CN112972527A - Fengliaochangweikang tablet and its extraction process - Google Patents
Fengliaochangweikang tablet and its extraction process Download PDFInfo
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- daphniphyllum calycinum
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/70—Polygonaceae (Buckwheat family), e.g. spineflower or dock
- A61K36/704—Polygonum, e.g. knotweed
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2022—Organic macromolecular compounds
- A61K9/205—Polysaccharides, e.g. alginate, gums; Cyclodextrin
- A61K9/2059—Starch, including chemically or physically modified derivatives; Amylose; Amylopectin; Dextrin
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- A61P1/04—Drugs for disorders of the alimentary tract or the digestive system for ulcers, gastritis or reflux esophagitis, e.g. antacids, inhibitors of acid secretion, mucosal protectants
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A61K2236/50—Methods involving additional extraction steps
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Abstract
The invention relates to a daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablet and an extraction process thereof, and the tablet comprises the following steps: (1) soaking; (2) decocting; (3) concentrating to obtain paste; (4) precipitating with ethanol; (5) and (5) drying the extract. The alcohol precipitation process comprises the following steps: s1, carrying out primary alcohol precipitation; s2 secondary alcohol precipitation; s3 ultrasonic processing; s4 concentration and recovery of ethanol. The extraction process adds an alcohol precipitation procedure, can quickly remove impurities, reduce the loss of effective components and reduce the dosage, and the added alcohol precipitation process does not need to be cooled in advance, shortens the whole alcohol precipitation time, and reduces the probability that substances such as starch, protein and the like are rapidly precipitated to form a wrapping liquid when directly contacting a high-concentration ethanol solution. Furthermore, an ultrasonic treatment process is added in the precipitation process, and the formed wrapping liquid can be destroyed by utilizing the secondary effects of ultrasonic waves, such as mechanical vibration, diffusion, crushing and the like, so that the diffusion and release of the component to be extracted are accelerated to be fully mixed with the solvent, the whole alcohol precipitation time is greatly shortened, and the alcohol precipitation is more full.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicines, and particularly relates to a daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablet and an alcohol precipitation process thereof.
Background
Fengliaochangweikang is a classical Chinese medicinal compound for preventing and treating gastrointestinal diseases. Is prepared from two Chinese medicinal materials of daphniphyllum calycinum and red-knees herb according to the proportion of 2: 1. The Daphniphyllum calycinum (Daphniphyllum calycinum Benth.) also called as fructus Arctii Bell is a plant belonging to genus Photinia of family Photiniaceae (Daphniphylllaceae), and has high medicinal value, and fruits, branches and leaves thereof can be used as medicine. The composition has effects of promoting blood circulation, removing blood stasis, dispelling pathogenic wind, relieving pain, stopping dysentery, clearing heat, etc., and can be used for treating dysentery, rheumatalgia, common cold, fever, etc. Polygonum hydropiper L (also called Polygonum hydropiper L) is a plant of Polygonum of Polygonaceae (Polygonaceae). The whole herb can be used as a medicine and has the effects of stopping dysentery, promoting blood circulation by removing blood stasis, relieving itching, killing parasites and the like. It can be used for treating diarrhea, gastroenteritis, rheumatic arthralgia, and traumatic injury. Modern pharmacological research shows that the compound contains chemical components such as flavonoids, sesquiterpenes, alkaloids, organic acids and the like, has pharmacological effects in various aspects such as anti-inflammation, pain relieving, bacteriostasis, anti-ulcerative colitis, gastric mucosa protection and the like, and has good effects in treating diseases such as acute gastroenteritis, dyspepsia and stomachache by clinical application.
