohol becomes 10%, the filtrate of collecting with first time after collecting filtrate cold filtration merges, and collects filtering residue.
Collected filtrate is condensed into thick paste.
(2) Rhizoma Atractylodis, Cortex Magnoliae Officinalis volatile oil constituents extraction
The Rhizoma Atractylodis magnolia obovata of recipe quantity, crosses 100 mesh sieves after pulverizing, carries out microwave extracting, wherein microwave extracting power is 450w, solid-liquid ratio 1:38, Extraction solvent is the alcoholic solution of 75%, extracts 10min, after repeating extraction 3 times, filter, merging filtrate, by filtrate reduced in volume, obtain Mixed chaotic sequences, and collect filtering residue.
(3) process of preparing Chinese medicine of Poria
After simply being washed by the Poria raw material of recipe quantity, be cut into the lamellar of thickness equalization, and the thick paste of positive and negative uniform application step (1) gained repeatedly in Indian buead tablet, steaming and decocting 25min in steamer, controls steamer temperature and is no more than 70 DEG C.
After first time steaming and decocting terminates, again smear remaining thick paste, carry out steaming and decocting; Steaming and decocting is coated with most to thick paste and infiltrates in Indian buead tablet completely for 3 times so repeatedly, is dried by Poria and wears into fine powder, for subsequent use.
(4) preparation of tablet
The cane sugar powder of recipe quantity is broken into fine powder.
By the Radix Glycyrrhizae extractum mix homogeneously of the dried cream powder in step (3) and recipe quantity, add Icing Sugar, starch slurry, mix soft material granulation processed, dry after crossing 14 mesh sieves.
After the Folium perillae acutae oil of the Mixed chaotic sequences of step (2) and recipe quantity, patchouli oil being mixed homogeneously, add granule dry after sieving, and add magnesium stearate mixing, be pressed into 500, every sheet 0.55g.
Embodiment 5
Prescription:
Rhizoma Atractylodis 160g, Pericarpium Citri Reticulatae 160g, Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 160g, Radix Angelicae Dahuricae 240g, Poria 240g, Pericarpium Arecae 240g, Rhizoma Pinelliae 160g, Radix Glycyrrhizae extractum 20g, patchouli oil 1.6ml, Folium perillae acutae oil 0.8ml,
Adjuvant: magnesium stearate 3g, sucrose 1.2g, the starch slurry of 10%, 1.5g microcrystalline Cellulose
Preparation method:
(1) dynamically concentration ethanol extracts Pericarpium Arecae, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae effective ingredient continuously
The alcoholic solution of 95% is added in Chinese medicament extracting device, mixed after the Pericarpium Arecae of recipe quantity, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae are pulverized 100 mesh sieves, from the dog-house of extractor, dropped into material after infiltration, after feeding intake, heated and stirred is carried out to extractor, and to control final temperature be 68 DEG C.
Extractor top connects a water tank, makes it and extractor UNICOM, is provided with valve switch and effusion meter between water tank and extractor, and wherein effusion meter can control water in water tank and flow into the speed of extractor.While extractor is heated, also water in water tank is heated, make Water in Water Tanks temperature consistent with temperature in extractor.
After temperature stabilization in water tank and extractor, opening the valve switch of water tank, by controlling the flow velocity of water in water tank, the water in water tank slowly being instilled in extractor, ensure that in extractor, concentration of alcohol rate of change is 0.42%/min, continuing to stir also, control temperature is constant.After reaction 2h, when concentration of alcohol in extractor is 50%, stopped reaction.
Extractor bottoms can folding be provided with filter screen, and after first set reaction terminates, extractor bottoms is opened, and medicinal residues are extracted device bottom screen and intercept, and extracting solution flows down along extractor bottoms and filters after condensation and collect.
Again closed extractor bottoms, the ethanol that concentration is 50% is added in medicinal residues after first set reaction terminates, and slowly add water according to the step of the first reaction, concentration of alcohol rate of change in extractor is kept to be 0.68%/min, in reaction 1h to extractor, concentration of alcohol becomes 10%, the filtrate of collecting with first time after collecting filtrate cold filtration merges, and collects filtering residue.
Collected filtrate is condensed into thick paste.
