CN115192637A - Daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet and preparation process thereof - Google Patents
Daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet and preparation process thereof Download PDFInfo
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Abstract
The invention relates to a preparation process of daphniphyllum calycinum and polygonum flaccidum tablets for intestines and stomach, which comprises the steps of soaking, decocting, concentrating and preparing paste, alcohol precipitating, drying the extract, preparing the tablet and the like. Wherein, the decocting process comprises the following steps: s1, decocting for the first time; s2, carrying out first enzymolysis; s3, decocting for the second time; and S4, carrying out second enzymolysis. According to the process, two times of enzymolysis are set in the decocting process, wherein the first enzymolysis reaction is carried out between the first decocting and the second decocting, the first decocting can be utilized to firstly hydrolyze part of cellulose of plant cells, the compactness of cell walls of the plant cells is reduced, the enzymolysis reaction is utilized to further destroy the cell walls, and the extraction rate of the subsequent second decocting is greatly improved. And the liquid medicine obtained after the two times of decoction is subjected to the second enzymolysis, so that the viscosity of the liquid medicine is favorably reduced, and the phenomenon that the liquid medicine is wrapped by sediment during the subsequent alcohol precipitation is prevented. In addition, the purposes of removing impurities, reducing the loss of effective components and reducing the dosage are further achieved by adding an alcohol precipitation process.
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 a preparation process thereof.
Background
Fengliaochangweikang is a classical Chinese medicine compound for preventing and treating gastrointestinal diseases, and is prepared from two Chinese medicinal materials of Daphniphyllum calycinum and Polygonum hydropiper in a ratio of 2: 1. The daphniphyllum calycinum is a plant belonging to genus Photinia of family Photiniaceae, and has high medicinal value, and can be used as medicine for fruits, branches and leaves. 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. Herba Polygoni Hydropiperis is also called Polygonum hydropiper, and is a plant of Polygonum of 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 flavonoid, sesquiterpene, alkaloid, organic acid and the like, has pharmacological effects in multiple aspects such as anti-inflammation, analgesia, bacteriostasis, anti-ulcerative colitis, gastric mucosa protection and the like, and has good effect in treating diseases such as acute gastroenteritis, dyspepsia and stomachache.
The preparation of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets in the prior art mostly adopts a water extraction concentration method, as shown in figure 1, which is a flow chart of the preparation process of the 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, 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 the extracting solution; (3) concentrating to obtain soft extract, mixing extractive solutions, filtering, and concentrating under reduced pressure to obtain soft extract; (4) drying the extract, controlling the temperature at 60-80 ℃, drying the extract of the thick paste, and finally crushing to obtain dry extract powder; (5) tabletting, adding carboxymethyl starch sodium and magnesium stearate into the dry extract powder, mixing and tabletting, and coating sugar coat or film coat to obtain final product. The method has simple operation steps and relatively low equipment cost.
However, the aqueous extraction and concentration method has many disadvantages: (1) The loss of active ingredients, especially water-insoluble ingredients, is high by the decocting method; (2) The non-effective components can not be removed to the maximum extent, and the concentration rate is not high enough; (3) The extracting solution has more impurities and fat-soluble components besides the active ingredients, which brings disadvantages to the refining; (4) High temperature operation can cause substantial decomposition of heat sensitive active ingredients; (5) The prepared extract has more impurities, so that more tablets need to be taken by patients every day in daily treatment, and the whole drug effect can be influenced by excessive impurities.
In order to solve the problems and improve the overall quality and efficacy of the traditional Chinese medicine, the extraction process of the traditional Chinese medicine is greatly improved in recent years. Wherein, the enzyme extraction method is a new technology applied to the extraction of the effective components of the traditional Chinese medicine. Especially, the cellulase can destroy the compact structure of plant cell wall, accelerate the dissolution and diffusion of the components in plant cell, and simultaneously the enzyme reaction process can not influence the effective components of traditional Chinese medicine, thereby ensuring the extraction rate. The enzyme extraction method in the prior art generally adds a proper amount of complex enzyme when soaking in water, and an enzymolysis reaction occurs before one-time decoction, so that the extraction rate of the traditional Chinese medicine can be greatly improved, but the method has the following defects: firstly, in order to ensure the efficiency of the whole preparation process, the enzyme-adding water immersion time is generally controlled to be 30-60 minutes, and the destruction rate of plant cell walls cannot be ensured due to the limited compact structure and immersion time of the plant cell walls; secondly, the high temperature during the first decoction completely loses the activity of the enzyme, so that the enzyme effect cannot be extended to the second decoction, the loss of the medicine during the second decoction is more, and the extraction rate of the whole extraction process is reduced; thirdly, the viscosity of the solution after enzyme extraction is high, which increases the difficulty of the subsequent concentration process.
Therefore, increasing the content of active ingredients in the traditional Chinese medicine extraction process and removing non-active ingredients still remain problems to be solved urgently at present.
Disclosure of Invention
Based on the above, the invention aims to overcome the defects in the prior art, and provides a preparation process of daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablets, so as to solve the problems of more impurities in an extracting solution and more loss of active ingredients in the preparation process of daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablets in the prior art.
The technical scheme for solving the technical problems comprises the following steps of soaking, decocting, concentrating and preparing paste, precipitating with ethanol, drying the extract and preparing a preparation into tablets, wherein the decocting and extracting step comprises the following steps:
step S1: the first time of decoction, the medicinal materials and water with the weight 6 to 10 times of the medicinal materials are decocted for 1 to 3 hours in an extraction tank, and then decoction liquid a is extracted;
step S2: carrying out first enzymolysis, adding water with the weight 1 time that of the medicinal materials into the extraction tank, cooling the extraction tank to 45-55 ℃, adding enzyme, and carrying out heat preservation reaction for 30-60 minutes;
and step S3: carrying out second decoction, continuously adding water with the weight 6-10 times that of the medicinal materials into the extraction tank, decocting for 1-3 hours, extracting decoction liquid b, and combining the decoction liquid b with the decoction liquid a to obtain liquid medicine c;
and step S4: and (3) carrying out second enzymolysis, namely cooling the liquid medicine c to 55-65 ℃, adding amylase, and carrying out heat preservation reaction for 1-2 hours.
