CN107582747B - Preparation method of Jinma Gantai preparation - Google Patents
Preparation method of Jinma Gantai preparation Download PDFInfo
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Abstract
The invention discloses a preparation method of a Jinma Gantai preparation, belonging to the technical field of traditional Chinese medicine preparations. JINMAGANTAI preparation is prepared from herba Eleocharis Turerosae, herba Berchemiae Lineatae, herba Verbenae, radix Stephaniae Tetrandrae, herba Patriniae, herba Epimedii, radix astragali, radix Paeoniae Rubra, Saviae Miltiorrhizae radix and adjuvants; the invention makes clear the category and the property of the active ingredients according to the functional main treatment of the Jinma Gantai capsule, extracts and purifies the active ingredients of the traditional Chinese medicines in a classified way, and adopts a mode of combining high-speed centrifugation and macroporous adsorption resin, thereby maximally extracting and purifying the active ingredients of the traditional Chinese medicines and improving the curative effect of the Jinma Gantai preparation on acute and chronic hepatitis.
Description
Technical Field
The invention relates to a preparation method of a Jinma Gantai preparation, belonging to the technical field of traditional Chinese medicine preparations.
Background
Hypochondriac swelling pain and burning sensation, abdominal distention and anorexia, bitter taste and nausea, scanty or yellow urine, irregular stool, yellow eyes and body, red tongue with yellow and greasy coating, and wiry and rapid pulse are common clinical symptoms. Traditional Chinese medicine usually adopts means of soothing liver and nourishing blood, and regulating qi and removing blood stasis to treat the liver and blood stasis. Traditional Chinese medicine considers that the deficiency of vital qi easily infects epidemic toxin, the bad dietary habit damages the spleen and stomach but can not resolve dampness, damp-heat is endogenous, liver is injured by spleen to cause incoordination between liver, gallbladder and spleen, and damage to vital qi is increased. The Jinma Gantai preparation is prepared with creeping dichondra, verbena, patrinia and tetrandra root with the functions of clearing away heat and toxic material and promoting diuresis, astragalus root as qi invigorating medicine, red sage and berchemia lineate as well as red peony root and epimedium for clearing away heat and cooling blood and nourishing liver and kidney. In the formula, the creeping dichondra, the verbena, the patrinia herb and the radix stephaniae tetrandrae are taken as main bodies and are used for clearing the accumulated damp-heat of the liver and the gallbladder, the epimedium is added for tonifying the liver and the kidney and strengthening the bones and muscles, the berchemia lineate and the salvia miltiorrhiza can not only activate blood and nourish blood but also can regulate qi to generate blood stasis caused by deficiency, and the astragalus is also used for tonifying qi and invigorating yang, inducing diuresis to alleviate edema, enhancing the effects of activating blood and dissolving stasis, clearing heat and promoting diuresis, and relieving the symptoms of. The medicines are mutually assisted, mainly clear liver and gallbladder damp-heat, promote blood circulation to remove blood stasis and tonify qi, nourish blood, sooth liver and remove blood stasis as the root, and the whole formula treats both symptoms and root causes by differentiation of symptoms and signs; is good at relieving symptoms such as hypochondriac distending pain and burning sensation, abdominal distention and anorexia, bitter taste and nausea, scanty and brownish urine, abnormal stool, or yellow eyes and body, red tongue with yellow and greasy fur, wiry and rapid pulse, etc. caused by deficiency of vital qi, incoordination between spleen and stomach, damp-heat in liver and gallbladder, and qi stagnation and blood stasis. Modern pharmacological research proves that the prescription has the effects of protecting liver, resisting inflammation and virus, relieving pain, enhancing immunity, resisting thrombus and the like; has exact curative effect on treating acute and chronic hepatitis caused by damp-heat in liver and gallbladder and qi stagnation and blood stasis.
The existing method for producing the Jinma Gantai capsule generally adopts the method recorded in the drug standard (YBZ08762009), and the method recorded in the standard is simpler, so that the product contains a large amount of ineffective components and impurities, and the clinical curative effect of the Jinma Gantai granular preparation is not ideal.
In addition, chinese patent CN102813752 a discloses a preparation method of a Jinma Gantai preparation, which is prepared from creeping dichondra, berchemia lineate, verbena, radix stephaniae tetrandrae, herba patriniae, herba epimedii, radix astragali, radix paeoniae rubra, radix salviae miltiorrhizae and auxiliary materials; according to the properties of each medicine in the formula of the Jinma Gantai granule and the action of the medicine in the formula, the preparation process is optimized, and compared with the method recorded on the medicine standard (WS-10313(ZD-0313) -2002), the product prepared by the process has high content of active ingredients and good clinical curative effect. However, the method simply extracts and purifies the six traditional Chinese medicines except the zanthoxylum dissitum, the radix stephaniae tetrandrae and the epimedium by adopting a water extraction and alcohol precipitation process, the water extraction and alcohol precipitation process has non-negligible influence on the content of various active ingredients of the traditional Chinese medicines, not only can cause different degrees of loss on small molecule active ingredients such as alkaloids, flavonoids, saponins, organic acids and the like, but also can cause loss of a large part of active ingredients under the actions of adsorption, wrapping and the like in the alcohol precipitation process, and the removal rate and the type of impurities are greatly different along with the influence of alcohol precipitation concentration and human factors. In addition, the alcohol precipitation process causes serious loss of total solids and effective components, has large ethanol consumption, low recovery rate and long production period, and the alcohol precipitation treatment affects the content of the effective components and greatly reduces the internal quality of finished products. After the precipitate is removed, ethanol is required to be recovered, and the process of recovering ethanol not only consumes time and energy, but also has great influence on the effective components of the traditional Chinese medicine.