(2) Rhizoma Atractylodis, Cortex Magnoliae Officinalis volatile oil constituents extraction
The Rhizoma Atractylodis magnolia obovata of recipe quantity, crosses 150 mesh sieves after pulverizing, carries out microwave extracting, wherein microwave extracting power is 400w, solid-liquid ratio 1:40, Extraction solvent is the alcoholic solution of 80%, extracts 15min, after repeating extraction 3 times, filter, merging filtrate, by filtrate reduced in volume, obtain Mixed chaotic sequences, and collect filtering residue.
(3) process of preparing Chinese medicine of Poria and the mixing of thick paste
After simply being washed by the Poria raw material of recipe quantity, be cut into the lamellar of thickness equalization, and the thick paste of positive and negative uniform application step (1) gained repeatedly in Indian buead tablet, steaming and decocting 30min in steamer, controls steamer temperature and is no more than 70 DEG C.
After first time steaming and decocting terminates, again smear remaining thick paste, carry out steaming and decocting; Steaming and decocting is coated with most to thick paste and infiltrates in Indian buead tablet completely for 3 times so repeatedly, is dried by Poria and wears into fine powder, for subsequent use.
(4) preparation of tablet
The cane sugar powder of recipe quantity is broken into fine powder.
By the Radix Glycyrrhizae extractum mix homogeneously of the dried cream powder in step (3) and recipe quantity, add the microcrystalline Cellulose of Icing Sugar, starch slurry and recipe quantity, mix soft material granulation processed, dry after crossing 14 mesh sieves.
After the Folium perillae acutae oil of the Mixed chaotic sequences of step (2) and recipe quantity, patchouli oil being mixed homogeneously, add granule dry after sieving, and add magnesium stearate mixing, be pressed into 925, every sheet 0.62g.
Comparative example
1. Radix Angelicae Dahuricae extracts active ingredients (percolation)
Ethanol percolate extraction: medical material soaks 24h, and alcoholic solution crosses 120 mesh sieves, and supersound process (300w, 45kHz) adds the ethanol 8 times amount percolation of 80% for 30 minutes, extracts percolate, and concentrating under reduced pressure reclaims ethanol and obtains percolate.
2, Radix Angelicae Dahuricae extracts active ingredients (alcohol extraction)
Radix Angelicae Dahuricae root with 95% ethanol extraction 3 times, each 2 hours, merge extractive liquid, was evaporated to without alcohol taste.
3. Pericarpium Citri Reticulatae extracts active ingredients
Volatile oil in Pericarpium Citri Reticulatae take alcohol extraction as the best, is first collected by volatile oil in Pericarpium Citri Reticulatae by the way of distillation, is being dissolve to extract with ethanol.
Tangerine peel powder is broken into most coarse powder, at 85 DEG C of Extracting temperature, concentration of alcohol 95%, extracts 3 times, each extraction time 1h.Merge extractive liquid, concentrating under reduced pressure reclaims ethanol must beat Pericarpium Citri Reticulatae extract.
4. Rhzoma Atractylodis Lanceae volatile oil extracts
Rhizoma Atractylodis being ground into granularity is 0.05-0.15mm, ethanol: petroleum ether=2:1 is that solvent carries out microwave extraction, and wherein solid-liquid ratio is 1:40, extraction time 25min, pressure 20Mpa, and Extracting temperature is 45 DEG C, collects volatile oil.
5. the extraction of Cortex Magnoliae Officinalis volatile oil
After Cortex Magnoliae Officinalis being pulverized, carry out microwave extraction, wherein microwave power is 350W, and solvent is the ethanol of 75%, and extraction time is 4min, and solid-liquid ratio is 1:40.