At present, the preparation of daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets mostly adopts a water extraction concentration method, as shown in figure 1, which is a flow chart of the preparation process of daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets in the prior art, and the preparation process comprises the following steps: (1) soaking, namely weighing the medicinal materials according to the formula amount, and adding water to soak for 45 minutes; (2) decocting, namely adding water in an amount (w/w) which is 6-10 times of the weight of the medicinal materials, extracting liquid medicine after decocting, repeating the operation for 1-3 times, and then combining extracting solutions; (3) concentrating to obtain extract, mixing the extractive solutions, filtering, and concentrating under reduced pressure to obtain soft extract; (4) drying the extract, controlling the temperature to be 60-80 ℃, drying the extract of the thick paste, and finally crushing to obtain dry paste powder; (5) making into tablet, adding carboxymethyl starch sodium and magnesium stearate into the dry extract powder, mixing and tabletting, and coating with sugar coating or film coating to obtain final product. The method has simple operation steps and relatively low equipment cost.
However, the aqueous concentration method has many disadvantages: (1) the loss of active ingredients, especially water-insoluble ingredients, is high by the decocting method; (2) the organic solvent possibly reacts with the effective components in the extraction process to cause the effective components to lose the original effectiveness; (3) the non-effective components can not be removed to the maximum extent, and the concentration rate is not high enough; (4) the extracting solution is often rich in impurities except for the active ingredients, and a small amount of fat-soluble ingredients are still contained, which brings disadvantages to the refining; (5) high temperature operation can cause substantial decomposition of heat sensitive active ingredients; (6) the prepared extract has more impurities, so that more tablets need to be taken by a patient every day in daily treatment, and the whole drug effect can be influenced by excessive impurities.
Disclosure of Invention
Based on the above, the invention aims to overcome the defects in the prior art, and provides an extraction process of daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets, so as to solve the problems of more impurities in an extracting solution and more loss of active ingredients in the extraction process of daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets in the prior art.
The technical scheme for solving the technical problems is as follows, the extraction process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets comprises the working procedures of soaking, decocting, concentrating and preparing paste and drying extract, and also comprises the working procedure of alcohol precipitation after the working procedure of concentrating and preparing paste and before the working procedure of drying extract, and the steps are as follows:
step S1: performing primary alcohol precipitation, namely adding 30-50% by volume of ethanol aqueous solution into clear paste of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets with the relative density of 1.25-1.30 after the concentration paste preparation process, and stirring while adding, wherein the volume ratio of the clear paste to the ethanol aqueous solution is 1: 1-1: 2;
step S2: performing secondary alcohol precipitation, namely adding an ethanol water solution with the volume fraction of 95% into the clear paste stirred in the step S1, stirring while adding until the alcohol content of the clear paste is 50% -70%;
step S3: and (4) ultrasonic treatment, namely ultrasonic treatment is carried out on the clear paste with the alcohol content of 50-70% in the step S2 for 30-50 minutes, and then cooling and standing are carried out.
Compared with the prior art, the daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets achieve the purposes of removing impurities, reducing the loss of active ingredients and reducing the dosage by adding an alcohol precipitation process, the alcohol precipitation process directly and uniformly disperses a low-concentration ethanol solution into the clear paste, and then a high-concentration ethanol solution is added to uniformly distribute the alcohol content in the clear paste, the process does not need to be cooled in advance, the overall alcohol precipitation time is shortened, and the process reduces the probability that starch, protein and other substances are rapidly precipitated to form a wrapping liquid by directly contacting the high-concentration ethanol solution. Furthermore, an ultrasonic treatment process is added in the precipitation process, the extraction of the effective components of the traditional Chinese medicine is accelerated by utilizing the cavitation of ultrasonic waves, the formed wrapping liquid can be destroyed by the secondary effects of ultrasonic waves, such as mechanical vibration, diffusion, crushing and the like, the diffusion and release of the components to be extracted are accelerated to be fully mixed with the solvent, and the process greatly shortens the whole alcohol precipitation time and ensures that the alcohol precipitation is more full. The extraction process flow of the daphniphyllum calycinum and polygonum flaccidum tablets for treating gastrointestinal diseases is simple, stable, sufficient in alcohol precipitation, short in extraction time and high in yield, can meet the requirements of large-scale industrial production, and has wide application prospects and markets.
Further, the ultrasonic temperature of the ultrasonic treatment in the step S3 is 40-45 ℃. Is beneficial to the dissolution of the wrapping liquid and the leaching and extraction of the active ingredients of the traditional Chinese medicine.
