CN116036144A - Preparation method of water-soluble liver and gall extract powder - Google Patents

Preparation method of water-soluble liver and gall extract powder Download PDF

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Publication number
CN116036144A
CN116036144A CN202310230836.XA CN202310230836A CN116036144A CN 116036144 A CN116036144 A CN 116036144A CN 202310230836 A CN202310230836 A CN 202310230836A CN 116036144 A CN116036144 A CN 116036144A
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extract powder
water
supernatant
gall
drying
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邵谱
杨鹤云
刘佳
董玉青
李建强
王佳琪
郭莉
安宥静
王孟
张金蕾
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Baoding Jizhong Pharmaceutical Co ltd
BAODING YANGGUANG BENCAO PHARM
Baoding Jizhong Biotechnology Co ltd
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Baoding Jizhong Pharmaceutical Co ltd
BAODING YANGGUANG BENCAO PHARM
Baoding Jizhong Biotechnology Co ltd
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Abstract

The invention relates to the technical field of traditional Chinese veterinary medicines, and provides a preparation method of water-soluble liver and gall extract powder, which comprises the following steps: s1, extracting herba Artemisiae Scopariae with ethanol to obtain herba Artemisiae Scopariae supernatant and herba Artemisiae Scopariae residue; s2, concentrating the virgate wormwood supernatant under reduced pressure, and filtering to obtain filtrate; s3, heating the filtrate to 55-65 ℃, adding hydroxypropyl beta cyclodextrin, and preserving heat for 1-2h; s4, drying and crushing to obtain capillary artemisia alcohol extract powder; s5, adding radix isatidis and trehalose into the capillary artemisia herb residue, mixing and extracting with water to obtain a supernatant; s6, concentrating the supernatant under reduced pressure, filtering, drying, crushing, and uniformly mixing with the capillary artemisia alcohol extract powder to obtain water-soluble liver and gall extract powder. By the technical scheme, the problems of identification of virgate wormwood herb and arginine in liver and gall particles and precipitation during dissolution of the particles in the prior art are solved.

Description

Preparation method of water-soluble liver and gall extract powder
Technical Field
The invention relates to the technical field of traditional Chinese veterinary medicines, in particular to a preparation method of water-soluble liver and gall extract powder.
Background
The liver and gall granule is a variety recorded in traditional Chinese medicine rolls of the 2017 edition of veterinary quality standard, and the main components of the liver and gall granule are isatis root and virgate wormwood herb, and the product produced according to the existing production method has the following problems in the inspection process:
1. the quantity and the color of the fluorescence spots identified by the herba artemisiae capillaries are inconsistent with those of the fluorescence spots of the control medicinal material;
2. the particles have sediment when dissolved, and the dissolubility is unqualified;
3. arginine identifies tailing.
According to the existing production operation method, the problem 1 and the problem 2 can not be solved at the same time, so that the method for manufacturing the compound capable of solving the identification problem of the capillary artemisia and the arginine and solving the solubility problem is very important to find out in actual production.
In order to solve the problems of the products, the related technical personnel adds an organic solvent extraction link in the manufacturing method process, and the problems of spot color and quantity of the identified virgate wormwood herb can be met, but the generated products have precipitates in the dissolution process, so that the dissolubility is unqualified. And the use of multiple organic solvents during the production process also increases the production safety risk. There are also related technicians who modify the sample in terms of pre-test treatment and test result decision criteria, but there is a question of not changing the product manufacturing method itself, and there is a suspicion of cutting off proper performance.
Disclosure of Invention
The invention provides a preparation method of water-soluble liver and gall extract powder, which solves the problems of identification of virgate wormwood herb and arginine in liver and gall particles and precipitation when the particles are dissolved in the prior art.
