CN115006355B

CN115006355B - Preparation method of veterinary coptis chinensis granules with full-component extraction

Info

Publication number: CN115006355B
Application number: CN202210898424.9A
Authority: CN
Inventors: 田继业; 张世显; 安卓娜; 王佳琪; 韩愈杰; 邵谱; 牛婵娟; 王孟
Original assignee: Baoding Jizhong Pharmaceutical Co ltd; BAODING YANGGUANG BENCAO PHARM; Baoding Jizhong Biotechnology Co ltd
Current assignee: Baoding Jizhong Pharmaceutical Co ltd; BAODING YANGGUANG BENCAO PHARM; Baoding Jizhong Biotechnology Co ltd
Priority date: 2022-07-28
Filing date: 2022-07-28
Publication date: 2023-02-10
Anticipated expiration: 2042-07-28
Also published as: CN115006355A

Abstract

The invention discloses a preparation method of veterinary coptis chinensis granules by full-ingredient extraction, which comprises the following steps: s1, adding water into fresh purslane to prepare pulp, filtering and centrifuging the pulp, taking supernate, concentrating the supernate, drying the concentrated liquid under reduced pressure, and crushing the dried liquid to prepare dry powder A; s2, percolating herba andrographitis, chinese pulsatilla root, myrobalan and ash bark with ethanol, and performing spray drying to obtain ethanol extraction dry powder B; s3, adding the medicinal materials percolated in the step S2 into an extraction tank, adding garden burnet, liquorice and scutellaria baicalensis, carrying out water extraction, and carrying out spray drying to obtain water extraction dry powder C; and S4, uniformly mixing various dry powders, cane sugar and dextrin, and granulating by using a dry-method granulator to obtain the sugar-free starch. The preparation method of the veterinary coptis chinensis particle with the full-component extraction is adopted, so that the active ingredients in the medicine are extracted to the maximum extent, the biological activity of the fresh purslane can be greatly improved, a large amount of effective active ingredients are reserved, the loss in the processing process is low, and the prepared finished product coptis chinensis particle has a good dysentery stopping effect.

Description

Preparation method of veterinary lotus seed and coptis chinensis granules with full-ingredient extraction

Technical Field

The invention relates to the technical field of medicine extraction, and particularly relates to a preparation method of veterinary lotus seed and coptis chinensis granules extracted from all components.

Background

At present, the traditional Chinese medicine granules are generally prepared by an aqueous extraction and concentration preparation method, however, the problem of effective transfer of active ingredients of medicinal materials is ignored in the preparation process. Some medicinal materials, especially purslane, can obtain better treatment effect when being fresh, and the active protein can be denatured and inactivated after the medicinal materials are subjected to the production steps of sun curing, steaming, airing, decocting, concentrating and the like, so that the due curative effect cannot be achieved.

In both literature reports and practical applications, the dysentery stopping effect of fresh purslane is superior to that of purslane extracted after being steamed, aired and decocted. How to obtain more comprehensive medicinal components at lower temperature is an urgent problem to be solved in the fresh purslane medicament processing technology.

For other Chinese herbal medicines, which contain both fat-soluble ingredients and water-soluble ingredients, the dissolution of the active ingredients of the two ingredients are mutually influenced, so that the conversion efficiency of the single decoction extraction of the fat-soluble active ingredients is low, and the efficacy of the final product is not ideal.

Disclosure of Invention

The invention aims to provide a preparation method of veterinary coptis chinensis granules extracted from all components, which is simple to operate, enhances the drug effect of fresh drugs, improves the water extraction and transfer rate of esters, oleates and triterpenes, and optimizes the single extraction step of alkaloid so that active components in the veterinary coptis chinensis granules are transferred to a final product to the maximum extent.

In order to realize the purpose, the invention provides a preparation method of veterinary lotus seed and coptis root granules by full-ingredient extraction, which comprises the following steps:

s1, cleaning collected fresh purslane, adding water to prepare pulp, filtering, centrifuging, taking supernate, concentrating the supernate through an RO reverse osmosis membrane, drying the concentrated liquid at 60 ℃ under reduced pressure, and crushing to prepare dry powder A;

s2, percolating herba andrographitis, chinese pulsatilla root, myrobalan and ash bark with ethanol, recovering ethanol from percolate until no ethanol smell exists, and performing spray drying to obtain ethanol extraction dry powder B;

s3, adding the medicinal materials percolated in the step S2 into a traditional Chinese medicine extraction tank, adding garden burnet, liquorice and scutellaria baicalensis, carrying out water extraction, and carrying out spray drying to obtain water extraction dry powder C;

and S4, uniformly mixing the dry powder A, the dry powder B, the dry powder C, the cane sugar and the dextrin, and granulating by using a dry granulating machine to obtain the powder.

Preferably, in step S1, the amount of pure water added is 2 times of the mass of fresh purslane, the filter screen is 200 meshes, the centrifugation rate is 3000r/min, and the concentration ratio of the supernatant concentrated by the RO reverse osmosis membrane is 4.