6. the preparation (pharmacopeia) of HUOXIANG ZHENGQI PIAN
Prescription: Rhizoma Atractylodis 86g, Pericarpium Citri Reticulatae 86g, Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 86g, Radix Angelicae Dahuricae 130g, Poria 130g, Pericarpium Arecae 130g, Rhizoma Pinelliae 86g, Radix Glycyrrhizae extractum 11g, patchouli oil 0.9ml, Folium perillae acutae oil 0.4ml
Preparation method: ten tastes more than (1), Radix Angelicae Dahuricae 81g is ground into fine powder, for subsequent use;
(2) Pericarpium Citri Reticulatae extracts after volatile oil mixes with patchouli oil, Folium perillae acutae oil and dissolves with appropriate amount of ethanol, for subsequent use;
(3) aqueous solution carried after oil is continued to employ, and medicinal residues decoct with water 1 hour, and filter, filtrate is for subsequent use;
(4) Pericarpium Arecae, Poria decoct with water secondary, 2 hours first times, second time 1 hour, and filter, merging filtrate, adds the aqueous solution after carrying oil and above-mentioned filtrate, and filter, filtrate is for subsequent use;
(5) Rhizoma Pinelliae cold water soak, does not have within 8 hours, change water once, separately adds Rhizoma Zingiberis 7.3g after the brewed heart, decoct with water secondary, filter, merging filtrate, add above-mentioned filtrate and Radix Glycyrrhizae extractum, be concentrated into the clear paste that relative density is 1.2-1.3 (55 DEG C);
(6) Radix Angelicae Dahuricae 49g, Rhizoma Atractylodis, Cortex Magnoliae Officinalis 60% alcohol reflux three times, 6 hours first times, second time 4 hours, 2 hours third times, merges above-mentioned ethanol extract, and filter, filtrate recycling ethanol, is condensed into cream;
(7) merge water, alcohol condensed cream, add Radix Angelicae Dahuricae fine powder and right amount of auxiliary materials, mixed pelletization is dry, is blended into the alcoholic solution of patchouli oil, Folium perillae acutae oil and Oleum Citri Reticulatae, and mixing is pressed into 1000, or is pressed into 1000 film coatings.
Experimental example:
1, Pericarpium Arecae, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and the research of Pericarpium Citri Reticulatae extracts active ingredients
Chemical composition of Chinese materia medica is complicated, and heterogeneity polarity difference is large, the polyol that such as glucose, sucrose equimolecular are smaller, has strongly hydrophilic, very easily water-soluble.Protein and aminoacid are all soda acid amphoteric compounds, have polarity to a certain degree, so can be water-soluble, be insoluble to or be insoluble in organic solvent.The dissolubility of flavone compound has very big-difference because of structure and existence (glycosides or aglycon, monoglycosides, disaccharidase glycosides or three glucosides) difference.Glycoside is all strong than the hydrophilic of its aglycon, and be particularly often combined with most glycan molecule in the molecule of saponin due to them, hydroxy number is many, can show stronger hydrophilic, and sapogenin then belongs to the strong compound of lipotropy.Most free alkaloids is lipophilic compound, after acid is in conjunction with salify, can ionizing, and strengthen polarity, these alkaloids can be described as semi-polarity compound.So alkaloidal salt is soluble in water, insoluble or be insoluble in organic solvent; And most free alkaloid is insoluble or be insoluble in water, be soluble in lipophilic solvent.Oils and fats, volatile oil, fat-soluble pigment are all strong lipophilic compositions.Chinese medicine extraction often needs effective component extracting as much as possible, strengthens pharmaceutically active.Step of the present invention (2) adopts continuously the method that dynamically concentration of alcohol extracts to extract Chinese medicine, can extract the effective ingredient of opposed polarity more fully.
The present invention is in the extraction to described medical material effective ingredient, Automatic continuous is taked to change the method for concentration of alcohol, extract the active ingredient in described medicine, to guarantee the extraction dynamics of the described medical material effective ingredient of raising in described medical material, guarantee that described medical material effective ingredient can extract completely at different conditions simultaneously.
In 1.1 researchs, random selecting Pericarpium Citri Reticulatae, the Rhizoma Pinelliae and the Radix Angelicae Dahuricae are studied, and utilize GC-MS to analyze its chemical composition, the results are shown in Table 1.
Table 1 extraction conditions is studied
Conclusion: by the extracting method in step of the present invention (1), can more complete by the extracts active ingredients in medical material.
1.2 step of the present invention (1) extracting method compared with the prior art
Extracting method and the prior art extracting method of step of the present invention (1) compare, the material Radix Angelicae Dahuricae in 3 in random selecting step (2), Pericarpium Citri Reticulatae and the Rhizoma Pinelliae, for comparing material, contrast with existing extractive technique, and its comparative result is as shown in table 2.
The comparison of table 2 Different Extraction Method
Conclusion: as can be seen from Table 2, compared with prior art, the extraction of effective ingredient is more complete, and the extraction ratio of effective ingredient is higher for extracting method of the present invention.
Can be found out by table 1 and table 2, the extraction ratio of the present invention to medical material effective ingredient is higher.For the reason producing this experimental result, although those skilled in the art temporarily cannot provide mechanism explain accurately, but the applicant infers, may be because the effective ingredient dissolubility in a solvent of medical material under different ethanol concentration is different, the effective ingredient that thus can extract is more, and different material contained in different medical material may to other effective ingredient in ethanol be dissolved with facilitation, thus cause specific active constituent content to improve.