Further, the volume ratio of the clear paste to the ethanol water solution in the step S1 is 1: 1.5. The probability of forming the wrapping liquid is reduced.
Further, the alcohol content of the clear paste in the step S2 is 65%. When the alcohol content is 65%, almost all starch, polysaccharide and protein impurities can be removed.
Further, the cooling and standing time of the step S3 is 6 hours. At this point the precipitation was complete.
Further, the alcohol precipitation process further includes a step S4, in which the step S4 is to extract a supernatant after standing, concentrate the supernatant, and recover ethanol. The ethanol is easy to volatilize, and can be recycled, so that the waste of raw materials is reduced.
Further, the preparation process of the clear paste of the daphniphyllum calycinum and polygonum hydropiper tablets comprises the steps of weighing daphniphyllum calycinum and polygonum hydropiper in a mass ratio of 2:1, adding 6-10 times (w/w) of water into the daphniphyllum calycinum and polygonum hydropiper by taking the total weight of the daphniphyllum calycinum and the polygonum hydropiper as a reference, decocting for 1-3 hours, extracting an extracting solution, repeating the decocting and extracting operation for 1-3 times, combining the extracting solutions, and concentrating to obtain the clear paste.
Further, the preparation process of the clear paste of the daphniphyllum calycinum and polygonum hydropiper tablets comprises the steps of weighing daphniphyllum calycinum and polygonum hydropiper in a mass ratio of 2:1, adding 8 times (w/w) of water into the daphniphyllum calycinum and polygonum hydropiper by taking the total weight of the daphniphyllum calycinum and the polygonum hydropiper as a reference, decocting for 2 times, combining extracting solutions, and concentrating to obtain the clear paste.
The invention also provides a daphniphyllum calycinum and polygonum orientale gastrointestinal health tablet which is prepared according to the extraction process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablet.
Compared with the prior art, the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets prepared by the extraction process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets have the advantages of good treatment effect, good quality and high safety.
Drawings
Fig. 1 is a flow chart of a preparation process of daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets in the prior art.
Fig. 2 is a flow chart of the extraction process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets.
Fig. 3 is a flow chart of an alcohol precipitation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets.
Detailed Description
The daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets and the extraction process thereof are further explained by the following specific examples.
Example 1
As shown in fig. 2, fig. 2 is a flow chart of the extraction process of daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets, and the extraction process comprises the following steps:
(1) soaking: sequentially putting the selected daphniphyllum calycinum and polygonum hydropiper in an extraction tank according to the mass ratio of 2:1, adding 8 times (w/w) of water, and soaking for 45 minutes;
(2) decocting: comprises primary decoction and secondary decoction
Primary decoction: and (3) decocting the soaked medicinal materials for one time, raising the temperature to 100 ℃, quickly closing a steam valve, then opening a jacket steam valve of the extraction tank, heating the liquid medicine in the extraction tank through the jacket, keeping the liquid medicine in the extraction tank in a slightly boiling state, and decocting for 2 hours to obtain a primary decoction. Opening the liquid outlet valve of the extraction tank to extract the liquid medicine, and closing the liquid outlet valve of the extraction tank after the primary decoction enters the liquid storage tank.
And (3) secondary decoction: continuously adding 8 times (w/w) of water into the extraction tank for secondary decoction, quickly closing a steam valve when the temperature is raised to 100 ℃, then opening a jacket steam valve of the extraction tank, heating the liquid medicine in the extraction tank through the jacket to ensure that the liquid medicine in the extraction tank is in a slightly boiling state, and decocting for 2 hours to obtain secondary decoction. Opening the liquid outlet valve of the extraction tank to extract the secondary decoction, allowing the secondary decoction to enter the liquid storage tank to be mixed with the primary decoction to obtain mixed liquid medicine, and closing the liquid outlet valve of the extraction tank after the mixed liquid medicine is completely extracted.