Compared with the prior art, the preparation process of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet provided by the invention has the advantages that two enzymolysis steps are sequentially arranged aiming at different objects in the decocting process. Wherein enzymolysis reaction is first mainly to the plant cell wall, and it sets up between first decocte and second decocte, and the high temperature heat preservation reaction when first decocte can make the partial cellulose of plant cell hydrolyze, has reduced the compactedness of plant cell wall, carries out enzymolysis reaction again this moment, and efficiency is higher, and whole process time is shorter, and is more energy-conserving, and carries out the second time after the enzymolysis a period and decocte again, great improvement the extraction rate of second time decocte. The second enzymolysis reaction is arranged after the second decoction, and the added amylase can hydrolyze starch with larger molecular weight in the liquid medicine obtained by the two times of decoction into substances with smaller molecular weight, such as maltose, glucose and the like, so that on one hand, the viscosity of the liquid medicine is reduced by liquefying the starch in the liquid medicine, which is convenient for the subsequent concentration process, and on the other hand, the probability of forming a wrapping liquid when a high-concentration ethanol solution is added into the concentrated liquid medicine in the alcohol precipitation stage can be reduced. The preparation method is simple and stable, has concise flow, can meet the requirement of large-scale industrial production, and has wide application prospect and market.
Further, the enzyme in the step S2 is at least one or more of cellulase, pectinase, ligninase and hemicellulase; the amylase in step S4 is alpha-amylase. The extraction process of the Chinese medicinal preparation is mainly blocked by plant cell walls, so that the diffusion speed of chemical components in the Chinese medicinal preparation is relatively low, and the cellulase, the pectinase, the ligninase and the hemicellulase can improve the cracking speed of plant cells and accelerate the diffusion speed of the chemical components. Alpha-amylase acts on amylose and amylopectin to cleave the α -1, 4-chain inside thereof indiscriminately, thereby converting macromolecular starch into substances having a relatively small molecular weight, such as maltose and glucose.
Further, the enzyme in the step S2 is a complex enzyme composed of cellulase, pectinase and hemicellulase, and the weight parts of each component in the complex enzyme are 40-60 parts of cellulase, 30-50 parts of hemicellulase and 10-30 parts of pectinase; the amylase in the step S4 consists of medium-temperature alpha-amylase and high-temperature alpha-amylase in a weight ratio of 1. The raw materials for preparing the traditional Chinese medicine preparation generally adopt roots, stems and leaves of plants, and the roots, the stems, the leaves and the leaves not only have cell walls which mainly comprise cellulose and hemicellulose, but also have pectin adhesion among cells. The cellulase, the pectinase and the hemicellulase are compounded, so that the enzymolysis efficiency is higher. The amylase containing the medium-temperature alpha-amylase and the high-temperature alpha-amylase can keep higher activity at the temperature of 30-100 ℃, so that on one hand, the heat preservation and enzymolysis can be carried out at lower temperature during the second enzymolysis, the energy consumption of the heat preservation is reduced, on the other hand, the starch and dextrin in the liquid medicine can be continuously subjected to enzymolysis in the subsequent liquid medicine concentration process, the enzymolysis time can be effectively prolonged, and the viscosity of the liquid medicine is further reduced.
Furthermore, the addition amount of the complex enzyme and the amylase is 0.6-1.6% of the weight of the medicinal materials respectively.
Further, ultrasonic treatment is carried out on the decoction liquid of the heat preservation reaction while the heat preservation reaction is carried out in the steps S2 and S4, so that the enzymolysis is more sufficient, and the viscosity of the solution after the enzymolysis is reduced.
Further, the alcohol precipitation process comprises the following specific steps:
step A: adding alcohol for the first time, adding ethanol aqueous solution with the volume fraction of 90-95% into the clear paste after the concentrated paste making procedure to obtain alcohol-containing liquid medicine d, stopping adding the alcohol when the alcohol content of the liquid medicine d is 80-85%, carrying out ultrasonic treatment while adding the alcohol, and continuing the ultrasonic treatment for 30-45 minutes after stopping adding the alcohol;
and B: b, first precipitation, namely standing the liquid medicine d subjected to ultrasonic treatment in the step A, and separating to obtain supernatant e and lower precipitate f;
and C: adding alcohol for the second time, adding 90-95% by volume of ethanol aqueous solution into the precipitate f obtained after treatment in the step B, carrying out ultrasonic treatment while adding alcohol, and continuing ultrasonic treatment until the total ultrasonic time is 30-45 minutes after stopping adding alcohol;
step D: and D, performing secondary precipitation, namely standing the mixture subjected to ultrasonic treatment in the step C, extracting supernatant g, and combining the supernatant g and the supernatant e to obtain liquid medicine h.
By adding the alcohol precipitation process, the purposes of removing impurities, reducing the loss of effective components and reducing the dosage are achieved. And the alcohol precipitation process comprises two times of alcohol addition, wherein the alcohol addition for the first time can directly add high-concentration ethanol into the clear paste, and starch in the clear paste is hydrolyzed into maltose and glucose with smaller molecular weight, so that the precipitation which can wrap the liquid medicine is not easily generated even if the clear paste is directly contacted with the high-concentration ethanol. In addition, the invention carries out ultrasonic treatment while adding alcohol, and accelerates the leaching and extraction of the effective components of the traditional Chinese medicine by utilizing the cavitation of ultrasonic waves. Even if a small amount of macromolecular substances such as protein in the fluid extract form hardened precipitates to wrap the liquid medicine when contacting ethanol, the formed wrapping liquid can be destroyed by secondary effects of ultrasonic waves, such as mechanical vibration, diffusion, crushing and the like, so that the diffusion and release of the components to be extracted are accelerated to ensure that the components are fully mixed with the solvent. The process greatly shortens the whole alcohol precipitation time, and ensures that the alcohol precipitation is more sufficient. The second alcohol adding and ultrasonic processing is to perform the crushing and alcohol extracting to the precipitate obtained after the first alcohol precipitation, so as to extract more effective components wrapped in the solid into the liquid medicine and prevent the effective components from losing in the precipitation process. In the scheme, 90-95% ethanol solution is directly used in the two times of alcohol addition, and compared with the method of adding low-concentration ethanol solution and then adding high-concentration solution to reach the target alcohol content in the prior art, the ethanol content required by the scheme is less. And hardened precipitates are not easy to appear under high-concentration ethanol, so that the scheme can take higher ethanol content as an ethanol adding end point, and the ethanol can be more completely purified and is more favorable for ethanol recovery in the subsequent process.