Therefore, the extracting method in step of the present invention (1) is adopted high efficiency extraction can be carried out to active substance in medical material.
2. the research of Rhizoma Atractylodis magnolia obovata essential oil extraction method
In prior art, the extracting method of Rhizoma Atractylodis magnolia obovata volatile oil has multiple, adopts microwave to help extracting method to extract the Mixed chaotic sequences of Rhizoma Atractylodis magnolia obovata in step of the present invention (2), to expect, by improving extraction conditions, to improve the extraction ratio of Mixed chaotic sequences.
Study the process conditions of step in embodiment of the present invention 1-5 (2), and carry out GC-MS analysis to gained volatile oil, acquired results is in table 3 and table 4.
The selection of table 3 experiment condition of the present invention
The contrast of table 4 the present invention and prior art
Conclusion: adopt microwave to help in step of the present invention (2) and carry extraction Rhizoma Atractylodis magnolia obovata Mixed chaotic sequences, its effective ingredient is consistent with prior art, the yield of its active substance is higher than prior art, proves that step of the present invention (2) has certain superiority.
For acquired results in step of the present invention (2), although those skilled in the art temporarily cannot provide and explain accurately, but the applicant infers, may be because different material contained in different medical material may have facilitation to other effective ingredient in extraction, thus cause specific active constituent content to improve.
3. the process of preparing Chinese medicine research of dry extract and Poria
Step 3 of the present invention) in by Poria concoct after mix with thick paste.In the processing of medical material, the method that Chang Huiyong concocts is processed, and usual medical material, after concocting, can reduce the content of harmful substance, improves the ratio of effective ingredient.Therefore, step 3 of the present invention) method of also attempting to use for reference the process of preparing Chinese medicine conventional in Chinese medicine processes Poria and thick paste, to reaching useful effect.To this, the present invention to the effective ingredient after concocting in Poria and after concocting the mixture of Poria and thick paste analyze, its experimental procedure and result as follows.
The mensuration of 3.1 pachyman content
Phenol 100g is got in the preparation of 4% phenol solution, with aluminium flake 0.1g and sodium bicarbonate 0.05g, distill and collect 182 DEG C of fractions, taking 4g, be dissolved in water to graduation mark at 100ml volumetric flask, then put cold preservation in refrigerator (its fraction must be collected 182 DEG C time) for subsequent use.In still-process, also to control degree of condensation well, if the discharge in condensing tube is too fast, then can makes fraction crystallization wherein very soon and have influence on the normal collection of fraction.
Preparation standard curve
Precision takes the anhydrous grape saccharide 15mg putting dry more than 12h in phosphorus pentoxide vacuum drying apparatus, put in 25ml volumetric flask, be dissolved in water and be diluted to scale, shaking up (about 24 DEG C) under putting room temperature (concentration is 0.6mg/ml) for subsequent use.Precision measures reference substance solution 0.0,1.0,2.0,3.0,4.0,5.0ml, is placed in 100ml volumetric flask respectively, and adds water to scale, shake up.Precision measures above-mentioned each solution 2ml, puts in tool plug test tube, adds the phenol solution 1ml of 4% respectively, after mixing
Add rapidly concentrated sulphuric acid 7.0ml, shake up, and take out be incubated 30min in 45 DEG C of water-baths after, put in ice-water bath and take out after 5min.Then with the 1st part for blank group, measure its trap A with spectrophotography at the wavelength place of 490nm, with absorbance (A) for vertical coordinate, solution concentration C is abscissa.Statistics, carries out linear regression.Obtain regression equation: Y=0.0114+0.0183X, correlation coefficient r=0.9995, concentration of glucose is good linear relationship at 0.006 ~ 0.03mg/ml scope internal absorbance and concentration.
Phend-sulphuric acid surveys pachyman content
Each extracting method gained sample is made the solution of 1g/ml, precision measures 2ml, method under the preparation of sighting target directrix curve, with its absorbance of determined by ultraviolet spectrophotometry, from the regression equation of standard curve, calculate solution concentration to be measured, and calculate its polyoses content (with glucose gauge) further.Shown in its result table table 5.
Table 5 measurement result result
The investigation of Poria and thick paste after 3.2 processes of preparing Chinese medicine
Learnt from else's experience after concocting and be mixed with the Indian buead tablet of thick paste, observe outward appearance and the uniformity etc. of powder after beating powder of material after concocting, it the results are shown in Table 6.