The technical scheme of the invention is as follows:
a preparation method of water-soluble liver and gall extract powder comprises the following steps:
s1, extracting herba Artemisiae Scopariae with ethanol to obtain herba Artemisiae Scopariae supernatant and herba Artemisiae Scopariae residue;
s2, concentrating the virgate wormwood supernatant under reduced pressure, and filtering to obtain filtrate;
s3, heating the filtrate to 55-65 ℃, adding hydroxypropyl beta cyclodextrin, and preserving heat for 1-2h;
s4, drying and crushing to obtain capillary artemisia alcohol extract powder;
s5, adding the isatis root and the trehalose into the capillary artemisia herb residues, mixing and extracting with water to obtain a supernatant;
s6, concentrating the supernatant under reduced pressure, filtering, drying, crushing, and uniformly mixing with the capillary artemisia alcohol extract powder to obtain water-soluble liver and gall extract powder.
As a further technical solution, the step S6 specifically includes:
concentrating the supernatant under reduced pressure, filtering, heating to 55-65deg.C, adding lactose, maintaining the temperature for 0.5-1 hr, oven drying, pulverizing, and mixing with the ethanol extract powder of herba Artemisiae Scopariae to obtain water-soluble liver and gallbladder extract powder.
As a further technical scheme, the preparation method of the water-soluble liver and gall extract powder comprises the following steps:
s1, adding 1200-1600L of ethanol into 120-200kg of herba Artemisiae Scopariae, and extracting with ethanol to obtain herba Artemisiae Scopariae supernatant and herba Artemisiae Scopariae residue;
s2, concentrating the virgate wormwood supernatant under reduced pressure, and filtering to obtain filtrate;
s3, heating the filtrate to 55-65 ℃, adding 24-40kg of hydroxypropyl beta cyclodextrin, and preserving heat for 1-2h;
s4, drying and crushing to obtain capillary artemisia alcohol extract powder;
s5, adding 120-200kg of radix isatidis and 6-10kg of trehalose into the capillary artemisia herb residue, mixing and extracting with water to obtain supernatant;
s6, concentrating the supernatant under reduced pressure, filtering, heating to 55-65 ℃, adding 3.6-6kg lactose, preserving heat for 0.5-1h, drying, crushing, and uniformly mixing with the capillary artemisia alcohol extract powder to obtain water-soluble liver and gall extract powder.
Preferably, the step S6 specifically includes:
concentrating the supernatant under reduced pressure, filtering, heating to 60+ -2deg.C, adding 3.6-6kg lactose, maintaining the temperature for 0.5h, oven drying, pulverizing, and mixing with the herba Artemisiae Scopariae ethanol extract powder to obtain water-soluble liver and gallbladder extract powder.
As a further technical solution, the step S5 specifically includes:
s51, adding 120-200kg of radix isatidis and 3-5kg of trehalose into the capillary artemisia herb residue, mixing, adding 1440-3200L of water, heating to boiling for one-time extraction, and collecting an extracting solution;
s52, continuously adding 1440-2400L of water and 3-5kg of trehalose into the residues, heating to boiling for secondary extraction, and mixing the two extracts to obtain a supernatant.
As a further technical scheme, in the step S51, water is added and then soaked for 1-2 hours.
As a further technical scheme, in the step S1, alcohol is soaked in ethanol for 1h in advance.
As a further technical scheme, in the step S1, the alcohol extraction temperature is 55-65 ℃ and the time is 1.5-3 hours; preferably, the alcohol extraction temperature is 60+/-2 ℃ for 2 hours.
As a further technical scheme, in the step S1, the alcohol extraction temperature is achieved by controlling the temperature of the interlayer circulating water of the extraction tank.
As a further technical scheme, in the step S1, the alcohol extraction is performed in a basket type extraction tank, and a circulating pump is adopted for cooperation.
The ethanol circularly flows in the extraction tank through the circulating pump, so that the ethanol fully contacts the capillary artemisia herb medicine and the ethanol extract is distributed more uniformly.