Further, the ethanol solution in the step A and the step C is 90% by volume, and the ethanol solution in the step A is added until the ethanol content of the liquid medicine d is 80%. By taking 90% ethanol solution as an additive and taking the ethanol content of 80% as an ethanol adding end point, on one hand, impurities such as starch, polysaccharide, protein and the like in the liquid medicine can be completely precipitated, and on the other hand, the method can also give consideration to less ethanol adding amount and lower ethanol recovery difficulty, and effectively reduces the production cost.
Further, the volume ratio of the lower layer solid to the ethanol aqueous solution in the step C is 1.
Further, the ultrasonic treatment temperature in the alcohol precipitation step A and the ultrasonic treatment temperature in the alcohol precipitation step C are 40-45 ℃. Is beneficial to the dissolution of the wrapping liquid and the leaching and extraction of the effective components of the traditional Chinese medicine.
Further, the alcohol precipitation process also comprises a step D, and the alcohol precipitation process also comprises a step E, wherein the step E is to concentrate the liquid medicine h obtained in the step D and recover the ethanol. The ethanol is easy to volatilize, and can be recycled, so that the waste of raw materials is reduced.
Drawings
Fig. 1 is a process flow chart of preparation of daphniphyllum calycinum and polygonum hydropiper tablets in the prior art.
Fig. 2 is a flow chart of the preparation process of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet.
Fig. 3 is a flow chart of the decocting process of daphniphyllum calycinum and polygonum hydropiper tablets for intestine and stomach.
Fig. 4 is a flow chart of the alcohol precipitation process of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablets of the invention.
Detailed Description
As shown in fig. 2, fig. 2 is a flow chart of the preparation process of daphniphyllum calycinum and polygonum hydropiper tablets for intestine and stomach of the present invention, and the extraction process comprises the following procedures:
(1) Soaking: putting the selected daphniphyllum calycinum and polygonum hydropiper in an extraction tank in sequence according to the mass ratio of 2 to 1, adding 6 to 10 times (w/w) of water, and soaking for 30 to 45 minutes;
(2) Decocting, as shown in figure 3, which is a flow chart of the decocting process of the daphniphyllum calycinum and polygonum flaccidum tablets for intestines and stomach of the invention, comprises the procedures of first decocting, first enzymolysis, second decocting and second enzymolysis, and comprises the following specific steps:
step S1: the first decoction is carried out, the temperature is raised to 100 ℃ to ensure that the liquid medicine in the extraction tank is in a micro-boiling state, and the decoction is carried out for 1 to 3 hours to obtain decoction a. 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 decoction a enters the liquid storage tank;
step S2: performing first enzymolysis, after extracting the liquid medicine, firstly adding 1 time of water into an extraction tank, adding enzyme when controlling the temperature to be 45-55 ℃, preserving the temperature and performing ultrasonic treatment for 30-60 minutes.
And step S3: and (3) after the second decoction, continuing to add 6-10 times (w/w) of water into the extraction tank for second decoction, raising the temperature to 100 ℃ to ensure that the liquid medicine in the extraction tank is in a micro-boiling state, and decocting for 1-3 hours to obtain decoction b. Opening the liquid outlet valve of the extraction tank to extract the decoction b, and mixing the decoction b with the decoction a to obtain the liquid medicine c.
And step S4: and (3) carrying out second enzymolysis, namely cooling the liquid medicine c to 55-65 ℃, adding amylase, and carrying out heat preservation reaction for 1-2 hours.
Specifically, in the decocting step in this embodiment, the enzyme in step S2 is a complex enzyme composed of cellulase, pectinase and hemicellulase, wherein the complex enzyme comprises, by weight, 40 to 60 parts of cellulase, 30 to 50 parts of hemicellulase, and 10 to 30 parts of pectinase; the amylase in the step S4 is composed of a medium-temperature alpha-amylase and a high-temperature alpha-amylase according to a weight ratio of 1. Wherein the addition amount of the complex enzyme and the amylase is 0.6 to 1.6 percent of the weight of the medicinal materials respectively.
(3) Concentrating to prepare paste: filtering the liquid medicine c after the second enzymolysis, and concentrating the filtrate under reduced pressure until the density is 1.05-1.10 (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 A: adding alcohol for the first time, conveying the concentrated clear paste into an alcohol precipitation tank through a pipeline, confirming the volume of the clear paste through a sight glass and scale marks, adding 90-95% of ethanol by volume fraction, stopping adding the alcohol when the alcohol content of an alcohol-containing liquid medicine d in the alcohol precipitation tank is 80-85%, performing ultrasonic treatment while adding the alcohol, and continuing the ultrasonic treatment for 30-45 minutes after stopping adding the alcohol;
and B: b, first precipitation, namely standing the liquid medicine d subjected to ultrasonic treatment in the step A, and separating to obtain supernatant e and lower precipitate f;
and C: adding alcohol for the second time, adding an ethanol aqueous solution with the volume fraction of 90-95% into the precipitate f obtained after the treatment in the step B, performing ultrasonic treatment while adding the alcohol, stopping adding the alcohol when the volume ratio of the lower-layer solid to the ethanol aqueous solution reaches 1-1.5, and continuing ultrasonic treatment until the total ultrasonic time is 30-45 minutes after stopping adding the alcohol;
step D: c, performing secondary precipitation, namely standing the mixture subjected to ultrasonic treatment in the step C, extracting supernatant g, and combining the supernatant g with supernatant e to obtain liquid medicine h;
step E: and D, concentrating and recovering ethanol, conveying the liquid medicine h obtained in the step D to a concentrator through a pipeline, and recovering and concentrating the ethanol.
Wherein the ultrasonic treatment temperature in the step A and the step C is 40-45 ℃.
(5) Drying the extract: delivering the concentrated solution after alcohol precipitation to an extract collecting tank in a clean area through a pipeline, continuously concentrating under reduced pressure 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, and drying under reduced pressure to obtain the dry extract powder of the ciderage gastrointestinal health.
(6) The preparation is tabletted, and the daphniphyllum calycinum and polygonum flaccidum intestine and stomach rehabilitation dry paste powder is mixed with disintegrating agent, filler, lubricant and flavoring agent, and tabletted to obtain daphniphyllum calycinum and polygonum flaccidum intestine and stomach rehabilitation tablets. Wherein the disintegrating agent is one or more of sodium carboxymethyl starch, crosslinked polyvinylpyrrolidone, low-substituted hydroxypropyl cellulose, and crosslinked sodium carboxymethyl cellulose; the filler is one or more of lactose, sucrose, mannitol, sorbitol, microcrystalline cellulose, starch, pregelatinized starch, calcium sulfate, and calcium hydrogen phosphate; the lubricant is one or more of magnesium stearate, silica gel micropowder and talcum powder; the correctant is one or more of aspartame, glycyrrhizin, betaine, and saccharin sodium.