The mixing situation of table 6 material
Conclusion: shown by the experiment of table 5 and 6, through the process of preparing Chinese medicine of step of the present invention (3), not only can improve the effective ingredient pachyman in Poria, and unexpected discovery the method can by thick paste and medical material Homogeneous phase mixing, this just makes the present invention in the preparation process of tablet, material be fully mixed into possibility, thus saving time, under saving the prerequisite of the energy, the content uniformity of medicine effective ingredient is improved, while raising drug effect, product of the present invention is realized further quality controllable, substantially increase its qualification rate.
The investigation of 4 adjuvants
Supplementary product starch is made starch slurry by the embodiment of the present invention 4 and 5, and in embodiment 5, add microcrystalline Cellulose as diluent and disintegrating agent, in this effects tablet, adjuvant is to its preparation and shaping etc., wherein the inspection of disintegration is according to disintegration in " Chinese Pharmacopoeia " annex in 2010, inspection technique measured, the condition that the stability of tablet examines wiping be tablet at 25 ± 2 DEG C, relative humidity is 60 ± 10%.Its result is as shown in table 7.
Table 7 starch slurry is on the impact of tablet
Conclusion: starch slurry of the present invention is binding agent, does binding agent than in additive method with water, it more can improve the stability of medicine; And after adding microcrystalline Cellulose, the disintegration of medicine can be improved, be more conducive to the drug effect playing medicine.
5. pharmacodynamic experiment
HUOXIANG ZHENGQI PIAN has removing dampness of inducing sweat, effect of regulating the flow of Qi and the middle Jiao.For summer-heat damp cold, headache heavy sensation of the body is uncomfortable in chest, or fever with aversion to cold, and abdominal distention, vomiting is had loose bowels.In general, HUOXIANG ZHENGQI PIAN is mainly applicable to following several situation: the influenza of common cold of gastrointestinal type, viral influenza and some types, diarrhoea, acute or chronic gastritis, functional gastropathy, catch cold summer the gastrointestinal upset caused, or because of the diarrhoea caused by eating and drinking without temperance, acute or chronic gastritis, functional gastropathy etc., use HUOXIANG ZHENGQI JIAONANG treatment also to have good therapeutic effect.
Therefore, the present invention is directed to effect of HUOXIANG ZHENGQI PIAN, adopt the drug effect of the HUOXIANG ZHENGQI PIAN of different animal model tests preparation method gained of the present invention.
5.1 analgesic experiment
Get white mice some, be divided into 7 groups at random, often organize 15.Give the medicine prepared by the normal saline of same dose, embodiment 1-5 and comparative example 6 medicament respectively.30 minutes lumbar injection 0.3% acetic acid after administration, 0.2ml/ only, observes the writhing number that in 30 minutes, each treated animal is brought out by acetic acid.Experiment shows, causes more lasting pain to irritate after mouse peritoneal injection acetic acid.After administration, in embodiment 1-5 group and comparative example 6 groups, the pain reaction of mice has and reduces in various degree, and the animal writhing number in embodiment 1-5 group is obviously less than comparative example example 1 group, and therefore analgesic activity of the present invention is remarkable.Experimental result is in table 8.
Table 8 writhing number of times is tested
| Group | Dosage (g/kg) | Writhing number of times |
| Normal saline group | ———— | 2l.3±1l.0 |
| Embodiment 1 | 20 | 7.8±4.1 |
| Embodiment 2 | 20 | 8.9±3.2 |
| Embodiment 3 | 20 | 8.5±4.0 |
| Embodiment 4 | 20 | 8.7±3.7 |
| Embodiment 5 | 20 | 7.8±4.1 |
| Comparative example 6 | 20 | 19.8±2.2 |
Compare with normal saline group: * p<0.05, * * p<0.01, with matched group ratio: #p<0.05
5.2 antiinflammatory experiments
Get 180-220g male rat some, be divided into 7 groups at random, often organize 15.Give same dose normal saline, embodiment 1-5 medicament and comparative example 6 medicament respectively, and be successive administration 2 days, fasting is after 10 hours, first survey before last administration and do not cause the sufficient volume of wasting time of scorching each Rat Right, then administration, and the carrageenin 0.2ml/ giving 1% only, to waste time subtenon injection in left foot.Then after causing inflammation, the sufficient volume of wasting time of each Rat Right within 1,2,4,6 hour, is surveyed, obtain different time and respectively organize the sufficient change in volume of wasting time of rat, each group of swelling is see table 8, statistical between t checks and organizes, here swelling=(volume after causing inflammation-cause scorching front volume)/cause scorching front volume × 100%, as table 8.Experimental result shows, the rat paw edema that medicament on Carrageenan prepared by the present invention causes has obvious inhibitory action, and its antiinflammatory action is better than comparative example 6 groups.