Although the refining of the alcohol precipitation method is the main mode of industrial production in most pharmaceutical factories at present, the method has the defects of large loss of effective components, incomplete impurity removal, poor stability and the like, so that the search for a new technology and a new process for replacing the water extraction and alcohol precipitation method is imperative. According to the related research and practice, the newly developed high-speed centrifugation technology, membrane separation technology, adsorption clarification technology, macroporous resin adsorption technology and the like show strong superiority in the aspects of clarification, separation, purification and the like of the traditional Chinese medicine extracting solution, and are gradually popularized and applied.
Macroporous resin column chromatography is a novel nonionic high molecular compound, is a common method for separating compounds with larger polarity in recent years, has stable physicochemical property, is insoluble in acid, alkali and organic solvents, has good selectivity to organic matters, and is not influenced by inorganic salt plasma and low molecular compounds. The macroporous resin column chromatography is to pass the aqueous solution of the Chinese medicinal extract through a macroporous resin column to adsorb the active ingredients therein, wash with water to remove water-soluble impurities, then wash with ethanol with different concentrations sequentially from low to high, and finally subpackage according to different concentrations and recover samples. The macroporous adsorption resin has good adsorption and separation performance and is also suitable for industrial production, so the macroporous adsorption resin separation method is a better separation method.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a Jinma Gantai preparation.
In order to solve the technical problems, the invention adopts the following technical scheme:
a Jinma Gantai preparation is prepared from 900-1000 parts of creeping dichondra, 450-600 parts of berchemia lineate, 300-450 parts of verbena, 600-700 parts of tetrandra root, 300-450 parts of herba patriniae, 450-600 parts of epimedium, 450-600 parts of astragalus root, 450-600 parts of red peony root, 700-800 parts of salvia miltiorrhiza and auxiliary materials according to weight parts.
Specifically, the Jinma Gantai preparation is prepared from 960.7 parts of creeping dichondra, 511 parts of berchemia lineate, 383.3 parts of verbena, 638.7 parts of radix stephaniae tetrandrae, 383.3 parts of herba patriniae, 511 parts of herba epimedii, 511 parts of radix astragali, 511 parts of red paeony root, 766.7 parts of salvia miltiorrhiza and auxiliary materials according to the weight parts.
The preparation method of the Jinma Gantai preparation comprises the following steps:
(1) pulverizing herba Eleocharitis Turerosa, extracting with ethanol under reflux, filtering, recovering ethanol from filtrate, and concentrating into soft extract;
(2) drying radix Stephaniae Tetrandrae, pulverizing into coarse powder, extracting with ethanol under reflux, recovering ethanol from the extractive solution until no ethanol smell exists, adding hydrochloric acid dropwise under stirring to adjust pH to 5, standing, filtering, adjusting pH to 9 with concentrated ammonia water, standing, vacuum filtering, drying the precipitate, dissolving with acetone under heating, adding distilled water into the solution until the solution is slightly turbid, recovering acetone, and concentrating into soft extract;
(3) pulverizing herba Epimedii, radix Berchemiae Lineatae and herba Verbenae, extracting with water, mixing decoctions, filtering, concentrating into soft extract, cooling, precipitating with ethanol, standing, recovering ethanol from the filtrate, and concentrating into soft extract.
(4) Pulverizing Saviae Miltiorrhizae radix, radix astragali, herba Patriniae, and radix Paeoniae Rubra, extracting with ethanol under reflux, filtering, recovering ethanol, and concentrating the filtrate into soft extract.
(5) And (4) combining the thick paste obtained in the step (3) and the step (4), centrifuging, and purifying by macroporous adsorption resin.
(6) Mixing the soft extracts of steps (1), (2) and (5), adding conventional adjuvants, and making into different oral preparations by conventional method.
Further, the extraction process of the dichondra repens in the step (1) comprises the following steps: crushing the creeping dichondra into coarse powder, performing reflux extraction for 3 times by using 90% ethanol in an amount which is 6 times that of the coarse powder, performing 1 hour each time, filtering, combining filtrates, recovering ethanol, and concentrating to obtain thick paste with the relative density of 1.34-1.40 at 50-60 ℃.
The extraction and purification process of the radix stephaniae tetrandrae in the step (2) comprises the following steps: drying radix stephaniae tetrandrae, crushing the dried radix stephaniae tetrandrae into coarse powder, extracting the coarse powder for 3 times by adopting 85% ethanol under reflux, combining extracting solutions, recovering ethanol until no alcohol smell exists, dropwise adding 1% hydrochloric acid under stirring to enable the pH value to be 5, standing for 48 hours, filtering, adjusting the pH value to be 9 by using concentrated ammonia water, standing for 48 hours, carrying out suction filtration, heating and dissolving the precipitate by using 2 times of acetone after drying, adding distilled water into the solution until the solution is slightly turbid, recovering the acetone, and concentrating the acetone to form thick paste with the relative density of 1.34-1.40 at 50-60 ℃.
The extraction and purification process of the epimedium, the berchemia lineata and the verbena in the step (3) comprises the following steps: taking dry medicinal materials of herba epimedii, berchemia lineata and verbena, crushing into coarse powder, decocting for 2 times with water for 2 hours each time, combining decoction, filtering, concentrating filtrate to thick paste with the relative density of 1.10-1.13, cooling, adding ethanol until the ethanol content reaches 75%, standing for 48 hours, filtering, recovering ethanol from filtrate, and concentrating to thick paste with the relative density of 1.18-1.20.
The extraction and purification process of the salvia miltiorrhiza, the astragalus, the patrinia and the red paeony root in the step (4) comprises the following steps: drying the red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, crushing, carrying out reflux extraction for 2h by using 80% ethanol in an amount which is 8-12 times that of the dried red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, combining extracting solutions, recovering the ethanol under reduced pressure (70 ℃, P ═ 0.08Mpa), and concentrating to obtain thick paste with the relative density of 1.18-1.20.