As a further technical scheme, in the step S2, the mixture is concentrated to a relative density of 0.95-1.15 under reduced pressure; in the step S6, the mixture is concentrated to the relative density of 1.15-1.25 under reduced pressure.
As a further technical scheme, in the step S4 and the step S6, the continuous vacuum crawler-type dryer is adopted for drying, and the temperature is controlled to be 55-65 ℃ for 4 hours.
As a further technical scheme, in the step S1 and the step S5, the alcohol extraction and the water extraction are performed in a basket type extraction tank; in the step S2 and the step S6, the concentration adopts a multifunctional double-effect concentrator.
As a further technical scheme, in the step S2 and the step S6, the filtration is 200 mesh filtration.
As a further technical scheme, after the step S1 is finished, steam is introduced for 30min to remove alcohol.
As a further technical scheme, in the step S4 and the step S6, 100 mesh crushing is performed after drying.
The working principle and the beneficial effects of the invention are as follows:
1. in the invention, ethanol is used as an extractant to increase the dissolution of fat-soluble substances, and hydroxypropyl beta cyclodextrin is added in the concentration process of the capillary artemisia, so that the solubility of fat-soluble components extracted by the capillary artemisia through the ethanol is improved, and the problem of unqualified product solubility is solved.
2. When the capillary artemisia is extracted, ethanol is adopted as an extractant, the low-temperature extraction temperature is controlled, and then the capillary artemisia is matched with a circulating pump for use, so that the dispersion and dissolution of capillary artemisia ethanol extract are promoted, the production time is shortened, the use of various organic solvents is avoided, the production safety risk is reduced, the sewage treatment pressure is reduced, the problem that blue spots and red spots appear in the capillary artemisia thin-layer identification chromatography of liver and gall extract powder is solved, and the number and the positions of the spots are consistent with those of capillary artemisia control medicinal materials.
3. According to the invention, the isatis root is extracted by water, the trehalose is added in the concentration process, the compound auxiliary material mode is combined with the cooling friability of the continuous low-temperature vacuum crawler-type dryer, the trehalose is matched with the lactose for use, the trehalose plays a role in supporting a framework when materials are in a solid-liquid mixed state, viscous substances are uniformly dispersed and are not aggregated, the drying and crushing of the materials are facilitated, the viscosity of the materials is reduced, and therefore, the problem of tailing in drug identification and inspection is solved, the product percent of pass is improved, and the problem that the clinical effect of the product is influenced by removing the isatis root polysaccharides with biological activity in the alcohol precipitation operation in the conventional production method is avoided.
4. In the invention, the capillary artemisia alcohol extract is dried by a continuous low-temperature vacuum crawler-type dryer, the included alcohol extract is not easy to volatilize in a low-temperature vacuum environment, and the effective substances can be completely reserved.
5. The production materials obtained by the preparation method can be used for product dosage forms such as wet granulation, boiling granulation, dry granulation, capsules, tabletting and the like.
6. According to the characteristics of medicines, the invention adopts production equipment matched with a hanging basket type extracting tank, a multifunctional double-effect concentrator, a liquid storage tank and a continuous low-temperature vacuum crawler-type dryer, and the production equipment and related production conditions have explosion-proof functions, thereby ensuring the production safety.
Drawings
The invention will be described in further detail with reference to the drawings and the detailed description.