(3) Concentrating the liquid medicine: opening a liquid inlet valve, conveying the mixed liquid medicine from a liquid storage tank to a double-effect concentrator through a liquid medicine pump, wherein the effective vacuum degree is-0.02 MPa to-0.08 MPa, the temperature is less than or equal to 95 ℃, the double-effect vacuum degree is-0.02 MPa to-0.08 MPa, the temperature is less than or equal to 75 ℃, the air pressure is controlled to be less than 0.3MPa, and the concentration is stopped when the concentration of the liquid medicine is concentrated to the density of 1.10(80 ℃) to obtain clear paste.
(4) Alcohol precipitation, please refer to fig. 3, which is a flow chart of the alcohol precipitation process of the daphniphyllum calycinum and polygonum hydropiper tablets for gastrointestinal health of the present invention, comprising the following steps:
step S1: carrying out primary alcohol precipitation, conveying the concentrated clear paste with the relative density of 1.10 into an alcohol precipitation tank through a pipeline, confirming the volume of the clear paste through a sight glass and scale marks, adding 30% ethanol according to the volume fraction of 1.5:1, stirring while adding, and controlling the stirring time to be 10-30 minutes;
step S2: performing secondary alcohol precipitation, namely adding 95% by volume of ethanol into the ethanol-containing fluid extract stirred in the step S1 while stirring, stopping adding the ethanol when the ethanol content of the fluid extract is 70%, and continuing stirring for 10-30 minutes;
step S3: ultrasonic processing, ultrasonic processing the clear paste with 70% alcohol content in step S2 for 45 minutes, cooling and standing.
Step S4: concentrating and recovering ethanol, extracting supernatant liquid after standing in the step S3, conveying the supernatant liquid to a concentrator through a pipeline, recovering ethanol and concentrating.
(5) Drying the extract: delivering the concentrated solution after alcohol precipitation to an extract collecting tank in a clean area through a pipeline, continuing to carry out reduced pressure concentration until the relative density of the extract is 1.25(80 ℃), thus obtaining thick paste, then opening a discharge valve, introducing the thick paste into a container for reduced pressure drying, and obtaining the daphniphyllum calycinum gastrointestinal health dry extract powder.
Example 2
The preparation process of the clear paste of daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1, and is not described herein again. The alcohol precipitation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablet of the embodiment is different from the alcohol precipitation process of the embodiment 1 as follows:
step S1: carrying out primary alcohol precipitation, conveying the concentrated clear paste with the relative density of 1.10 into an alcohol precipitation tank through a pipeline, confirming the volume of the clear paste through a sight glass and scale marks, adding 35% ethanol, stirring while adding the ethanol, wherein the volume ratio of the ethanol to the clear paste is 1.5:1, and stirring for 10-30 minutes;
step S2: performing secondary alcohol precipitation, continuously adding 95% ethanol while stirring, and continuously stirring for 10-30 minutes when the alcohol content of the clear paste is 50%;
step S3: and (4) ultrasonic treatment, namely performing ultrasonic treatment on the stirred paste for 45 minutes, and then cooling and standing.
Example 3
The preparation process of the clear paste of daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1, and is not described herein again. The alcohol precipitation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablet of the embodiment is different from the alcohol precipitation process of the embodiment 1 as follows:
step S1: carrying out primary alcohol precipitation, conveying the concentrated clear paste with the relative density of 1.1 into an alcohol precipitation tank through a pipeline, confirming the volume of the clear paste through a sight glass and scale marks, adding 40% ethanol, stirring while adding the ethanol, wherein the volume ratio of the ethanol to the clear paste is 1:1, and stirring for 10-30 minutes;
step S2: performing secondary alcohol precipitation, continuously adding 95% ethanol while stirring, and continuously stirring for 10-30 minutes when the alcohol content of the clear paste is 55%;
step S3: and (4) ultrasonic treatment, namely performing ultrasonic treatment on the stirred paste for 45 minutes, and then cooling and standing.