And (5) centrifuging at the rotating speed of 5000r/min for 20 min.
The purification of the step (5) is as follows: concentrating the extractive solution (concentration of 0.2 g/mL)-1) Passing through D101 macroporous resin (medicinal material: resin ratio 1:2, resin diameter/height ratio 1:8), and adsorbing at flow rate of 1 mL/min-1Washing with 5BV distilled water, eluting with 5BV 90%, 85%, 70%, 50% and 20% ethanol, collecting ethanol eluate, recovering ethanol, and drying.
Specifically, the preparation method of the Jinma Gantai preparation comprises the following steps:
(1) crushing the creeping dichondra into coarse powder, performing reflux extraction for 3 times by using 90% ethanol in an amount which is 6 times that of the coarse powder, performing 1 hour each time, filtering, combining filtrates, recovering ethanol, and concentrating to obtain thick paste with the relative density of 1.34-1.40 at 50-60 ℃ for later use;
(2) drying radix stephaniae tetrandrae, crushing the dried radix stephaniae tetrandrae into coarse powder, performing reflux extraction for 3 times by using 85% ethanol, each time for 1 hour, combining extracting solutions, recovering ethanol until no alcohol smell exists, dropwise adding 1% hydrochloric acid under stirring to enable the pH to be 5, standing for 48 hours, filtering, adjusting the pH to be 9 by using concentrated ammonia water, standing for 48 hours, performing suction filtration, heating and dissolving the precipitate by using 2 times of acetone after drying, adding distilled water into the solution until the solution is slightly turbid, recovering the acetone, and concentrating the acetone to a thick paste with the relative density of 1.34-1.40 at 50-60 ℃ for later use;
(3) taking dry medicinal materials of herba epimedii, berchemia lineata and verbena, crushing into coarse powder, decocting for 2 times with water for 2 hours each time, combining decoction, filtering, concentrating filtrate to thick paste with the relative density of 1.10-1.13, cooling, adding ethanol until the ethanol content reaches 75%, standing for 48 hours, filtering, recovering ethanol from filtrate, and concentrating to thick paste with the relative density of 1.18-1.20 for later use;
(4) drying the red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, crushing, performing reflux extraction for 2 hours by using 80% ethanol in an amount which is 10 times that of the dried red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, merging extracting solutions, recovering the ethanol under reduced pressure (70 ℃, P ═ 0.08Mpa), and concentrating the extracting solution to thick paste with the relative density of 1.18-1.20 for later use;
(5) mixing the soft extracts of step (3) and step (4), centrifuging at 5000r/min for 20min, collecting supernatant, adding water to desired volume to obtain a concentration of 0.2 g/mL-1Passing the centrifugate through D101 macroporous resin (medicinal material: resin ratio 1:2, resin diameter/height ratio 1:8), adsorbing at flow rate of 1 mL/min-1Washing with 5BV distilled water, eluting with 5BV 90%, 85%, 70%, 50% and 20% ethanol, collecting ethanol eluate, recovering ethanol, and drying;
(6) mixing the soft extracts of steps (1), (2) and (5), adding conventional adjuvants, and making into different oral preparations by conventional method.
The oral preparation is capsule, granule, tablet, dripping pill or soft capsule.
The capsules are prepared by:
(1) pulverizing herba Eleocharitis Turerosa, extracting with ethanol under reflux, filtering, recovering ethanol from filtrate, and concentrating into soft extract;
(2) drying radix Stephaniae Tetrandrae, pulverizing into coarse powder, extracting with ethanol under reflux, recovering ethanol from the extractive solution until no ethanol smell exists, adding hydrochloric acid dropwise under stirring to adjust pH to 5, standing, filtering, adjusting pH to 9 with concentrated ammonia water, standing, vacuum filtering, drying the precipitate, dissolving with acetone under heating, adding distilled water into the solution until the solution is slightly turbid, recovering acetone, and concentrating into soft extract;
(3) pulverizing herba Epimedii, radix Berchemiae Lineatae and herba Verbenae, extracting with water, mixing decoctions, filtering, concentrating into soft extract, cooling, precipitating with ethanol, standing, recovering ethanol from the filtrate, and concentrating into soft extract.
(4) Pulverizing Saviae Miltiorrhizae radix, radix astragali, herba Patriniae, and radix Paeoniae Rubra, extracting with ethanol under reflux, filtering, recovering ethanol, and concentrating the filtrate into soft extract.
(5) And (4) combining the thick paste obtained in the step (3) and the step (4), centrifuging, and purifying by macroporous adsorption resin.
(6) Mixing the soft extracts of steps (1), (2) and (5), drying at 60 deg.C, pulverizing, adding 0.5% magnesium stearate, mixing, and making into capsule.
The invention has the beneficial effects that:
(1) the invention makes clear the category and the property of the active ingredients according to the functional indication of the Jinma Gantai capsule, extracts the traditional Chinese medicine materials in a classified way, extracts the active substances of the traditional Chinese medicine to the maximum extent, and improves the curative effect of the Jinma Gantai preparation on treating acute and chronic hepatitis.
(2) The invention adopts a macroporous adsorption resin method to purify and refine the extract, the macroporous resin can enrich and separate medicines with different mother nucleus structures, and can be used for separating and purifying active ingredients in a single medicinal material or a compound preparation, and D101 macroporous resin with good adsorption and elution capacities on all active ingredients of the preparation is selected through experiments from various types of macroporous resin; the method determines parameters such as the concentration of liquid medicine, volume flow during column loading and elution, the type and dosage of eluent, the diameter-height ratio of a resin column and the like, and tests prove that the macroporous adsorption resin method can effectively remove plant components with stronger hydrophilicity such as saccharides, tannins and the like, retains effective components such as flavonoids, saponins and the like required by the preparation, has high purification yield, stable purification process and easy operation, and can be used for industrial production.