FIG. 1 is a schematic diagram of a production facility of the present invention;
FIG. 2 shows the result of solubility detection;
FIG. 3 shows a thin-layer chromatography for discriminating herba Artemisiae Scopariae of liver and gall extract powder;
fig. 4 is a thin-layer identification chart of liver and gall extract powder arginine.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A preparation method of liver and gall extract powder comprises the following steps:
s1, weighing 180kg of virgate wormwood herb, adding 180kg of virgate wormwood herb into a hanging basket, controlling the hanging basket to enter an extraction tank, adding 1260L of ethanol, starting a circulating pump in the tank, circularly soaking for 1h, starting an interlayer valve, controlling the water temperature, carrying out heat preservation and circulation extraction at 60 ℃ for 2h, closing the interlayer valve and the circulating pump in the tank after the completion, pumping the liquid medicine into a storage tank, and standing to obtain virgate wormwood herb supernatant; closing the extraction tank opening, opening the condensing device, opening the bottom steam valve, introducing steam into the tank for 30min, and introducing the steam into the ethanol storage tank for recycling;
s2, filtering the virgate wormwood supernatant, concentrating the filtrate under reduced pressure until the relative density is 1.05, stopping concentrating, filtering the concentrated solution by 200 meshes, and pumping the concentrated solution into a storage tank;
s3, opening a valve of a heating layer of the storage tank, keeping the temperature of the liquid medicine at 60 ℃, adding 30kg of hydroxypropyl beta cyclodextrin, and carrying out heat preservation and stirring for 90min;
s4, after stirring, putting the mixture into a continuous vacuum crawler dryer preheated in advance for drying, controlling the drying temperature to be 55-65 ℃ and the drying time to be 4 hours, and crushing the dried mixture by 100 meshes to obtain capillary artemisia alcohol extract powder;
s51, adding 180kg of radix isatidis and 4kg of trehalose into a hanging basket containing virgate wormwood herb residues, controlling the hanging basket to enter an extraction tank, adding 2880L of water, simultaneously opening a circulating pump in the tank, circularly soaking for 1h, heating to boiling, extracting for 2h, and collecting an extracting solution;
s52, continuously adding 2160L of water and 4kg of trehalose into an extraction tank, heating to boil, extracting for 1h, mixing the two extracts to obtain a supernatant, and standing for 1h;
s6, after standing, sucking supernatant fluid, filtering, pumping filtrate into a concentration tank, concentrating under reduced pressure at 55-65 ℃ until the relative density is 1.2, filtering concentrated solution by 200 meshes, pumping the concentrated solution into the storage tank, opening a valve of a heating layer, keeping the temperature of the concentrated solution at 60+/-2 ℃, adding 5kg lactose, and stirring for 30min under heat preservation;
and S7, filtering the concentrated solution by 200 meshes after stirring, putting the concentrated solution into a continuous vacuum crawler-type dryer preheated in advance for drying, controlling the drying temperature to be 55-65 ℃, drying for 4 hours, crushing the dried concentrated solution by 100 meshes, uniformly mixing the crushed concentrated solution with the capillary artemisia alcohol extract powder, and sealing for later use.
Comparative example 1
A preparation method of liver and gall extract powder comprises the following steps:
s1, weighing 180kg of virgate wormwood herb and 180kg of radix isatidis, adding the virgate wormwood herb and the 180kg of radix isatidis into a hanging basket, controlling the hanging basket to enter an extraction tank, adding 2880 liters of water, and simultaneously opening a circulating pump in the tank for circulating soaking for 1h; then, a steam valve is opened to start heating, a circulating pump in the tank is in an open state, the heating is carried out for 2 hours after boiling, the steam valve and the circulating pump are closed after the heating is finished, concentrated solution is pumped into a storage tank, 2160L water is added into the extraction tank, the circulating pump in the tank is opened, the steam valve is opened to carry out secondary extraction, the heating is carried out for 1 hour after boiling, the two extraction solutions are combined, and the mixture is kept stand for 1 hour;
s2, after standing, sucking supernatant fluid, filtering, pumping filtrate into a concentration tank, starting to decompress and concentrate, controlling the concentration temperature between 55 ℃ and 65 ℃, concentrating to a relative density of 1.2, filtering concentrated solution by 200 meshes, pumping the concentrated solution into an alcohol precipitation tank, adding ethanol to ensure that the alcohol content is 60%, standing for 24 hours, filtering supernatant fluid, recovering ethanol, and stopping concentrating when the decompression concentration is performed to the relative density of 1.2;
and S3, filtering the concentrated solution by 200 meshes, putting the filtered concentrated solution into a continuous vacuum crawler-type dryer preheated in advance for drying, controlling the drying temperature to be 55-65 ℃ and the drying time to be 4 hours, crushing the dried concentrated solution by 100 meshes, and sealing for later use.