Example 4
The preparation process of the clear paste of daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1, and is not described herein again. The alcohol precipitation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablet of the embodiment is different from the alcohol precipitation process of the embodiment 1 as follows:
step S1: carrying out primary alcohol precipitation, conveying the concentrated clear paste with the relative density of 1.1 into an alcohol precipitation tank through a pipeline, confirming the volume of the clear paste through a sight glass and scale marks, adding 40% ethanol, stirring while adding the ethanol, wherein the volume ratio of the ethanol to the clear paste is 1: 1-1.5: 1, and stirring for 10-30 minutes;
step S2: performing secondary alcohol precipitation, continuously adding 95% ethanol while stirring, and continuously stirring for 10-30 minutes when the alcohol content of the clear paste is 70%;
step S3: and (4) ultrasonic treatment, namely performing ultrasonic treatment on the stirred paste for 45 minutes, and then cooling and standing.
Example 5
The preparation process of the clear paste of daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1, and is not described herein again. The alcohol precipitation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablet of the embodiment is different from the alcohol precipitation process of the embodiment 1 as follows:
step S1: carrying out primary alcohol precipitation, conveying the concentrated clear paste with the relative density of 1.1 into an alcohol precipitation tank through a pipeline, confirming the volume of the clear paste through a sight glass and scale marks, adding 45% ethanol, stirring while adding the ethanol, wherein the volume ratio of the ethanol to the clear paste is 1:1, and stirring for 10-30 minutes;
step S2: performing secondary alcohol precipitation, continuously adding 95% ethanol while stirring, and continuously stirring for 10-30 minutes when the alcohol content of the clear paste is 50%;
step S3: and (4) ultrasonic treatment, namely performing ultrasonic treatment on the stirred paste for 45 minutes, and then cooling and standing.
Example 6
The preparation process of the clear paste of daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1, and is not described herein again. The alcohol precipitation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablet of the embodiment is different from the alcohol precipitation process of the embodiment 1 as follows:
step S1: carrying out primary alcohol precipitation, conveying the concentrated clear paste with the relative density of 1.1 into an alcohol precipitation tank through a pipeline, confirming the volume of the clear paste through a sight glass and scale marks, adding 45% ethanol, stirring while adding the ethanol, wherein the volume ratio of the ethanol to the clear paste is 1:1, and stirring for 10-30 minutes;
step S2: performing secondary alcohol precipitation, continuously adding 95% ethanol while stirring, and continuously stirring for 10-30 minutes when the alcohol content of the clear paste is 65%;
step S3: and (4) ultrasonic treatment, namely performing ultrasonic treatment on the stirred paste for 45 minutes, and then cooling and standing.
Example 7
The preparation process of the clear paste of daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1, and is not described herein again. The alcohol precipitation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablet of the embodiment is different from the alcohol precipitation process of the embodiment 1 as follows:
step S1: carrying out primary alcohol precipitation, conveying the concentrated clear paste with the relative density of 1.1 into an alcohol precipitation tank through a pipeline, confirming the volume of the clear paste through a sight glass and scale marks, adding 45% ethanol, stirring while adding the ethanol, wherein the volume ratio of the ethanol to the clear paste is 1:1, and stirring for 10-30 minutes;
step S2: performing secondary alcohol precipitation, continuously adding 95% ethanol while stirring, and continuously stirring for 10-30 minutes when the alcohol content of the clear paste is 70%;
step S3: and (4) ultrasonic treatment, namely performing ultrasonic treatment on the stirred paste for 45 minutes, and then cooling and standing.
Example 8
The preparation process of the clear paste of daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1, and is not described herein again. The alcohol precipitation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablet of the embodiment is different from the alcohol precipitation process of the embodiment 1 as follows:
step S1: carrying out primary alcohol precipitation, conveying the concentrated clear paste with the relative density of 1.1 into an alcohol precipitation tank through a pipeline, confirming the volume of the clear paste through a sight glass and scale marks, adding 50% ethanol, stirring while adding the ethanol, wherein the volume ratio of the ethanol to the clear paste is 1:1, and stirring for 10-30 minutes;
step S2: performing secondary alcohol precipitation, continuously adding 95% ethanol while stirring, and continuously stirring for 10-30 minutes when the alcohol content of the clear paste is 70%;
step S3: and (4) ultrasonic treatment, namely performing ultrasonic treatment on the stirred paste for 45 minutes, and then cooling and standing.