(3) The invention carries out special treatment on special active ingredients of special medicinal materials, carries out single extraction on the dichondra repens and the radix stephaniae tetrandrae, adopts an ethanol reflux method to extract alkaloid in the radix stephaniae tetrandrae, and utilizes an acid-base method and an organic solvent to remove ineffective impurities such as phenols, organic acids, saccharides and the like in the radix stephaniae tetrandrae extracting solution, thereby improving the content of active substances in the radix stephaniae tetrandrae;
(4) primarily purifying herba Epimedii, TIEBAOJIN and herba Verbenae by water extraction and ethanol precipitation, wherein the ethanol precipitation is carried out to reduce ethanol consumption and appropriately concentrate medicinal liquid; in order to avoid the loss of ethanol due to heat volatilization, the concentrated liquid medicine is cooled and then added with ethanol; in addition, the method adopts a slow-speed stirring mode during alcohol precipitation, namely, the liquid medicine is quickly stirred, and ethanol is slowly added, so that the loss of effective components caused by over-high concentration of local alcohol is avoided; most of the impurities with alcohol content of more than 75 percent can be removed by precipitation. Finally, the alcohol content of the invention reaches 75 percent, which can primarily remove most of starch, protein, polysaccharide and other substances and lay a foundation for the adsorption and elution of macroporous resin.
Detailed Description
The technical solution of the present invention is further defined below with reference to the specific embodiments, but the scope of the claims is not limited to the description.
EXAMPLE A preparation of Jinma Gantai Capsule
The formula is as follows: 960.7g of creeping dichondra, 511g of berchemia lineate, 383.3g of verbena, 638.7g of tetrandra root, 383.3g of patrinia, 511g of epimedium, 511g of astragalus root, 511g of red peony root and 766.7g of salvia miltiorrhiza
The process comprises the following steps:
(1) crushing the creeping dichondra into coarse powder, performing reflux extraction for 3 times by using 90% ethanol in an amount which is 6 times that of the coarse powder, performing 1 hour each time, filtering, combining filtrates, recovering ethanol, and concentrating to obtain thick paste with the relative density of 1.34-1.40 at 50-60 ℃ for later use;
(2) drying radix stephaniae tetrandrae, crushing the dried radix stephaniae tetrandrae into coarse powder, performing reflux extraction for 3 times by using 85% ethanol, each time for 1 hour, combining extracting solutions, recovering ethanol until no alcohol smell exists, dropwise adding 1% hydrochloric acid under stirring to enable the pH to be 5, standing for 48 hours, filtering, adjusting the pH to be 9 by using concentrated ammonia water, standing for 48 hours, performing suction filtration, heating and dissolving the precipitate by using 2 times of acetone after drying, adding distilled water into the solution until the solution is slightly turbid, recovering the acetone, and concentrating the acetone to a thick paste with the relative density of 1.34-1.40 at 50-60 ℃ for later use;
(3) taking dry medicinal materials of herba epimedii, berchemia lineata and verbena, crushing into coarse powder, decocting for 2 times with water for 2 hours each time, combining decoction, filtering, concentrating filtrate to thick paste with the relative density of 1.10-1.13, cooling, adding ethanol until the ethanol content reaches 75%, standing for 48 hours, filtering, recovering ethanol from filtrate, and concentrating to thick paste with the relative density of 1.18-1.20 for later use;
(4) drying the red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, crushing, performing reflux extraction for 2 hours by using 80% ethanol in an amount which is 10 times that of the dried red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, merging extracting solutions, recovering the ethanol under reduced pressure (70 ℃, P ═ 0.08Mpa), and concentrating the extracting solution to thick paste with the relative density of 1.18-1.20 for later use;
(5) mixing the soft extracts of step (3) and step (4), centrifuging at 5000r/min for 20min, collecting supernatant, adding water to desired volume to obtain a concentration of 0.2 g/mL-1Passing the centrifugate through D101 macroporous resin (medicinal material: resin ratio 1:2, resin diameter/height ratio 1:8), adsorbing at flow rate of 1 mL/min-1Washing with 5BV distilled water, eluting with 5BV 90%, 85%, 70%, 50% and 20% ethanol, collecting ethanol eluate, recovering ethanol, and drying;
(6) mixing the soft extracts of steps (1), (2) and (5), drying at 60 deg.C, pulverizing, adding starch and 0.5% magnesium stearate, mixing, and making into capsule (1000 granules).
Specification: 0.4 g/pellet.
The application and dosage are as follows: it is administered orally 2 granules at a time, 3 times daily.