Table 9 the present invention is on the impact of the sufficient swelling of wasting time of rat
5.3 In vivo antibacterial experiment
First the trial test of infection dosage is carried out.Get the NIH kind mice 100 that body weight is 12-14g, male and female half and half, are divided into 5 groups at random, often organize 20, and each group body weight is without significant difference (p<0.05).Only, each group infection dosage is respectively 2 × 10 to each group of staphylococcus aureus respectively at lumbar injection variable concentrations gradient (being purchased from Nat'l Pharmaceutical & Biological Products Control Institute's strain room) liquid 0.4ml/
8/ only, 4 × 10
8only, 6 × 10
8only, 8 × 10
8/ only, 10 × 10
8/ only.Observe the death condition of animal in 15 days, result is see table 9.Table 10 illustrates that infection dosage is 6 × 10
8/ mouse death rate only, more than 80%, is finally determined with 6 × 10
8/ be only test infection dosage.
Table 10 mouse infection bacterium amount preliminary result
| Infection dosage/only | Number of animals | Death toll | Mortality rate/% |
| 2×10 8 | 20 | 4 | 20 |
| 4×10 8 | 20 | 11 | 55 |
| 6×10 8 | 20 | 17 | 85 |
| 8×10 8 | 20 | 20 | 100 |
| 10×10 8 | 20 | 20 | 100 |
Get NIH kind mice some, body weight is 12.8 ± 0.96g, and male and female half and half are divided into 7 groups at random, often organizes 20, is respectively and infects matched group, embodiment 1-5 group and comparative example 6 groups.Except infection matched group, each group gives 40.0g crude drug respectively, each group weight ratio comparatively there was no significant difference (p<0.05), before infection, embodiment 1-5 group and comparative example 6 groups, respectively gastric infusion 1 day, 2 times on the one, infect matched group and fill with distilled water; Second day, only, infection dosage was 6 × 10 to each group lumbar injection S. aureus L-forms liquid 0.4ml/
8/ only, embodiment 1-5 group and comparative example 6 groups, continue gastric infusion respectively, 2 times on the one, successive administration 2 days; Then the general behavior of animal, death toll and death time is observed, Continuous Observation 15 days, X
2(2 × 2) method inspection experimental result, result is see table 10, and result shows, and the animal dis motility rate of embodiment 1-5 group is significantly higher than comparative example 6 groups, illustrates that antibacterial action of the present invention obtains reinforcement.
The anti-bacterial result in table 11 body
| Group | Number of animals | Death toll | Mortality rate/% |
| Matched group | 20 | 17 | 85 |
| Embodiment 1 | 20 | 3 | 15 |
| Embodiment 2 | 20 | 6 | 30 |
| Embodiment 3 | 20 | 5 | 25 |
| Embodiment 4 | 20 | 4 | 20 |
| Embodiment 5 | 20 | 3 | 15 |
| Comparative example 6 | 20 | 11 | 55 |
Claims (4)
1. a HUOXIANG ZHENGQI PIAN, its prescription and consumption are Rhizoma Atractylodis 160g, Pericarpium Citri Reticulatae 160g, Sichuan Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 160g, Radix Angelicae Dahuricae 240g, Poria 240g, Pericarpium Arecae 240g, Rhizoma Pinelliae 160g, Radix Glycyrrhizae extractum 20g, patchouli oil 1.6ml, Folium perillae acutae oil 0.8ml, its adjuvant and consumption thereof are magnesium stearate 3g, and Icing Sugar 1.2g, is characterized in that: its preparation method is 1) dynamically concentration change alcoholic solution extracts Pericarpium Arecae, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae effective ingredient continuously; 2) Rhizoma Atractylodis, Cortex Magnoliae Officinalis volatile oil constituents extraction; 3) process of preparing Chinese medicine of Poria and the mixing of thick paste; 4) preparation of tablet.