Comparative example 2
A preparation method of liver and gall extract powder comprises the following steps:
the difference from example 1 is that step S3 is not performed, and the concentrated solution obtained in step S2 is directly dried in step S4 after being filtered; the other steps are the same as in example 1.
Comparative example 3
A preparation method of liver and gall extract powder comprises the following steps:
the only difference from example 1 is in step S6:
s6, sucking supernatant after standing is finished, filtering, pumping filtrate into a concentration tank, concentrating under reduced pressure, controlling the concentration temperature between 55 and 65 ℃, stopping concentrating when the relative density of concentrated solution is 1.02, filtering concentrated solution with 200 meshes, and pumping the concentrated solution into the storage tank.
Example 2
A preparation method of liver and gall extract powder comprises the following steps:
s1, weighing 120kg of herba artemisiae scopariae, adding into a hanging basket, controlling the hanging basket to enter an extraction tank, adding 1200L of ethanol, starting a circulating pump in the tank, circularly soaking for 1h, starting an interlayer valve, controlling the water temperature, carrying out heat preservation and circulation extraction at 55 ℃ for 3h, closing the interlayer valve and the circulating pump in the tank after the completion, pumping the liquid medicine into a storage tank, and standing to obtain herba artemisiae scopariae supernatant; closing the extraction tank opening, opening the condensing device, opening the bottom steam valve, introducing steam into the tank for 30min, and introducing the steam into the ethanol storage tank for recycling;
s2, filtering the virgate wormwood supernatant, concentrating the filtrate under reduced pressure until the relative density is 0.95, stopping concentrating, filtering the concentrated solution by 200 meshes, and pumping the concentrated solution into a storage tank;
s3, opening a valve of a heating layer of the storage tank, keeping the temperature of the liquid medicine at 65 ℃, adding 24kg of hydroxypropyl beta cyclodextrin, and carrying out heat preservation and stirring for 60min;
s4, after stirring, putting the mixture into a continuous vacuum crawler dryer preheated in advance for drying, controlling the drying temperature to be 55-65 ℃ and the drying time to be 4 hours, and crushing the dried mixture by 100 meshes to obtain capillary artemisia alcohol extract powder;
s51, adding 120kg of radix isatidis and 3kg of trehalose into a hanging basket containing capillary artemisia herb residues, controlling the hanging basket to enter an extraction tank, adding 1440L of water, simultaneously opening a circulating pump in the tank, circularly soaking for 1h, heating to boiling, extracting for 2h, and collecting an extracting solution;
s52, continuously adding 1440L of water and 3kg of trehalose into an extraction tank, heating to boil, extracting for 1h, mixing the two extracts to obtain a supernatant, and standing for 1h;
s6, after standing, sucking supernatant fluid, filtering, pumping filtrate into a concentration tank, concentrating under reduced pressure at 55-65 ℃ until the relative density is 1.15, filtering concentrated solution by 200 meshes, pumping the concentrated solution into the storage tank, opening a valve of a heating layer, keeping the temperature of the concentrated solution at 60+/-2 ℃, adding 3.6kg lactose, and carrying out heat preservation and stirring for 30min;
and S7, filtering the concentrated solution by 200 meshes after stirring, putting the concentrated solution into a continuous vacuum crawler-type dryer preheated in advance for drying, controlling the drying temperature to be 55-65 ℃, drying for 4 hours, crushing the dried concentrated solution by 100 meshes, uniformly mixing the crushed concentrated solution with the capillary artemisia alcohol extract powder, and sealing for later use.