Example preparation of Dijinma Gantai granules
The formula is as follows: 1000g of creeping dichondra, 600g of berchemia lineate, 450g of verbena, 700g of radix stephaniae tetrandrae, 450g of herba patriniae, 600g of herba epimedii, 600g of radix astragali, 600g of red paeony root and 800g of salvia miltiorrhiza
The process comprises the following steps:
(1) crushing the creeping dichondra into coarse powder, performing reflux extraction for 3 times by using 90% ethanol in an amount which is 6 times that of the coarse powder, performing 1 hour each time, filtering, combining filtrates, recovering ethanol, and concentrating to obtain thick paste with the relative density of 1.34-1.40 at 50-60 ℃ for later use;
(2) drying radix stephaniae tetrandrae, crushing the dried radix stephaniae tetrandrae into coarse powder, performing reflux extraction for 3 times by using 85% ethanol, each time for 1 hour, combining extracting solutions, recovering ethanol until no alcohol smell exists, dropwise adding 1% hydrochloric acid under stirring to enable the pH to be 5, standing for 48 hours, filtering, adjusting the pH to be 9 by using concentrated ammonia water, standing for 48 hours, performing suction filtration, heating and dissolving the precipitate by using 2 times of acetone after drying, adding distilled water into the solution until the solution is slightly turbid, recovering the acetone, and concentrating the acetone to a thick paste with the relative density of 1.34-1.40 at 50-60 ℃ for later use;
(3) taking dry medicinal materials of herba epimedii, berchemia lineata and verbena, crushing into coarse powder, decocting for 2 times with water for 2 hours each time, combining decoction, filtering, concentrating filtrate to thick paste with the relative density of 1.10-1.13, cooling, adding ethanol until the ethanol content reaches 75%, standing for 48 hours, filtering, recovering ethanol from filtrate, and concentrating to thick paste with the relative density of 1.18-1.20 for later use;
(4) drying the red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, crushing, performing reflux extraction for 2 hours by using 80% ethanol in an amount which is 10 times that of the dried red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, merging extracting solutions, recovering the ethanol under reduced pressure (70 ℃, P ═ 0.08Mpa), and concentrating the extracting solution to thick paste with the relative density of 1.18-1.20 for later use;
(5) mixing the soft extracts of step (3) and step (4), centrifuging at 5000r/min for 20min, collecting supernatant, adding water to desired volume to obtain a concentration of 0.2 g/mL-1Passing the centrifugate through D101 macroporous resin (medicinal material: resin ratio 1:2, resin diameter/height ratio 1:8), adsorbing at flow rate of 1 mL/min-1Washing with 5BV distilled water, eluting with 5BV 90%, 85%, 70%, 50% and 20% ethanol, collecting ethanol eluate, recovering ethanol, and drying;
(6) mixing the soft extracts of steps (1), (2) and (5), drying at 60 deg.C, pulverizing, adding starch, granulating, spraying 2% hydroxypropyl methylcellulose ethanol solution 80m1, granulating, mixing, and making into 500 bags.
Specification: 10 g/bag.
The application and dosage are as follows: it is administered orally 1 bag at a time, 3 times daily.
Example preparation of a SANJINMAGANTAI tablet
The formula is as follows: 900g of creeping dichondra, 450g of berchemia lineate, 300g of verbena, 600g of radix stephaniae tetrandrae, 300g of herba patriniae, 450g of herba epimedii, 450g of radix astragali, 450g of red paeony root and 700g of salvia miltiorrhiza
The process comprises the following steps:
(1) crushing the creeping dichondra into coarse powder, performing reflux extraction for 3 times by using 90% ethanol in an amount which is 6 times that of the coarse powder, performing 1 hour each time, filtering, combining filtrates, recovering ethanol, and concentrating to obtain thick paste with the relative density of 1.34-1.40 at 50-60 ℃ for later use;
(2) drying radix stephaniae tetrandrae, crushing the dried radix stephaniae tetrandrae into coarse powder, performing reflux extraction for 3 times by using 85% ethanol, each time for 1 hour, combining extracting solutions, recovering ethanol until no alcohol smell exists, dropwise adding 1% hydrochloric acid under stirring to enable the pH to be 5, standing for 48 hours, filtering, adjusting the pH to be 9 by using concentrated ammonia water, standing for 48 hours, performing suction filtration, heating and dissolving the precipitate by using 2 times of acetone after drying, adding distilled water into the solution until the solution is slightly turbid, recovering the acetone, and concentrating the acetone to a thick paste with the relative density of 1.34-1.40 at 50-60 ℃ for later use;
(3) taking dry medicinal materials of herba epimedii, berchemia lineata and verbena, crushing into coarse powder, decocting for 2 times with water for 2 hours each time, combining decoction, filtering, concentrating filtrate to thick paste with the relative density of 1.10-1.13, cooling, adding ethanol until the ethanol content reaches 75%, standing for 48 hours, filtering, recovering ethanol from filtrate, and concentrating to thick paste with the relative density of 1.18-1.20 for later use;
(4) drying the red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, crushing, performing reflux extraction for 2 hours by using 80% ethanol in an amount which is 10 times that of the dried red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, merging extracting solutions, recovering the ethanol under reduced pressure (70 ℃, P ═ 0.08Mpa), and concentrating the extracting solution to thick paste with the relative density of 1.18-1.20 for later use;
(5) mixing the soft extracts of step (3) and step (4), centrifuging at 5000r/min for 20min, collecting supernatant, adding water to desired volume to obtain a concentration of 0.2 g/mL-1Passing the centrifugate through D101 macroporous resin (medicinal material: resin ratio 1:2, resin diameter/height ratio 1:8), adsorbing at flow rate of 1 mL/min-1Washing with 5BV distilled water, eluting with 5BV 90%, 85%, 70%, 50% and 20% ethanol, collecting ethanol eluate, recovering ethanol, and drying;
(6) mixing the soft extracts of steps (1), (2) and (5), adding 32% starch and 1.3% microcrystalline cellulose, granulating, drying at 60 deg.C, adding 0.1% magnesium stearate, mixing, tabletting, and coating to obtain 1000 tablets.
Specification: 0.3 g/tablet.
The application and dosage are as follows: it is administered orally 2 tablets at a time, 3 times a day.