Example 9
The preparation process of the clear paste of daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1, and is not described herein again. The alcohol precipitation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablet of the embodiment is different from the alcohol precipitation process of the embodiment 1 as follows:
step S1: carrying out primary alcohol precipitation, conveying the concentrated clear paste with the relative density of 1.1 into an alcohol precipitation tank through a pipeline, confirming the volume of the clear paste through a sight glass and scale marks, adding 50% ethanol, stirring while adding the ethanol, wherein the volume ratio of the ethanol to the clear paste is 1:1, and stirring for 10-30 minutes;
step S2: performing secondary alcohol precipitation, continuously adding 95% ethanol while stirring, and continuously stirring for 10-30 minutes when the alcohol content of the clear paste is 50%;
step S3: and (4) ultrasonic treatment, namely performing ultrasonic treatment on the stirred paste for 45 minutes, and then cooling and standing.
Comparative example 1
The preparation process of the clear paste of daphniphyllum calycinum and polygonum flaccidum tablets for intestines and stomach in the comparative example 1 has no alcohol precipitation process, and other steps are completely the same as those in the example 1 and are not repeated.
Comparative example 2
The preparation process of the clear paste of daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1, and is not described herein again. The alcohol precipitation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablet of the embodiment is different from the alcohol precipitation process of the embodiment 1 as follows:
step S1: conveying the concentrated clear paste with the relative density of 1.1 into an alcohol precipitation tank through a pipeline, confirming the volume of the clear paste through a sight glass and scale marks, adding 95% of ethanol while stirring, stopping adding the alcohol when the alcohol content of the clear paste is 65%, and continuing stirring for 10-30 minutes;
step S2: and cooling the stirred paste to room temperature and then standing.
Test examples, comparative experiment of Total Flavonoids content
This test example verifies that the preparation method of daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets provided by the present invention has a high extraction rate by measuring and calculating the total flavone content in example 1, example 2, example 3, example 4, example 5, example 6, example 7, example 8, example 9, comparative example 1 and comparative example 2.
In this test example, the materials used were: rutin reference substance (purity is more than or equal to 95%, Chinese medicine biological product identification institute). The used instruments are: UV759 ultraviolet-visible spectrophotometer (shanghaiengaceae); CP214 electronic analytical balance (aohaus instruments shanghai ltd).
Firstly, accurately weighing dried rutin control substance with constant weight of 5mg, dissolving with 60% ethanol, fixing the volume to a 25ml capacity bottle, and shaking up to obtain rutin control substance solution with concentration of 0.2 mg/ml. Precisely sucking 1ml, 2ml, 3ml, 4ml and 5ml of rutin reference substance solution, respectively placing in a 25ml volumetric flask, adding 1ml of 5% sodium nitrite, shaking up, placing for 7 minutes, adding 1ml of 10% aluminum nitrate, shaking up, continuing to place for 7 minutes, adding 10.0ml of 4% sodium hydroxide solution, fixing the volume to the scale with 60% ethanol, shaking up, and placing for 10 minutes. And (3) determining the absorbance (A) at 510nm by using an ultraviolet spectrophotometer with the corresponding reagent as a blank, and drawing a standard curve with the absorbance (A) as a vertical coordinate and the concentration (mg/ml) of the rutin control solution as a horizontal coordinate. The results are shown in Table 1.
TABLE 1 preparation of standard curves for rutin control solutions
The result shows that the rutin concentration is between 0.008mg/ml and 0.040mg/ml, the linearity is good, wherein X is the concentration (mg/ml) of the rutin control substance, and Y is the absorbance.