Example 3
A preparation method of liver and gall extract powder comprises the following steps:
s1, weighing 200kg of virgate wormwood herb, adding 200kg of virgate wormwood herb into a hanging basket, controlling the hanging basket to enter an extraction tank, adding 1600L of ethanol, starting a circulating pump in the tank, circularly soaking for 1h, starting an interlayer valve, controlling the water temperature, carrying out heat preservation and circular extraction at 65 ℃ for 1.5h, closing the interlayer valve and the circulating pump in the tank after the completion, pumping the liquid medicine into a storage tank, and standing to obtain virgate wormwood herb supernatant; closing the extraction tank opening, opening the condensing device, opening the bottom steam valve, introducing steam into the tank for 30min, and introducing the steam into the ethanol storage tank for recycling;
s2, filtering the virgate wormwood supernatant, concentrating the filtrate under reduced pressure until the relative density is 1.15, stopping concentrating, filtering the concentrated solution by 200 meshes, and pumping the concentrated solution into a storage tank;
s3, opening a valve of a heating layer of the storage tank, keeping the temperature of the liquid medicine at 55 ℃, adding 40kg of hydroxypropyl beta cyclodextrin, and carrying out heat preservation and stirring for 120min;
s4, after stirring, putting the mixture into a continuous vacuum crawler dryer preheated in advance for drying, controlling the drying temperature to be 55-65 ℃ and the drying time to be 4 hours, and crushing the dried mixture by 100 meshes to obtain capillary artemisia alcohol extract powder;
s51, adding 200kg of radix isatidis and 5kg of trehalose into a hanging basket containing virgate wormwood herb residues, controlling the hanging basket to enter an extraction tank, adding 3200L of water, simultaneously opening a circulating pump in the tank, circularly soaking for 1h, heating to boiling, extracting for 2h, and collecting an extracting solution;
s52, continuously adding 2400L of water and 5kg of trehalose into the extraction tank, heating to boil, extracting for 1h, mixing the two extracts to obtain a supernatant, and standing for 1h;
s6, after standing, sucking supernatant fluid, filtering, pumping filtrate into a concentration tank, concentrating under reduced pressure at 55-65 ℃ until the relative density is 1.25, filtering concentrated solution with 200 meshes, pumping the concentrated solution into the storage tank, opening a valve of a heating layer, keeping the temperature of the concentrated solution at 60+/-2 ℃, adding 6kg lactose, and stirring for 30min under heat preservation;
and S7, filtering the concentrated solution by 200 meshes after stirring, putting the concentrated solution into a continuous vacuum crawler-type dryer preheated in advance for drying, controlling the drying temperature to be 55-65 ℃, drying for 4 hours, crushing the dried concentrated solution by 100 meshes, uniformly mixing the crushed concentrated solution with the capillary artemisia alcohol extract powder, and sealing for later use.
And (3) experimental detection:
the liver and gall extract powder obtained through experiments is subjected to conversion of the proportion of raw materials, and is detected according to the following detection method (refer to traditional Chinese medicine rolls of the 2017 edition of veterinary quality standard):
dissolving 30g of extract powder of raw materials in 200mL of hot water under stirring, and observing immediately, wherein all the extract powder should be dissolved, and no foreign matters such as coke dust can be seen.
[ herba Artemisiae Scopariae identification ] taking extract powder containing 15g of raw materials, adding 30mL of ethanol, performing ultrasonic treatment for 20min, filtering, evaporating filtrate to dryness, and dissolving the residue with 2mL of ethanol to obtain test solution. 2g of herba Artemisiae Scopariae control is prepared into a control solution. According to a thin layer chromatography test, 5uL of each of the two solutions is absorbed and respectively spotted on the same silica gel G thin layer plate, petroleum ether (60-90 ℃) and ethyl acetate-acetone (5:3:2) are taken as developing agents, and the developing agents are developed, taken out, dried and sprayed with 5% potassium hydroxide ethanol solution and then are detected under an ultraviolet lamp (365 nm). In the chromatogram of the test sample, fluorescent spots of the same color are displayed at positions corresponding to those of the chromatogram of the control drug.