Example preparation of Sijinma Gantai dripping pills
The formula is as follows: 1000g of creeping dichondra, 450g of berchemia lineate, 450g of verbena, 600g of radix stephaniae tetrandrae, 450g of herba patriniae, 450g of herba epimedii, 600g of radix astragali, 450g of red paeony root and 800g of salvia miltiorrhiza
The process comprises the following steps:
(1) crushing the creeping dichondra into coarse powder, performing reflux extraction for 3 times by using 90% ethanol in an amount which is 6 times that of the coarse powder, performing 1 hour each time, filtering, combining filtrates, recovering ethanol, and concentrating to obtain thick paste with the relative density of 1.34-1.40 at 50-60 ℃ for later use;
(2) drying radix stephaniae tetrandrae, crushing the dried radix stephaniae tetrandrae into coarse powder, performing reflux extraction for 3 times by using 85% ethanol, each time for 1 hour, combining extracting solutions, recovering ethanol until no alcohol smell exists, dropwise adding 1% hydrochloric acid under stirring to enable the pH to be 5, standing for 48 hours, filtering, adjusting the pH to be 9 by using concentrated ammonia water, standing for 48 hours, performing suction filtration, heating and dissolving the precipitate by using 2 times of acetone after drying, adding distilled water into the solution until the solution is slightly turbid, recovering the acetone, and concentrating the acetone to a thick paste with the relative density of 1.34-1.40 at 50-60 ℃ for later use;
(3) taking dry medicinal materials of herba epimedii, berchemia lineata and verbena, crushing into coarse powder, decocting for 2 times with water for 2 hours each time, combining decoction, filtering, concentrating filtrate to thick paste with the relative density of 1.10-1.13, cooling, adding ethanol until the ethanol content reaches 75%, standing for 48 hours, filtering, recovering ethanol from filtrate, and concentrating to thick paste with the relative density of 1.18-1.20 for later use;
(4) drying the red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, crushing, performing reflux extraction for 2 hours by using 80% ethanol in an amount which is 10 times that of the dried red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, merging extracting solutions, recovering the ethanol under reduced pressure (70 ℃, P ═ 0.08Mpa), and concentrating the extracting solution to thick paste with the relative density of 1.18-1.20 for later use;
(5) mixing the soft extracts of step (3) and step (4), centrifuging at 5000r/min for 20min, collecting supernatant, adding water to desired volume to obtain a concentration of 0.2 g/mL-1Passing the centrifugate through D101 macroporous resin (medicinal material: resin ratio 1:2, resin diameter/height ratio 1:8), adsorbing at flow rate of 1 mL/min-1Washing with 5BV distilled water, eluting with 5BV 90%, 85%, 70%, 50%, 20% ethanol, collecting ethanol eluate, and recovering ethanolDrying for later use;
(6) mixing the soft extracts of steps (1), (2) and (5), adding into molten polyethylene glycol (polyethylene glycol 4000 and polyethylene glycol 6000) at a ratio of 3:2, mixing, and making into dripping pill 5000 pills.
Specification: 50 mg/pill.
The application and dosage are as follows: it is administered orally 6-10 granules at a time, 3 times daily.
Example preparation of Wu' e Mahan Gantai Soft Capsule
The formula is as follows: 900g of creeping dichondra, 600g of berchemia lineate, 300g of verbena, 700g of radix stephaniae tetrandrae, 300g of herba patriniae, 600g of herba epimedii, 450g of radix astragali, 600g of red paeony root and 700g of salvia miltiorrhiza
The process comprises the following steps:
(1) crushing the creeping dichondra into coarse powder, performing reflux extraction for 3 times by using 90% ethanol in an amount which is 6 times that of the coarse powder, performing 1 hour each time, filtering, combining filtrates, recovering ethanol, and concentrating to obtain thick paste with the relative density of 1.34-1.40 at 50-60 ℃ for later use;
(2) drying radix stephaniae tetrandrae, crushing the dried radix stephaniae tetrandrae into coarse powder, performing reflux extraction for 3 times by using 85% ethanol, each time for 1 hour, combining extracting solutions, recovering ethanol until no alcohol smell exists, dropwise adding 1% hydrochloric acid under stirring to enable the pH to be 5, standing for 48 hours, filtering, adjusting the pH to be 9 by using concentrated ammonia water, standing for 48 hours, performing suction filtration, heating and dissolving the precipitate by using 2 times of acetone after drying, adding distilled water into the solution until the solution is slightly turbid, recovering the acetone, and concentrating the acetone to a thick paste with the relative density of 1.34-1.40 at 50-60 ℃ for later use;
(3) taking dry medicinal materials of herba epimedii, berchemia lineata and verbena, crushing into coarse powder, decocting for 2 times with water for 2 hours each time, combining decoction, filtering, concentrating filtrate to thick paste with the relative density of 1.10-1.13, cooling, adding ethanol until the ethanol content reaches 75%, standing for 48 hours, filtering, recovering ethanol from filtrate, and concentrating to thick paste with the relative density of 1.18-1.20 for later use;
(4) drying the red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, crushing, performing reflux extraction for 2 hours by using 80% ethanol in an amount which is 10 times that of the dried red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, merging extracting solutions, recovering the ethanol under reduced pressure (70 ℃, P ═ 0.08Mpa), and concentrating the extracting solution to thick paste with the relative density of 1.18-1.20 for later use;
(5) mixing the soft extracts of step (3) and step (4), centrifuging at 5000r/min for 20min, collecting supernatant, adding water to desired volume to obtain a concentration of 0.2 g/mL-1Passing the centrifugate through D101 macroporous resin (medicinal material: resin ratio 1:2, resin diameter/height ratio 1:8), adsorbing at flow rate of 1 mL/min-1Washing with 5BV distilled water, eluting with 5BV 90%, 85%, 70%, 50% and 20% ethanol, collecting ethanol eluate, recovering ethanol, and drying;
(6) and (3) combining the thick paste obtained in the steps (1), (2) and (5) to obtain the soft capsule core material. Heating to prepare the gelatin capsule wall, and adhering the core material and the wall material by using a capsule machine to prepare 1000 soft capsules.
Specification: 0.5 g/pellet.
The application and dosage are as follows: it is administered orally 2 granules at a time, 3 times daily.
Drug Performance evaluation test
Next, the drugs prepared in the preparation examples 1 to 5, the method described in the drug standard (YBZ08762009), and the preparation method disclosed in chinese patent CN 102813752A were subjected to an action experiment in terms of anti-inflammatory, analgesic, and liver protection, and an evaluation experiment of acute toxicity and stability.