Compared with the prior art, the preparation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablet comprises two times of enzymolysis reaction, wherein the first time of enzymolysis mainly aims at plant cell walls, and the second time of enzymolysis mainly aims at starch in decoction liquid.
Wherein the enzymolysis setting goes on after first decocte, compare with the scheme that carries out the enzymolysis before the decocte among the prior art directly to the chinese medicinal material earlier, the high temperature heat preservation reaction when this scheme utilization first decocte makes the partial cellulose of plant cell hydrolyze earlier, has reduced the compactedness of plant cell wall, carries out the enzymolysis reaction again this moment, and efficiency is higher, has shortened whole process time, and adds ultrasonic treatment in the enzymolysis reaction, can reduce the viscidity after the liquid medicine enzymolysis. Furthermore, the second decoction is carried out after the enzymolysis is carried out for a period of time, so that the extraction rate of the second decoction is greatly improved.
The second enzymolysis mainly aims at starch in the liquid medicine obtained by two times of decoction. Starch is widely present in tissues such as roots, stems, seeds and the like of plants, and liquid medicine obtained after decoction of traditional Chinese medicinal materials often contains a large amount of starch, so that the liquid medicine has high viscosity, and the difficulty of subsequent concentration and other processes is easily increased. Moreover, because of the large molecular weight of starch, when the water extract is subjected to impurity removal by an alcohol precipitation process, the starch is easily precipitated instantly by high-concentration ethanol, and the starch and protein precipitate form hardening and wrap the liquid medicine, so that the active ingredients are lost. The process can simultaneously act on amylose and amylopectin by adding alpha-amylase into the liquid medicine obtained after two times of decoction, so that the starch with larger molecular weight in the liquid medicine is hydrolyzed into substances with smaller molecular weight, such as maltose, glucose and the like. Furthermore, the alpha-amylase used in the scheme consists of medium-temperature alpha-amylase and high-temperature alpha-amylase, wherein the medium-temperature alpha-amylase has higher activity within the range of 30-70 ℃, the high-temperature alpha-amylase has higher activity within the range of 70-100 ℃, and the combination of the medium-temperature alpha-amylase and the high-temperature alpha-amylase can widen the width range of starch enzymolysis. In the process, the medium-temperature alpha-amylase can enable the enzymolysis reaction to be carried out at a lower temperature, so that the energy consumption in the heat preservation process is reduced, the high-temperature alpha-amylase can continue the starch hydrolysis process to the subsequent reduced-pressure concentration process, namely, the starch and dextrin remained in the liquid medicine can be continuously subjected to enzymolysis while concentrating, so that the reaction is more sufficient, the viscosity of the liquid medicine is further reduced, and the probability of precipitation hardening and liquid medicine wrapping caused by adding high-concentration ethanol in the alcohol precipitation stage is reduced.
In addition, the preparation process of the daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets correspondingly improves the alcohol precipitation process, and achieves the purposes of removing impurities, reducing the loss of effective components, reducing the dosage, reducing the addition of ethanol and reducing the energy consumption of subsequent ethanol recovery. In the scheme, because the enzymolysis reaction is carried out on the medicinal materials and the liquid medicine in the earlier stage and the ultrasonic treatment in the alcohol adding process is carried out, the probability of precipitate hardening is reduced, 95% of ethanol solution can be directly added into the clear paste, and higher end point ethanol concentration can be set. Compared with the method of adding the ethanol solution with the concentration from low to high step by step in the prior art, the method has the advantages of less ethanol amount, quicker and more sufficient precipitation and no increase of the loss of effective components. And the higher end point ethanol concentration can reduce the energy consumption required in the subsequent processes of concentrating the liquid medicine and recovering the ethanol. In addition, compared with the prior art, the scheme adds alcohol again to the sediment obtained after the first alcohol precipitation and carries out ultrasonic treatment, so that the liquid medicine wrapped in the sediment can be released, the loss of effective components is further reduced, and the aim of reducing the dosage is fulfilled.
The preparation process of the tablet is further explained by the following specific examples.
Example 1
The preparation process of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablets 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 to 1, adding 8 times (w/w) of water, and soaking for 30-45 minutes;
(2) Decocting:
step S1: the first decoction, the temperature is raised to 100 ℃ to ensure that the liquid medicine in the extraction tank is in a slightly boiling state, and the decoction is carried out for 2 hours to obtain decoction A. 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 decoction a enters the liquid storage tank;
step S2: performing first enzymolysis, after extracting the liquid medicine, firstly adding 1 time of water into an extraction tank, controlling the temperature to be 45 ℃, adding complex enzyme, preserving heat and performing ultrasonic treatment for 60 minutes.
And step S3: and (3) after the second decoction, continuing adding 8 times (w/w) of water into the extraction tank for second decoction, raising the temperature to 100 ℃ to ensure that the liquid medicine in the extraction tank is in a slightly boiling state, and decocting for 2 hours to obtain decoction b. Opening the liquid outlet valve of the extraction tank to extract the decoction b, and mixing the decoction b with the decoction a to obtain the liquid medicine c.
And step S4: and (3) carrying out second enzymolysis, namely cooling the liquid medicine c to 60 ℃, adding amylase, and carrying out heat preservation reaction for 2 hours.
Specifically, in this embodiment, the compound enzyme comprises 60 parts by weight of cellulase, 40 parts by weight of hemicellulase, 20 parts by weight of pectinase, and the addition amounts of the compound enzyme and amylase are 1.2% and 1% of the weight of the medicinal materials, respectively.
(3) Concentrating the liquid medicine: filtering the liquid medicine c after the secondary enzymolysis, and concentrating the filtrate under reduced pressure until the density is 1.10 (80 ℃), thus obtaining clear paste.