[ Arg identification ] taking extract powder containing 6.0g of raw medicinal material, adding 20mL of diluted ethanol, performing ultrasonic treatment for 20min, filtering, evaporating filtrate to dryness, and adding 1mL of diluted ethanol into residue to dissolve, thereby obtaining a sample solution. And adding diluted ethanol into arginine reference substance to obtain a solution containing 0.5mg per 1mL, and taking the solution as reference substance solution. According to a thin layer chromatography (appendix 0502), 1-2 mu L of each of the two solutions is sucked and respectively spotted on the same silica gel G thin layer plate, the mixture is spread by taking n-butanol-glacial acetic acid-water (19:5:5) as a spreading agent, taken out, dried by hot air, sprayed with ninhydrin test solution, and heated at 105 ℃ until the spots develop clearly. Spots of the same color appear in the sample chromatogram at positions corresponding to those of the control chromatogram.
Table 1 experimental test results
Experimental comparison Solubility of Capillary artemisia identification Arginine identification Remarks
Example 1 Completely dissolve Consistent with control Consistent with control Qualified product
Comparative example 1 Completely dissolve Spot color inconsistency Consistent with control Failure to pass
Comparative example 2 With insoluble substances Consistent with control Consistent with control Failure to pass
Comparative example 3 Completely dissolve Consistent with control With tailing phenomenon Failure to pass
The result of the solubility test is shown in FIG. 2, and the solution is dark, and the lower layer liquid is taken out to be diluted and observed after the liquid is stood, as shown in the right graph of FIG. 2. The liver and gall extract powder capillary artemisia identification thin-layer chromatograms are shown in figure 3, and correspond to the example 1, the comparative example 2, the comparative example 3 and capillary artemisia reference substances respectively from left to right and from 1 to 5. The liver and gall extract powder arginine thin layer identification patterns are shown in figure 4, and correspond to the example 1, the comparative example 2, the comparative example 3 and the arginine reference substances respectively from left to right and from 1 to 5.
In the preparation method of the comparative example 1, the isatis root and the virgate wormwood herb are extracted together, the solubility is qualified, but when the virgate wormwood herb is identified, the quantity and the color of fluorescent spots are inconsistent with those of the reference medicinal material, and the arginine identification has no tail. In comparative example 2, hydroxypropyl beta cyclodextrin was not added during the concentration of herba Artemisiae Scopariae, and the solubility was poor and insoluble substances were contained. In comparative example 3, lactose was not added during the concentration of isatis root, and tailing was identified by arginine. Example 1 of the present invention can solve the problems of solubility, capillary artemisia identification and arginine identification at the same time.
Table 1 shows only the results of the study of example 1, and solubility, capillary artemisia identification, and arginine identification performance tests were also performed for other examples, and the test results were the same as those of example 1, and therefore omitted.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.

Claims (10)

1. The preparation method of the water-soluble liver and gall extract powder is characterized by comprising the following steps of:
s1, extracting herba Artemisiae Scopariae with ethanol to obtain herba Artemisiae Scopariae supernatant and herba Artemisiae Scopariae residue;
s2, concentrating the virgate wormwood supernatant under reduced pressure, and filtering to obtain filtrate;
s3, heating the filtrate to 55-65 ℃, adding hydroxypropyl beta cyclodextrin, and preserving heat for 1-2h;
s4, drying and crushing to obtain capillary artemisia alcohol extract powder;
s5, adding radix isatidis and trehalose into the capillary artemisia herb residue, mixing and extracting with water to obtain a supernatant;
s6, concentrating the supernatant under reduced pressure, filtering, drying, crushing, and uniformly mixing with the capillary artemisia alcohol extract powder to obtain water-soluble liver and gall extract powder.