2. HUOXIANG ZHENGQI PIAN according to claim 1, is characterized in that: preparation method is
1) dynamically concentration change alcoholic solution extracts Pericarpium Arecae, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae effective ingredient continuously
The alcoholic solution of 95% is added in Chinese medicament extracting device, mixed after the Pericarpium Arecae of recipe quantity, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae are pulverized 50-150 mesh sieve, from the dog-house of extractor, dropped into material after infiltration, after feeding intake, heated and stirred is carried out to extractor, and to control final temperature be 65-75 DEG C;
Extractor top connects a water tank, makes it and extractor UNICOM, is provided with valve switch and effusion meter between water tank and extractor, and wherein effusion meter can control water in water tank and flow into the speed of extractor; While extractor is heated, also water in water tank is heated, make Water in Water Tanks temperature consistent with temperature in extractor;
After temperature stabilization in water tank and extractor, open the valve switch of water tank, by controlling the flow velocity of water in water tank, water in water tank is slowly instilled in extractor, ensure that in extractor, concentration of alcohol rate of change is that also control temperature is constant in 0.3-0.5%/min continuation stirring, after reaction 1.5-2.5h, when in extractor, concentration of alcohol is about 40-60%, stopped reaction;
Extractor bottoms can folding be provided with filter screen, and after first set reaction terminates, extractor bottoms is opened, and medicinal residues are extracted device bottom screen and intercept, and extracting solution flows down along extractor bottoms and filters after condensation and collect;
Again closed extractor bottoms, the ethanol that concentration is 40-60% is added in medicinal residues after first set reaction terminates, and slowly add water according to the step of the first reaction, ensure that in extractor, concentration of alcohol rate of change is 0.2-1.3%/min, in reaction 0.5-1.5h to extractor, concentration of alcohol becomes 5-15%, the filtrate of collecting with first time after collecting filtrate cold filtration merges, and collects filtering residue; Collected filtrate is condensed into thick paste;
2) Rhizoma Atractylodis, Cortex Magnoliae Officinalis volatile oil constituents extraction
The Rhizoma Atractylodis magnolia obovata of recipe quantity, crosses 50-200 mesh sieve after pulverizing, carries out microwave extracting, wherein microwave extracting power is 300-450w, solid-liquid ratio 1:30-1:45, Extraction solvent is the alcoholic solution of 60-85%, extracts 10-25min, after repeating extraction 3 times, filter, merging filtrate, by filtrate reduced in volume, obtain Mixed chaotic sequences, and collect filtering residue;
3) process of preparing Chinese medicine of Poria and the mixing of thick paste
After simply being washed by the Poria raw material of recipe quantity, be cut into the lamellar of thickness equalization, and the thick paste of positive and negative uniform application step 1) gained repeatedly in Indian buead tablet, steaming and decocting 15-45min in steamer, controls steamer temperature and is no more than 70 DEG C;
After first time steaming and decocting terminates, again smear remaining thick paste, carry out steaming and decocting; So steaming and decocting is infiltrated in Indian buead tablet completely to thick paste for 3 times repeatedly, is dried by Poria and wears into fine powder, for subsequent use;
4) preparation of tablet
By the Radix Glycyrrhizae extractum mix homogeneously of the dried cream powder in step 3) and recipe quantity, add the sucrose of recipe quantity and appropriate water, mix soft material granulation processed, dry after crossing 14 mesh sieves;
By step 2) the Folium perillae acutae oil of Mixed chaotic sequences and recipe quantity, patchouli oil mix homogeneously after, add granule dry after sieving, and add magnesium stearate mixing, film coating is pressed into 500, every more than sheet 0.5g.