(4) Alcohol precipitation:
step A: adding alcohol for the first time, conveying the concentrated fluid extract into an alcohol precipitation tank through a pipeline, confirming the volume of the fluid extract through a sight glass and scale marks, adding ethanol with the volume fraction of 90%, stopping adding the alcohol when the alcohol content of the fluid extract is 80%, performing ultrasonic treatment while adding the alcohol, and continuing the ultrasonic treatment until the total ultrasonic time is 45 minutes after stopping adding the alcohol;
and B, step B: b, performing primary precipitation, namely standing the clear paste subjected to ultrasonic treatment in the step A, and separating to obtain a supernatant d and a lower-layer solid e;
and C: adding alcohol for the second time, adding an ethanol water solution with the volume fraction of 90% into the lower-layer solid e treated in the step B, performing ultrasonic treatment while adding the alcohol, stopping adding the alcohol when the volume ratio of the lower-layer solid to the ethanol water solution reaches 1, and continuing the ultrasonic treatment until the total ultrasonic time is 45 minutes after stopping adding the alcohol;
step D: c, performing secondary precipitation, namely standing the mixture subjected to ultrasonic treatment in the step C, extracting supernatant f, and combining the supernatant f with supernatant d to obtain liquid medicine g;
and E, step E: concentrating and recovering ethanol, conveying the liquid medicine g obtained in the step D 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, continuously concentrating under reduced pressure until the relative density of the extract is 1.25 (80 ℃) to obtain thick paste, opening a discharge valve, introducing the thick paste into a container, and drying under reduced pressure to obtain the daphniphyllum calycinum gastrointestinal health dry extract powder.
(6) The preparation is tabletted, the daphniphyllum calycinum and polygonum hydropiper intestine and stomach rehabilitation dry extract powder is mixed with sodium carboxymethyl starch, magnesium stearate and aspartame to be evenly mixed, and sugar coating or film coating is carried out after tabletting, thus obtaining the daphniphyllum calycinum and stomach rehabilitation tablet.
Example 2
The preparation process of the daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1 except that the steps S2 and S4 of the decoction process are different from that in embodiment 1, and the details are not repeated herein. The differences of the steps S2 and S4 of the decoction process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablet in the embodiment from the embodiment 1 are as follows:
(2) Decocting:
step S2: performing first enzymolysis, after extracting the liquid medicine, firstly adding 1 time of water into an extraction tank, controlling the temperature to be 55 ℃, adding complex enzyme, preserving heat and performing ultrasonic treatment for 30 minutes.
And step S4: and (3) carrying out second enzymolysis, namely cooling the liquid medicine c to 55 ℃, adding amylase, and carrying out heat preservation reaction for 1 hour.
Specifically, in this embodiment, the compound enzyme comprises 40 parts by weight of cellulase, 30 parts by weight of hemicellulase, 30 parts by weight of pectinase, and the addition amounts of the compound enzyme and the amylase are 0.6% and 0.8% of the weight of the medicinal materials, respectively.
Example 3
The preparation process of the daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1 except that the steps S2 and S4 of the decoction process are different from that in embodiment 1, and the details are not repeated herein. The differences of the steps S2 and S4 of the decoction process of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet in the embodiment from the embodiment 1 are as follows:
(2) Decocting:
step S2: performing first enzymolysis, after extracting the liquid medicine, firstly adding 1 time of water into an extraction tank, controlling the temperature to be 55 ℃, adding complex enzyme, preserving heat and performing ultrasonic treatment for 45 minutes.
And step S4: and (3) carrying out enzymolysis for the second time, cooling the liquid medicine c to 60 ℃, adding amylase, and carrying out heat preservation reaction for 1.5 hours.
Specifically, in this embodiment, the compound enzyme comprises 60 parts by weight of cellulase, 30 parts by weight of hemicellulase, 30 parts by weight of pectinase, and the addition amounts of the compound enzyme and the amylase are 0.6% and 0.6% of the weight of the medicinal materials, respectively.
Example 4
The preparation process of the daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1 except that the steps S2 and S4 of the decoction process are different from that in embodiment 1, and the details are not repeated herein. The differences of the steps S2 and S4 of the decoction process of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet in the embodiment from the embodiment 1 are as follows:
(2) Decocting:
step S2: performing first enzymolysis, after extracting the liquid medicine, firstly adding 1 time of water into an extraction tank, controlling the temperature to be 45 ℃, adding complex enzyme, preserving heat and performing ultrasonic treatment for 60 minutes.
And step S4: and (3) carrying out second enzymolysis, namely cooling the liquid medicine c to 55 ℃, adding amylase, and carrying out heat preservation reaction for 1 hour.
Specifically, in this embodiment, the compound enzyme comprises 40 parts by weight of cellulase, 50 parts by weight of hemicellulase, 30 parts by weight of pectinase, and the addition amounts of the compound enzyme and amylase are 0.8% and 1% of the weight of the medicinal materials, respectively.
Example 5
The preparation process of the daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1 except that the steps S2 and S4 of the decoction process are different from that in embodiment 1, and the details are not repeated herein. The differences of the steps S2 and S4 of the decoction process of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet in the embodiment from the embodiment 1 are as follows:
(2) Decocting:
step S2: performing first enzymolysis, after extracting the liquid medicine, firstly adding 1 time of water into an extraction tank, controlling the temperature at 50 ℃, adding a complex enzyme, preserving the temperature and performing ultrasonic treatment for 60 minutes.
And step S4: and (3) carrying out second enzymolysis, namely cooling the liquid medicine c to 65 ℃, adding amylase, and carrying out heat preservation reaction for 2 hours.
Specifically, in this embodiment, the composite enzyme comprises 40 parts by weight of cellulase, 50 parts by weight of hemicellulase, 10 parts by weight of pectinase, and the addition amounts of the composite enzyme and amylase are 1% and 1% of the weight of the medicinal materials, respectively.
Example 6
The preparation process of the daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1 except that the steps S2 and S4 of the decoction process are different from that in embodiment 1, and the details are not repeated herein. The differences of the steps S2 and S4 of the decoction process of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet in the embodiment from the embodiment 1 are as follows:
(2) Decocting:
step S2: performing first enzymolysis, after extracting the liquid medicine, firstly adding 1 time of water into an extraction tank, controlling the temperature at 45 ℃, adding a complex enzyme, preserving the temperature and performing ultrasonic treatment for 45 minutes.
And step S4: and (3) carrying out enzymolysis for the second time, cooling the liquid medicine c to 60 ℃, adding amylase, and carrying out heat preservation reaction for 1.5 hours.