Experimental example 1 anti-inflammatory assay
1.1 test animals, materials and drugs
18-22 g of Kunming mice, which are used as both male and female and purchased from the experimental center of Guizhou medical university; JN-A type precision torsion balance (Shanghai second balance instrument factory), and xylene (Shanghai reagent first factory).
Comparative example 1: the preparation is prepared by the method described in the pharmaceutical standard (YBZ08762009) in the original process.
Comparative example 2: the formulation disclosed in chinese patent CN102813752 a was prepared as in example 1.
Test examples 1 to 5: the preparation prepared by the method of the invention in the embodiment 1-5.
1.2 test methods
Half 105 mice were divided randomly into 7 groups of 15 mice each, and the gavage was administered separately. ControlNS is given, and the original process extract group (8.2g kg)-1) The extract of the present invention (8.2 g/kg)-1) And (4) grouping. 1 time daily for 7 days; 1h after the last administration, the two sides of the auricle of each group of mice are uniformly coated with 0.05ml of dimethylbenzene each, the left ear is not coated on a normal ear, 1h after inflammation and swelling, the ear is removed from the neck and killed, the left ear and the right ear are immediately cut along the edge of the auricle, and the ears are weighed by a precision torsion balance. The net swelling was calculated by subtracting the weight of the left ear from the weight of the right ear, and the rate of inhibition of swelling was calculated. The inhibition ratio (%) was (mean swelling value of control group-mean swelling value of administration group)/mean swelling value of control group × 100%.
1.3 results of the experiment
TABLE 1 Effect of extracts of groups on ear swelling in mice
Compared with the preparations prepared by the control group 1 and the control group 2, the preparation prepared by the process of the invention has the advantages that P < 0.05 shows that: the invention can effectively inhibit mouse auricle inflammatory edema caused by xylene, and the inhibition effect is better than that of the preparation prepared by the prior art preparation and the Chinese patent CN 102813752A.
EXAMPLE 2 analgesic test
2.1 Experimental methods
135 healthy Kunming mice are taken, male and female are respectively divided into 9 groups at random, each group comprises 15 mice, namely a physiological saline group, examples 1-5 (preparations prepared according to examples 1-5 of the invention), a preparation prepared by the original process (a preparation prepared according to a drug standard (YBZ 08762009)), a preparation prepared by Chinese patent CN 102813752A and an aspirin group, each group is continuously administrated for 7 days for 1 time every day, the physiological saline group is administrated with an equal volume of physiological saline (20ml/Kg), the rest groups are respectively filled with the preparation of the invention, the preparation prepared by the original process and aspirin liquid (0.2g/Kg, 20ml/Kg) according to the dose of 0.4g/Kg (20ml/Kg), the doses are 30min after the last administration, 0.8% acetic acid solution is injected into the abdominal cavity of each mouse for 0.2 ml/mouse, the times of body twisting reaction of each mouse in 20min are observed and recorded, the average number and the standard difference are calculated, differences between groups were compared.
2.2 the results are shown in Table 2.
Table 2 effect on number of writhing in mice (n 15, x ± s)
Note: the comparison between the group of this example and the group of the original process is P < 0.05
The preparation prepared by the process of the invention is compared with the preparation prepared by the original process and Chinese patent CN 102813752A in the aspect of mouse analgesia, P is less than 0.05, the analgesic effect of the invention is better than that of the preparation prepared by the original process and Chinese patent CN 102813752A, and the extraction and purification of the effective substances of the invention are higher.
Experimental example 3 liver protection Experimental study
3.1 test animals and materials
135 Kunming mice, 18-22 g, are available for both male and female, and are purchased from the experimental center of Guizhou medical university. A JN-A type precision torsion balance (Shanghai second balance instrument factory) and carbon tetrachloride (Shanghai reagent first factory).
3.2 test methods
135 mice, each half of male and female, were randomly divided into 9 groups, each group was 15, and each group was a normal control group (distilled water, 20ml/kg), a model group (distilled water, 20ml/kg), examples 1 to 5 groups (0.4g/kg) of the present invention, an original technical preparation group (a preparation prepared according to drug standard (YBZ08762009) (0.4g/kg), a preparation prepared according to chinese patent CN 102813752A) (0.4g/kg), and were administered by gavage 1 time per day for 1 week; after the last administration for 1h, except for a normal control group, mice in each group were injected with 10ml/kg body weight of a 1% carbon tetrachloride peanut oil solution in the abdominal cavity. After 20h, blood was taken from the orbital venous plexus of the mice and serum was isolated. The activity of serum alanine Aminotransferase (ALT), aspartate Aminotransferase (AST), total serum protein (TP) and Albumin (ALB) are determined by using a clinical kit method. Comparing the significant difference between each group and the model group, and evaluating the liver-protecting and enzyme-reducing effects of the extract of the prescription.
3.3 results of the experiment
The results are shown in Table 3.
Table 3 protection of carbon tetrachloride-induced liver injury mice by different formulations of the compositions (n 15, x ± s)
The results in Table 3 show that compared with the control group, the ALT, AST and TP activities of the serum of the model group are obviously improved compared with the control group, which indicates that the model is successfully made (P < 0.01); the embodiment group can reduce the ALT, AST and TP content and increase the ALB content, compared with the preparation prepared by the original process and the Chinese patent CN 102813752A group (P < 0.05), the composition preparation can obviously reduce the ALT, AST and TP activity (P < 0.05 or P < 0.01) in the serum of a mouse with liver injury caused by carbon tetrachloride and can obviously increase the ALB albumin content (P < 0.05 or P < 0.01), and compared with the original process and the Chinese patent CN 102813752A process, the extraction and purification effect of the composition preparation is better.