3. HUOXIANG ZHENGQI PIAN according to claim 2, is characterized in that: its preparation method is
1) dynamically concentration ethanol extracts Pericarpium Arecae, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae effective ingredient continuously
The alcoholic solution of 95% is added in Chinese medicament extracting device, mixed after the Pericarpium Arecae of recipe quantity, the Rhizoma Pinelliae, the Radix Angelicae Dahuricae and Pericarpium Citri Reticulatae are pulverized 100 mesh sieves, from the dog-house of extractor, dropped into material after infiltration, after feeding intake, heated and stirred is carried out to extractor, and to control final temperature be 68 DEG C;
Extractor top connects a water tank, makes it and extractor UNICOM, is provided with valve switch and effusion meter between water tank and extractor, and wherein effusion meter can control water in water tank and flow into the speed of extractor,
While extractor is heated, also water in water tank is heated, make Water in Water Tanks temperature consistent with temperature in extractor;
After temperature stabilization in water tank and extractor, opening the valve switch of water tank, by controlling the flow velocity of water in water tank, the water in water tank slowly being instilled in extractor, ensure that in extractor, concentration of alcohol rate of change is 0.42%/min, continuing to stir also, control temperature is constant; After reaction 2h, when concentration of alcohol in extractor is 50%, stopped reaction;
Extractor bottoms can folding be provided with filter screen, and after first set reaction terminates, extractor bottoms is opened, and medicinal residues are extracted device bottom screen and intercept, and extracting solution flows down along extractor bottoms and filters after condensation and collect;
Again closed extractor bottoms, the ethanol that concentration is 50% is added in medicinal residues after first set reaction terminates, and slowly add water according to the step of the first reaction, concentration of alcohol rate of change in extractor is kept to be 0.68%/min, in reaction 1h to extractor, concentration of alcohol becomes 10%, the filtrate of collecting with first time after collecting filtrate cold filtration merges, and collects filtering residue; Collected filtrate is condensed into thick paste;
2) Rhizoma Atractylodis, Cortex Magnoliae Officinalis volatile oil constituents extraction
The Rhizoma Atractylodis magnolia obovata of recipe quantity, crosses 150 mesh sieves after pulverizing, carries out microwave extracting, wherein microwave extracting power is 400w, solid-liquid ratio 1:40, Extraction solvent is the alcoholic solution of 80%, extracts 15min, after repeating extraction 3 times, filter, merging filtrate, by filtrate reduced in volume, obtain Mixed chaotic sequences, and collect filtering residue;
3) process of preparing Chinese medicine of Poria and the mixing of thick paste
After simply being washed by the Poria raw material of recipe quantity, be cut into the lamellar of thickness equalization, and the thick paste of positive and negative uniform application step 1) gained repeatedly in Indian buead tablet, steaming and decocting 30min in steamer, controls steamer temperature and is no more than 70 DEG C;
After first time steaming and decocting terminates, again smear remaining thick paste, carry out steaming and decocting; Steaming and decocting is coated with most to thick paste and infiltrates in Indian buead tablet completely for 3 times so repeatedly, is dried by Poria and wears into fine powder, for subsequent use;
4) preparation of tablet
By the Radix Glycyrrhizae extractum mix homogeneously of the dried cream powder in step 3) and recipe quantity, add the sucrose of recipe quantity and appropriate water, mix soft material granulation processed, dry after crossing 14 mesh sieves;
By step 2) the Folium perillae acutae oil of Mixed chaotic sequences and recipe quantity, patchouli oil mix homogeneously after, add granule dry after sieving, and add magnesium stearate mixing, film coating is pressed into 500, every sheet 0.62g.
4. the HUOXIANG ZHENGQI PIAN according to claim 1-3 any one, is characterized in that: its adjuvant can add starch slurry and microcrystalline Cellulose.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510588928.0A CN105079362A (en) | 2015-09-16 | 2015-09-16 | Huoxiang Zhengqi tablet |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510588928.0A CN105079362A (en) | 2015-09-16 | 2015-09-16 | Huoxiang Zhengqi tablet |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110982657A (en) * | 2019-12-29 | 2020-04-10 | 通化市赫思恩科技有限公司 | Method for rapidly preparing red ginseng wine by gradient ultrasonic extraction method |
| CN115105480A (en) * | 2021-03-18 | 2022-09-27 | 河北百善药业有限公司 | Agastache rugosus vital energy strengthening tablet and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614335A (en) * | 2011-01-28 | 2012-08-01 | 北京亚东生物制药有限公司 | Method for preparing Huoxiang Zhengqi oral liquid |
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2015
- 2015-09-16 CN CN201510588928.0A patent/CN105079362A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614335A (en) * | 2011-01-28 | 2012-08-01 | 北京亚东生物制药有限公司 | Method for preparing Huoxiang Zhengqi oral liquid |
Non-Patent Citations (1)
| Title |
|---|
| 孔令仪等: "《天然药物化学》", 31 August 2015, 中国医药科技出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110982657A (en) * | 2019-12-29 | 2020-04-10 | 通化市赫思恩科技有限公司 | Method for rapidly preparing red ginseng wine by gradient ultrasonic extraction method |
| CN115105480A (en) * | 2021-03-18 | 2022-09-27 | 河北百善药业有限公司 | Agastache rugosus vital energy strengthening tablet and preparation method thereof |
| CN115105480B (en) * | 2021-03-18 | 2024-02-27 | 河北百善药业有限公司 | Huoxiang Zhengqi tablet and preparation method thereof |
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Application publication date: 20151125 |