Specifically, in this embodiment, the compound enzyme comprises 50 parts by weight of cellulase, 30 parts by weight of hemicellulase, 20 parts by weight of pectinase, and the addition amounts of the compound enzyme and amylase are 1% and 0.8% of the weight of the medicinal materials, respectively.
Example 7
The preparation process of the daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets in this embodiment is completely the same as that in embodiment 1 except that the steps S2 and S4 of the decoction process are different from that in embodiment 1, and the details are not repeated herein. The differences of the steps S2 and S4 of the decoction process of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet in the embodiment from the embodiment 1 are as follows:
(2) Decocting:
step S2: performing first enzymolysis, after extracting the liquid medicine, firstly adding 1 time of water into an extraction tank, controlling the temperature at 50 ℃, adding a complex enzyme, preserving the temperature and performing ultrasonic treatment for 60 minutes.
And step S4: and (3) carrying out second enzymolysis, namely cooling the liquid medicine c to 55 ℃, adding amylase, and carrying out heat preservation reaction for 2 hours.
Specifically, in this embodiment, the composite enzyme comprises 60 parts by weight of cellulase, 40 parts by weight of hemicellulase, and 20 parts by weight of pectinase, and the addition amounts of the composite enzyme and amylase are 1% and 1.2% of the weight of the medicinal materials, respectively.
Example 8
The preparation process of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet in this embodiment is completely the same as that in embodiment 1 except that the steps S2 and S4 of the decoction process are different from that in embodiment 1, and the details are not repeated herein. The differences of the steps S2 and S4 of the decoction process of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet in the embodiment from the embodiment 1 are as follows:
(2) Decocting:
step S2: performing first enzymolysis, after extracting the liquid medicine, firstly adding 1 time of water into an extraction tank, controlling the temperature at 50 ℃, adding a complex enzyme, preserving the temperature and performing ultrasonic treatment for 30 minutes.
And step S4: and (3) carrying out enzymolysis for the second time, cooling the liquid medicine c to 60 ℃, adding amylase, and carrying out heat preservation reaction for 2 hours.
Specifically, in this embodiment, the compound enzyme comprises 40 parts by weight of cellulase, 50 parts by weight of hemicellulase, 20 parts by weight of pectinase, and the addition amounts of the compound enzyme and amylase are 0.8% and 0.6% of the weight of the medicinal materials, respectively.
Comparative example 1
The preparation process of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet comprises the following steps:
(1) Soaking: putting the selected daphniphyllum calycinum and polygonum hydropiper in an extraction tank in sequence according to the mass ratio of 2 to 1, adding 8 times (w/w) of water, and soaking for 30-45 minutes;
(2) Decocting:
step S1: decocting for the first time, raising the temperature to 100 ℃ to ensure that the liquid medicine in the extraction tank is in a slightly boiling state, and decocting for 2 hours to obtain decoction a. 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 decoction a enters the liquid storage tank;
step S2: continuously adding 8 times (w/w) of water into the extraction tank for second decoction, raising the temperature to 100 ℃ to ensure that the liquid medicine in the extraction tank is in a slightly boiling state, and decocting for 2 hours to obtain decoction liquid b. Opening the liquid outlet valve of the extraction tank to extract the decoction b, and mixing the decoction b with the decoction a to obtain the liquid medicine c.
(3) Concentrating the liquid medicine: filtering the liquid medicine c, and concentrating the filtrate under reduced pressure to density of 1.10 (80 deg.C) to obtain fluid extract.
(4) Alcohol precipitation:
step A: adding alcohol, conveying the concentrated fluid extract into an alcohol precipitation tank through a pipeline, confirming the volume of the fluid extract through a sight glass and scale marks, adding 90% of ethanol by volume fraction, stopping adding the alcohol when the alcohol content of the solution in the alcohol precipitation tank is 80%, performing ultrasonic treatment while adding the alcohol, and continuing the ultrasonic treatment for 45 minutes after stopping adding the alcohol;
and B, step B: precipitating, standing the clear paste subjected to ultrasonic treatment in the step A, and separating to obtain a supernatant d and a lower solid e;
step C: concentrating and recovering ethanol, conveying the supernatant d obtained in the step B to a concentrator through a pipeline, and recovering and concentrating the ethanol.
(5) Drying the extract: and introducing the thick paste into a container for drying under reduced pressure to obtain the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health dry paste powder.
(6) The preparation is tabletted, the daphniphyllum calycinum and polygonum hydropiper intestine and stomach rehabilitation dry extract powder is mixed with sodium carboxymethyl starch, magnesium stearate and aspartame to be evenly mixed, and sugar coating or film coating is carried out after tabletting, thus obtaining the daphniphyllum calycinum and stomach rehabilitation tablet.
Comparative example 2
The preparation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets comprises the following steps:
(1) Soaking: putting the selected daphniphyllum calycinum and polygonum hydropiper in an extraction tank in sequence according to the mass ratio of 2 to 1, adding 8 times (w/w) of water, and soaking for 30-45 minutes;
(2) Decocting:
step S1: decocting for the first time, raising the temperature to 100 ℃ to ensure that the liquid medicine in the extraction tank is in a slightly boiling state, and decocting for 2 hours to obtain decoction a. 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 decoction a enters the liquid storage tank;
step S2: continuously adding 8 times (w/w) of water into the extraction tank for second decoction, raising the temperature to 100 ℃ to ensure that the liquid medicine in the extraction tank is in a slightly boiling state, and decocting for 2 hours to obtain decoction b. Opening the liquid outlet valve of the extraction tank to extract the decoction b, and mixing the decoction b with the decoction a to obtain the liquid medicine c.
(3) Concentrating the liquid medicine: filtering the liquid medicine c, and concentrating the filtrate under reduced pressure to density of 1.10 (80 deg.C) to obtain fluid extract.