Then, 5ml of the supernatant obtained in the alcohol precipitation process of the daphniphyllum calycinum tablets of example 1, example 2, example 3, example 4, example 5, example 6, example 7, example 8, example 9, comparative example 1 and comparative example 2 of the present invention was precisely sucked, evaporated to dryness in an evaporation dish, dissolved in 60% ethanol, fully transferred to a 25ml volumetric flask, and the volume was fixed to the scale with 60% ethanol, 5ml of the supernatant was accurately measured from the volumetric flask and placed in the 25ml volumetric flask, 1ml of 5% sodium nitrite was added, shaking was carried out, after 7 minutes of standing, 1ml of 10% aluminum nitrate was added, shaking was carried out, standing was continued for 7 minutes, 10.0ml of 4% sodium hydroxide solution was added, the volume was fixed to the scale with 60% ethanol, shaking was carried out, and then standing was carried out for 10 minutes. Measuring absorbance (A) at 510nm with ultraviolet spectrophotometer, and calculating total flavone extraction rate according to standard curve and the following formula.
Total flavone extraction (mg/g) ═ CxV/W
Wherein C is the concentration (mg/ml) of flavone in supernatant liquid prepared in the alcohol precipitation process per ml calculated according to a standard curve equation; v is the total volume (ml) of supernatant liquid prepared in the alcohol precipitation process; w is the total mass (g) of daphniphyllum calycinum and polygonum hydropiper.
The results are given in table 2 below:
TABLE 2 flavone extraction amounts of the examples in the specific examples
In the experiment of measuring the extraction amount of the total flavone by using a spectrophotometer method, the following results are obtained: the concentration of rutin in the range of 0.008-0.048 mg/ml and the absorbance have a good linear relation, experiments show that the embodiment 6 is the best embodiment, firstly 45% of ethanol is added for carrying out primary alcohol precipitation treatment, then 95% of ethanol is added to enable the alcohol content to reach 65%, finally ultrasonic treatment is added in the standing process, the extraction amount of total flavonoids is the highest and can be 42.83mg/g, therefore, the effective components can be extracted and used to the maximum extent, and the prepared daphniphyllum calycinum and polygonum tablets for intestines and stomach have a good effect.
Compared with the prior art, the daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets achieve the purposes of removing impurities, reducing the loss of active ingredients and reducing the dosage by adding an alcohol precipitation process, the alcohol precipitation process directly and uniformly disperses a low-concentration ethanol solution into the clear paste, and then a high-concentration ethanol solution is added to uniformly distribute the alcohol content in the clear paste, the process does not need to be cooled in advance, the overall alcohol precipitation time is shortened, and the process reduces the probability that starch, protein and other substances are rapidly precipitated to form a wrapping liquid by directly contacting the high-concentration ethanol solution. Furthermore, an ultrasonic treatment process is added in the precipitation process, the extraction of the effective components of the traditional Chinese medicine is accelerated by utilizing the cavitation of ultrasonic waves, the formed wrapping liquid can be destroyed by the secondary effects of ultrasonic waves, such as mechanical vibration, diffusion, crushing and the like, the diffusion and release of the components to be extracted are accelerated to be fully mixed with the solvent, and the process greatly shortens the whole alcohol precipitation time and ensures that the alcohol precipitation is more full. The extraction process flow of the daphniphyllum calycinum and polygonum flaccidum tablets for treating gastrointestinal diseases is simple, stable, sufficient in alcohol precipitation, short in extraction time and high in yield, can meet the requirements of large-scale industrial production, and has wide application prospects and markets. The daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets prepared by the alcohol precipitation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets have the advantages of good treatment effect, good quality and high safety.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (9)
1. An extraction process of daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets comprises the working procedures of soaking, decocting, concentrating and preparing paste and drying extract, and is characterized by further comprising the working procedure of alcohol precipitation after the working procedure of concentrating and preparing paste and before the working procedure of drying extract, and the steps are as follows:
step S1: performing primary alcohol precipitation, namely adding 30-50% by volume of ethanol aqueous solution into clear paste of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets with the relative density of 1.25-1.30 after the concentration paste preparation process, and stirring while adding, wherein the volume ratio of the clear paste to the ethanol aqueous solution is 1: 1-1: 2;
step S2: performing secondary alcohol precipitation, namely adding an ethanol water solution with the volume fraction of 95% into the clear paste stirred in the step S1, stirring while adding until the alcohol content of the clear paste is 50% -70%;
step S3: and (4) ultrasonic treatment, namely ultrasonic treatment is carried out on the clear paste with the alcohol content of 50-70% in the step S2 for 30-50 minutes, and then cooling and standing are carried out.