2. The method for preparing water-soluble liver and gall extract powder according to claim 1, wherein the step S6 is specifically:
concentrating the supernatant under reduced pressure, filtering, heating to 55-65deg.C, adding lactose, maintaining the temperature for 0.5-1 hr, oven drying, pulverizing, and mixing with the ethanol extract powder of herba Artemisiae Scopariae to obtain water-soluble liver and gallbladder extract powder.
3. The method for preparing the water-soluble liver and gall extract powder according to claim 2, which is characterized by comprising the following steps:
s1, adding 1200-1600L of ethanol into 120-200kg of herba Artemisiae Scopariae, and extracting with ethanol to obtain herba Artemisiae Scopariae supernatant and herba Artemisiae Scopariae residue;
s2, concentrating the virgate wormwood supernatant under reduced pressure, and filtering to obtain filtrate;
s3, heating the filtrate to 55-65 ℃, adding 24-40kg of hydroxypropyl beta cyclodextrin, and preserving heat for 1-2h;
s4, drying and crushing to obtain capillary artemisia alcohol extract powder;
s5, adding 120-200kg of radix isatidis and 6-10kg of trehalose into the capillary artemisia herb residue, mixing and extracting with water to obtain supernatant;
s6, concentrating the supernatant under reduced pressure, filtering, heating to 55-65 ℃, adding 3.6-6kg lactose, preserving heat for 0.5-1h, drying, crushing, and uniformly mixing with the capillary artemisia alcohol extract powder to obtain water-soluble liver and gall extract powder.
4. The method for preparing water-soluble liver and gall extract powder according to claim 3, wherein the step S5 is specifically:
s51, adding 120-200kg of radix isatidis and 3-5kg of trehalose into the capillary artemisia herb residue, mixing, adding 1440-3200L of water, heating to boiling for one-time extraction, and collecting an extracting solution;
s52, continuously adding 1440-2400L of water and 3-5kg of trehalose into the residues, heating to boiling for secondary extraction, and mixing the two extracts to obtain a supernatant.
5. The method according to claim 4, wherein in the step S51, water is added and then soaked for 1-2 hours.
6. The method for preparing water-soluble liver and gall extract powder according to claim 1, wherein in the step S1, alcohol is soaked in ethanol for 1h in advance.
7. The method for preparing water-soluble liver and gall extract powder according to claim 1, wherein in the step S1, the alcohol extraction temperature is 55-65 ℃ and the time is 1.5-3h.
8. The method for preparing water-soluble liver and gall extract powder according to claim 1, further comprising any one of the following characteristics:
in the step S2, the mixture is concentrated to the relative density of 0.95-1.15 under reduced pressure;
in the step S6, the mixture is concentrated to the relative density of 1.15-1.25 under reduced pressure.
9. The method for preparing water-soluble liver and gall extract powder according to claim 1, wherein in the step S4 and the step S6, the drying is carried out in a continuous vacuum crawler-type dryer, and the temperature is controlled to be 55-65 ℃ for 4 hours.
10. The method for preparing water-soluble liver and gall extract powder according to claim 1, further comprising any one of the following characteristics:
in the step S2 and the step S6, the filtration is 200-mesh filtration;
in the step S4 and the step S6, 100 meshes of crushed powder are dried.
CN202310230836.XA 2023-03-11 2023-03-11 Preparation method of water-soluble liver and gall extract powder Pending CN116036144A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101849980A (en) * 2010-06-08 2010-10-06 江西中成药业集团有限公司 Particle for treating liver and gall diseases and preparation method thereof
CN102091299A (en) * 2007-08-03 2011-06-15 北京亚东生物制药有限公司 Method for detecting medicinal composition for treating viral hepatitis

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102091299A (en) * 2007-08-03 2011-06-15 北京亚东生物制药有限公司 Method for detecting medicinal composition for treating viral hepatitis
CN101849980A (en) * 2010-06-08 2010-10-06 江西中成药业集团有限公司 Particle for treating liver and gall diseases and preparation method thereof

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