(4) Alcohol precipitation:
step A: adding alcohol for the first time, conveying the concentrated fluid extract into an alcohol precipitation tank through a pipeline, confirming the volume of the fluid extract through a sight glass and scale marks, adding 90% ethanol by volume fraction, stopping adding alcohol when the alcohol content of the solution in the alcohol precipitation tank is 80%, performing ultrasonic treatment while adding alcohol, and continuing ultrasonic treatment for 45 minutes after stopping adding alcohol;
and B, step B: b, performing primary precipitation, namely standing the clear paste subjected to ultrasonic treatment in the step A, and separating to obtain a supernatant d and a lower-layer solid e;
step C: adding alcohol for the second time, adding an ethanol water solution with the volume fraction of 90% into the solid e obtained after the treatment in the step B, performing ultrasonic treatment while adding the alcohol, stopping adding the alcohol when the volume ratio of the lower-layer solid to the ethanol water solution reaches 1, and continuing ultrasonic treatment for 45 minutes after stopping adding the alcohol;
step D: c, performing secondary precipitation, namely standing the mixture subjected to ultrasonic treatment in the step C, extracting supernatant fluid f, and combining the supernatant fluid f with the supernatant fluid d to obtain liquid medicine g;
and E, step E: and D, concentrating and recovering ethanol, conveying the liquid medicine g obtained in the step D to a concentrator through a pipeline, and recovering and concentrating the ethanol.
(5) And (3) drying the extract: delivering the concentrated solution after alcohol precipitation to an extract collecting tank in a clean area through a pipeline, continuously concentrating under reduced pressure 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, and drying under reduced pressure to obtain the dry extract powder of the ciderage gastrointestinal health.
(6) The preparation is tabletted, the daphniphyllum calycinum and polygonum orientale intestine and stomach health dry extract powder is mixed with sodium carboxymethyl starch, magnesium stearate and aspartame, and the tablet is tabletted and coated with sugar coating or film coating to obtain the daphniphyllum calycinum and stomach health tablet.
Test examples, comparative experiment of Total Flavonoids content
The test example verifies that the preparation method of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablets has higher extraction rate by measuring and calculating the content of total flavonoids in examples 1-8, 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 percent, which is used in Chinese medicine biological product identification). The used instruments are: UV759 ultraviolet-visible spectrophotometer (shanghai seminaceae); CP214 electronic analytical balance (aohaus instruments shanghai ltd).
Firstly, accurately weighing 5mg of dried constant-weight rutin reference substance, dissolving the rutin reference substance by using 60% ethanol, fixing the volume to a 25ml volumetric flask, and shaking up to obtain a rutin reference substance solution with the 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, precisely sucking 5ml of supernatant liquor prepared in the alcohol precipitation process of the daphniphyllum calycinum tablets of examples 1 to 8 and comparative examples 1 and 2 of the invention respectively, evaporating to dryness in an evaporation dish, dissolving with 60% ethanol, fully transferring to a 25ml volumetric flask, fixing the volume to the scale with 60% ethanol, accurately measuring 5ml from the volumetric flask, placing in the 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. Measuring absorbance (A) at 510nm with ultraviolet spectrophotometer, and calculating the extraction rate of total flavone from the extract according to standard curve and the following formula.
Total flavone extraction amount (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 extraction of flavones from each of 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 has a good linear relation with the absorbance, experiments show that the embodiment 1 is the best embodiment, the compound enzyme which is composed of 60 parts of cellulase, 40 parts of hemicellulase and 20 parts of pectinase in parts by weight is adopted, the adding amount of the compound enzyme and the amylase is 1.2 percent and 1 percent of the weight of the medicinal materials respectively, the temperature of the primary enzymolysis is controlled at 45 ℃, the heat preservation and the ultrasonic treatment are carried out for 60 minutes, and the temperature of the secondary enzymolysis is controlled at 60 ℃, the heat preservation and the ultrasonic treatment are carried out for 2 hours. In the alcohol precipitation process, 90% ethanol is added firstly until the alcohol content in the solution is 80%, the first alcohol addition treatment is carried out, the ultrasonic treatment is carried out for 45 minutes after the standing separation and precipitation, the 90% ethanol is added into the precipitation for the second time, and then the ultrasonic treatment is carried out for 45 minutes, at the moment, the highest total flavone extraction amount can reach 46.14mg/g, so that the effective components can be extracted and used to the maximum extent, and the prepared daphniphyllum calycinum tablets have better effect.
Compared with the prior art, the preparation process of the daphniphyllum calycinum and polygonum flaccidum gastrointestinal health tablets comprises two times of enzymolysis reaction, wherein the first time of enzymolysis is carried out after the first decoction, and the high-temperature heat preservation reaction during the first decoction can hydrolyze part of cellulose of plant cells, so that the compactness of plant cell walls is reduced, the enzymolysis reaction is carried out again, the efficiency is higher, the whole process time is shortened, the ultrasonic treatment is added during the enzymolysis reaction, the viscosity of the liquid medicine after enzymolysis can be reduced, further, the second time of decoction is carried out after a period of enzymolysis, and the extraction rate of the second time of decoction is greatly improved. And the starch in the liquid medicine is hydrolyzed into maltose or glucose with smaller molecular weight by the second enzymolysis, so that the viscosity of the liquid medicine can be reduced, the subsequent concentration process can be facilitated, and the probability of precipitation hardening and liquid medicine wrapping caused by adding high-concentration ethanol in the alcohol precipitation stage can be reduced. Furthermore, the combination of the medium-temperature alpha-amylase and the high-temperature alpha-amylase in the second enzymolysis can prolong the enzymolysis time of the starch, so that the liquid medicine can be subjected to enzymolysis continuously in the concentration process, the reaction is more complete, the viscosity of the liquid medicine is further reduced, and the probability of precipitation hardening during alcohol precipitation is reduced.
In addition, the preparation process of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablet disclosed by the invention also improves an alcohol precipitation process, and achieves the purposes of removing impurities, reducing the loss of effective components, reducing the dosage, reducing the addition amount of ethanol and reducing the energy consumption for subsequent ethanol recovery. The ethanol precipitation process directly adds high-concentration ethanol solution into the fluid extract, the required ethanol amount is less, the precipitation is quicker and more sufficient, and the precipitation hardening is not easy to generate under the action of the early enzymolysis and ultrasonic wave to cause the loss of effective components. Furthermore, the scheme also adds a second alcohol adding process, which can release the liquid medicine wrapped in the sediment generated after the first alcohol adding, further reduces the loss of effective components, thereby achieving the purpose of reducing the dosage. In addition, the concentration of the ethanol at the reachable end point is higher, so that the energy consumption for subsequently recovering the ethanol can be further reduced.
The preparation process of the daphniphyllum calycinum and polygonum hydropiper gastrointestinal health tablets is simple, stable, sufficient in alcohol precipitation, short in extraction time, high in yield, capable of meeting the requirements of large-scale industrial production, and wide in application prospect and market. 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 various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention.