2. The extraction process of the daphniphyllum calycinum and polygonum orientale gastrointestinal rehabilitation tablet as claimed in claim 1, is characterized in that: the ultrasonic temperature of the ultrasonic treatment in the step S3 is 40-45 ℃.
3. The extraction process of the daphniphyllum calycinum and polygonum orientale gastrointestinal rehabilitation tablet as claimed in claim 2, is characterized in that: the volume ratio of the clear paste to the ethanol water solution in the step S1 is 1: 1.5.
4. The extraction process of the daphniphyllum calycinum and polygonum orientale gastrointestinal rehabilitation tablet as claimed in claim 3, is characterized in that: the alcohol content of the clear paste in the step S2 is 65 percent.
5. The extraction process of the daphniphyllum calycinum and polygonum orientale gastrointestinal rehabilitation tablet as claimed in claim 4, is characterized in that: the cooling and standing time after the step S3 is 6 hours.
6. The extraction process of the daphniphyllum calycinum and polygonum orientale gastrointestinal rehabilitation tablet as claimed in claim 5, is characterized in that: the alcohol precipitation process further comprises a step S4, wherein the step S4 is to extract the supernatant after standing, concentrate the supernatant and recover the ethanol.
7. The extraction process of the daphniphyllum calycinum and polygonum orientale gastrointestinal rehabilitation tablet as claimed in any one of claims 1 to 6, is characterized in that: the preparation process of the clear paste of the daphniphyllum calycinum and polygonum hydropiper tablets comprises the steps of weighing daphniphyllum calycinum and polygonum hydropiper in a mass ratio of 2:1, adding 6-10 times (w/w) of water into the daphniphyllum calycinum and polygonum hydropiper by taking the total weight of the daphniphyllum calycinum and the polygonum hydropiper as a reference, decocting for 1-3 hours, extracting, repeating the decoction and extraction for 1-3 times, combining the extracting solutions, and concentrating to obtain the clear paste.
8. The extraction process of the daphniphyllum calycinum and polygonum orientale gastrointestinal rehabilitation tablet as claimed in claim 7, is characterized in that: the preparation process of the clear paste of the daphniphyllum calycinum and polygonum hydropiper tablets comprises the steps of weighing daphniphyllum calycinum and polygonum hydropiper in a mass ratio of 2:1, adding 8 times (w/w) of water into the daphniphyllum calycinum and polygonum hydropiper by taking the total weight of the daphniphyllum calycinum and the polygonum hydropiper as a reference, decocting for 2 hours, repeatedly decocting and extracting for 2 times, combining extracting solutions, and concentrating to obtain the clear paste.
9. The daphniphyllum calycinum and polygonum orientale gastrointestinal health tablet is prepared according to the extraction process of any one of claims 1 to 8.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115192637A (en) * | 2022-08-10 | 2022-10-18 | 特一药业集团股份有限公司 | Daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet and preparation process thereof |
| CN116688049A (en) * | 2023-06-20 | 2023-09-05 | 江西品信药业股份有限公司 | Child intestine and stomach recovery granule and preparation process thereof |
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2019
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115192637A (en) * | 2022-08-10 | 2022-10-18 | 特一药业集团股份有限公司 | Daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet and preparation process thereof |
| WO2024031830A1 (en) * | 2022-08-10 | 2024-02-15 | 特一药业集团股份有限公司 | Feng liao chang wei kang tablet and preparation technology therefor |
| CN116688049A (en) * | 2023-06-20 | 2023-09-05 | 江西品信药业股份有限公司 | Child intestine and stomach recovery granule and preparation process thereof |
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