Experimental example 4: toxicity test study of the pharmaceutical composition of the present invention
4.1 Experimental materials:
medicine preparation: a: the capsule prepared in example 1;
b: granules obtained in example 2;
c, the tablet prepared in the example 3;
d: the dripping pill prepared in example 4;
e: the soft capsule prepared in example 5;
animals: 100 Kunming mice, 20 + -2 g weight, male and female.
4.2 acute toxicity test:
100 healthy mice were divided into 5 groups of 20 mice each, each half of which was male and female. Before the test, the animals are fasted for 16 hours without limiting drinking water, and then each group of mice are respectively gavaged with 0.5ml/10g of the drug and an equivalent amount of physiological saline solution, and the administration dose is as follows: medicine A: 30.84mg active ingredient/kg; b: 32.18mg active ingredient/kg; c: 36.41mg active ingredient/kg; d: 26.41mg active ingredient/kg; e: 35.38mg active ingredient/kg; f: 24.63mg active ingredient/kg; g: 40.11mg active ingredient/kg. The mice were observed for 7 days, normal diet, drinking water, general conditions (body weight change, diet, fur, behavior, secretion, excretion, etc.) and intoxication and death.
4.3 conclusion: acute toxicity test shows that animals have normal activity after administration of each group of the medicine, none of the animals die in the observation period, diet and activity of each group are normal, fur is smooth, and abnormal secretion is not found in mouth, nose, eyes and the like; it is clear that the components using the monomers of the present invention are non-toxic.
Experimental example 5 stability examination of pharmaceutical preparation of the present invention
Accelerated stability testing: 10g of each of the samples prepared in examples 1, 2, 3, 4 and 5, numbered 1-5, were randomly selected, placed at a temperature of 40 ℃. + -. 2 ℃ and a relative humidity of 75%. + -. 5%, and sampled at the end of 1 month, 2 months, 3 months and 6 months during the test period for examination.
And inspecting the stability of the product by inspecting the properties, identification and paeoniflorin content of the product. The results are shown in Table 4.
TABLE 4 accelerated stability test results
Through the anti-inflammatory, analgesic and liver-protecting curative effect, acute toxicity and stability experiments, it can be seen that the tablets, capsules, dripping pills, granules and soft capsules prepared by the composition have better curative effect than the existing Jinma Gantai capsules and the preparation prepared by Chinese patent CN 102813752A, have low toxicity and good stability, and are a good choice for treating acute and chronic hepatitis caused by liver and gallbladder damp-heat, qi stagnation and blood stasis.
Claims (2)
1. The preparation method of the Jinma Gantai preparation is characterized by comprising the following steps: (1) crushing the creeping dichondra into coarse powder, performing reflux extraction for 3 times by using 90% ethanol in an amount which is 6 times that of the coarse powder, performing 1 hour each time, filtering, combining filtrates, recovering ethanol, and concentrating to obtain thick paste with the relative density of 1.34-1.40 at 50-60 ℃ for later use;
(2) drying radix stephaniae tetrandrae, crushing the dried radix stephaniae tetrandrae into coarse powder, performing reflux extraction for 3 times by using 85% ethanol, each time for 1 hour, combining extracting solutions, recovering ethanol until no alcohol smell exists, dropwise adding 1% hydrochloric acid under stirring to enable the pH to be 5, standing for 48 hours, filtering, adjusting the pH to be 9 by using concentrated ammonia water, standing for 48 hours, performing suction filtration, heating and dissolving the precipitate by using 2 times of acetone after drying, adding distilled water into the solution until the solution is slightly turbid, recovering the acetone, and concentrating the acetone to a thick paste with the relative density of 1.34-1.40 at 50-60 ℃ for later use;
(3) taking dry medicinal materials of herba epimedii, berchemia lineata and verbena, crushing into coarse powder, decocting for 2 times with water for 2 hours each time, combining decoction, filtering, concentrating filtrate to thick paste with the relative density of 1.10-1.13, cooling, adding ethanol until the ethanol content reaches 75%, standing for 48 hours, filtering, recovering ethanol from filtrate, and concentrating to thick paste with the relative density of 1.18-1.20 for later use;
(4) drying the red sage root, the astragalus, the dahurian patrinia herb and the red paeony root, crushing, performing reflux extraction for 2 hours by using 10 times of 80% ethanol, merging extracting solutions, recovering ethanol under reduced pressure at 70 ℃ and under the condition that P is-0.08 Mpa, and concentrating to obtain thick paste with the relative density of 1.18-1.20 for later use;
(5) mixing the soft extracts of step (3) and step (4), centrifuging at 5000r/min for 20min, collecting supernatant, adding water to desired volume to obtain a solution with concentration of 0.2g·mL-1And (3) passing the centrifugate through D101 macroporous resin, wherein the medicinal materials are as follows: the resin ratio is 1:2, the ratio of the diameter to the height of the resin is 1:8, the adsorption flow rate is 1 mL/min-1Washing with 5BV distilled water, eluting with 5BV 90%, 85%, 70%, 50% and 20% ethanol, collecting ethanol eluate, recovering ethanol, and drying;
(6) mixing the soft extracts of steps (1), (2) and (5), adding conventional adjuvants, and making into different oral preparations by conventional method;
the Jinma Gantai preparation is prepared from 900-1000 parts of creeping dichondra, 450-600 parts of berchemia lineate, 300-450 parts of verbena, 600-700 parts of tetrandra root, 300-450 parts of field pennycress, 450-600 parts of epimedium, 450-600 parts of astragalus, 450-600 parts of red peony root, 700-800 parts of salvia miltiorrhiza and auxiliary materials according to weight parts.
2. The preparation method of claim 1, wherein the oral preparation is capsule, granule, tablet, or dripping pill.
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