Claims (10)
1. A preparation process of daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets comprises the working procedures of soaking, decocting, concentrating and preparing paste, alcohol precipitating, drying the paste and preparing tablets, and is characterized in that the decocting working procedure comprises the following steps:
step S1: first decocting, decocting the medicinal materials and water 6-10 times the weight of the medicinal materials in an extraction tank for 1-3 hours, and then extracting a decoction a;
step S2: performing first enzymolysis, adding water with the weight 1 time that of the medicinal materials into an extraction tank, cooling the extraction tank to 45-55 ℃, adding enzyme, and performing heat preservation reaction for 30-60 minutes;
and step S3: carrying out second decoction, continuously adding water with the weight 6-10 times that of the medicinal materials into the extraction tank, decocting for 1-3 hours, extracting decoction liquid b, and combining the decoction liquid b with the decoction liquid a to obtain liquid medicine c;
and step S4: and (3) carrying out second enzymolysis, namely cooling the liquid medicine c to 55-65 ℃, adding amylase, and carrying out heat preservation reaction for 1-2 hours.
2. The process for preparing daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets as claimed in claim 1, is characterized in that: the enzyme in the step S2 is at least one or more of cellulase, pectinase, ligninase and hemicellulase; the amylase in step S4 is alpha-amylase.
3. The preparation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal rehabilitation tablet as claimed in claim 2, is characterized in that: the enzyme in the step S2 is a complex enzyme consisting of 40-60 parts by weight of cellulase, 30-50 parts by weight of hemicellulase and 10-30 parts by weight of pectinase; the amylase in the step S4 is composed of medium-temperature alpha-amylase and high-temperature alpha-amylase according to a weight ratio of 1.
4. The preparation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal rehabilitation tablet as claimed in claim 3, is characterized in that: the addition amount of the complex enzyme and the amylase is 0.6 to 1.6 percent of the weight of the medicinal materials respectively.
5. The preparation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal rehabilitation tablet as claimed in claim 4, is characterized in that: and in the step S2 and the step S4, ultrasonic treatment is carried out on the decoction liquid of the heat preservation reaction while the heat preservation reaction is carried out.
6. The process for preparing daphniphyllum calycinum and polygonum orientale gastrointestinal health tablets as claimed in any one of claims 1 to 5, wherein: the alcohol precipitation procedure comprises the following steps:
step A: adding alcohol for the first time, adding 90-95% by volume of ethanol aqueous solution into the clear paste obtained after the concentrated paste making process to obtain alcohol-containing liquid medicine d, stopping adding the alcohol when the alcohol content of the liquid medicine d is 80-85%, performing ultrasonic treatment while adding the alcohol, and continuing the ultrasonic treatment for 30-45 minutes after stopping adding the alcohol;
and B, step B: b, first precipitation, namely standing the liquid medicine d subjected to ultrasonic treatment in the step A, and separating to obtain supernatant e and lower precipitate f;
and C: adding alcohol for the second time, adding 90-95% by volume of ethanol aqueous solution into the precipitate f obtained after treatment in the step B, carrying out ultrasonic treatment while adding alcohol, and continuing ultrasonic treatment until the total ultrasonic time is 30-45 minutes after stopping adding alcohol;
step D: and D, performing secondary precipitation, namely standing the mixture subjected to ultrasonic treatment in the step C, extracting supernatant g, and combining the supernatant g and the supernatant e to obtain liquid medicine h.
7. The preparation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal rehabilitation tablet as claimed in claim 6, is characterized in that: the ethanol solution in the step A and the ethanol solution in the step C are 90% by volume, and the ethanol solution is added in the step A until the ethanol content of the liquid medicine d is 80%.
8. The preparation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal rehabilitation tablet as claimed in claim 7, is characterized in that: the volume ratio of the ethanol solution added in the step C to the lower-layer solid f is 1.
9. The preparation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal rehabilitation tablet as claimed in claim 8, is characterized in that: the ultrasonic treatment temperature in the alcohol precipitation step A and the step C is 40-45 ℃.
10. The preparation process of the daphniphyllum calycinum and polygonum orientale gastrointestinal rehabilitation tablet as claimed in claim 9, is characterized in that: and the alcohol precipitation process also comprises a step E, wherein the step E is to concentrate the liquid medicine h obtained in the step D and recover the ethanol.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103040898A (en) * | 2012-12-19 | 2013-04-17 | 广西禅方药业有限公司 | Process of radix isatidis extract enzymolysis-alcohol precipitation for removing impurities |
| CN104069191A (en) * | 2014-06-30 | 2014-10-01 | 广东药学院 | Extraction process of total flavonoids of polygonum criopolitanum |
| CN105106327A (en) * | 2015-09-10 | 2015-12-02 | 广西大学 | Process for extracting total flavones of red-knees herb by adopting enzymolysis-ultrasonic coupling method |
| CN112972527A (en) * | 2019-12-13 | 2021-06-18 | 特一药业集团股份有限公司 | Fengliaochangweikang tablet and its extraction process |
Family Cites Families (1)
| 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 |
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2022
- 2022-08-10 CN CN202210954636.4A patent/CN115192637A/en active Pending
- 2022-10-18 WO PCT/CN2022/125904 patent/WO2024031830A1/en unknown
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103040898A (en) * | 2012-12-19 | 2013-04-17 | 广西禅方药业有限公司 | Process of radix isatidis extract enzymolysis-alcohol precipitation for removing impurities |
| CN104069191A (en) * | 2014-06-30 | 2014-10-01 | 广东药学院 | Extraction process of total flavonoids of polygonum criopolitanum |
| CN105106327A (en) * | 2015-09-10 | 2015-12-02 | 广西大学 | Process for extracting total flavones of red-knees herb by adopting enzymolysis-ultrasonic coupling method |
| CN112972527A (en) * | 2019-12-13 | 2021-06-18 | 特一药业集团股份有限公司 | Fengliaochangweikang tablet and its extraction process |
Non-Patent Citations (4)
| Title |
|---|
| 刘富梁等: "酶法在中药提取中的研究进展", 《时珍国医国药》 * |
| 刘洪梅等: "枫蓼发酵提取液总黄酮含量测定及药效", 《中国兽医学报》 * |
| 杨再等: "天然植物有效成分的提取新技术――生物酶解技术", 《饲料博览》 * |
| 罗文涓等: "酶解―超声偶联法提取辣蓼总黄酮方法研究", 《畜牧与饲料科学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| WO2024031830A1 (en) | 2024-02-15 |
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