Preferably, in step S2, the common andrographis herb, the Chinese pulsatilla root, the myrobalan and the ash bark are subjected to percolation extraction by 70-75% of ethanol solution; the air inlet temperature of the spray drying is 165 ℃, and the air outlet temperature is 80 ℃.

Preferably, in step S3, the sanguisorba officinalis and the licorice are added into a traditional Chinese medicine extraction tank in which the percolated medicinal materials are added, water with the amount of 10 times of the mass of the medicinal materials is added firstly, the scutellaria baicalensis is added when the temperature is heated to 80 ℃, the temperature is raised to 100 ℃, the reflux dynamic extraction is carried out, and the extraction is carried out for 2 hours.

Preferably, after the primary extraction, adding water with the weight of 8 times of that of the medicinal materials, heating to 100 ℃, and performing reflux dynamic extraction for 2 hours;

collecting extractive solution, concentrating to relative density of 1.10, and filtering with 200 mesh filter cloth;

the air inlet temperature of the spray drying is 180 ℃, and the air outlet temperature is 80 ℃.

Preferably, in step S4, the mass ratio of sucrose to dextrin is 3.

Therefore, the veterinary lotus seed yellow particles prepared by the preparation method of the full-ingredient extracted veterinary lotus seed yellow particles contain active protein ingredients of purslane and a plurality of fat-soluble and water-soluble medicinal ingredients, so that the loss of active ingredients of traditional Chinese medicinal materials in processing is reduced, the use effect of final products is improved, and a feasible reference method is provided for extraction of full ingredients of other traditional Chinese medicines.

The specific technical effects are as follows:

(1) The process can effectively avoid the damage effect of high temperature on the purslane active protein, furthest preserves various components in the purslane, has small processing loss, reduces the requirements of purslane medicinal materials on weather and humidity in airing, and reduces mould infection. Most of effective components can be intercepted by adopting the RO reverse osmosis membrane concentration, the energy consumption is low, and the concentration efficiency is improved.

(2) The invention percolates part of the medicinal materials containing more ester-soluble components by 70-75% ethanol, and then decocts the medicinal materials by water, wherein the medicine adding sequence and the medicine adding time of the medicinal materials containing organic acid and the medicinal materials containing alkaloid improve the transfer rate of effective components.

(3) The scutellaria baicalensis is rich in various alkaloids, and the alkaloid has higher transfer rate in the solution containing the organic acid. The radix sanguisorbae and the liquorice which are rich in organic acid assist in extracting the scutellaria baicalensis by water, so that the impurity removal step is omitted, the rotation of the two parties is promoted, and the drug effect is improved.

(4) The process for extracting the total components only carries out post-treatment such as filtering, spraying and the like, reduces the loss of the effective components in the post-treatment process, and retains the effective components to the maximum extent in the final product to play the maximum role.

(5) The sum of the dry powder B and the dry powder C obtained by the preparation method is far larger than the direct extraction amount.

(6) Compared with clinical application, the particle product prepared by the preparation method of the invention has obviously improved curative efficiency and effective rate.

The technical solution of the present invention is further described in detail by the following examples.

Detailed Description

The technical solution of the present invention is further illustrated by the following examples.

Example one

A preparation method of veterinary lotus seed and coptis granules with full component extraction comprises the following steps:

s1, taking 240kg of fresh purslane, cleaning to remove impurities such as silt, cutting into pieces with the length of about 1cm, putting the pieces into a pulping machine, and adding 480kg of purified water to prepare pulp; filtering with 200 mesh filter cloth, collecting filtrate, filtering with disc centrifuge, and collecting supernatant; concentrating the supernatant with RO reverse osmosis membrane, collecting concentrated water, controlling the ratio of the concentrated water to the discarded water to be 1.

S2, weighing 18kg of common andrographis herb, 18kg of Chinese pulsatilla root, 12kg of myrobalan and 12kg of ash bark, adding 600kg of 75% ethanol for percolation, collecting percolate, recovering ethanol under reduced pressure at 70 ℃ until no alcohol smell exists, carrying out spray drying, wherein the air inlet temperature is 165 ℃ and the air outlet temperature is 80 ℃ to obtain 3.4kg of alcohol extraction dry powder B.

S3, adding 1260kg of water into the percolated medicinal materials in the step S2, then adding 12kg of garden burnet and 12kg of liquorice, heating to 80 ℃, adding scutellaria baicalensis, heating to 100 ℃, performing reflux dynamic extraction, and extracting for 2 hours; adding 1040kg of water, heating to 100 ℃, refluxing and dynamically extracting for 2 hours; collecting the two extractive solutions, concentrating to relative density of 1.10, filtering with 200 mesh filter cloth, spray drying at air inlet temperature of 180 deg.C and air outlet temperature of 80 deg.C to obtain dry powder C (8.5 kg).

S4, adding 64.125kg of cane sugar and 21.375kg of dextrin into the mixture of the dry powder A, the dry powder B and the dry powder C, placing the mixture into a trough-shaped mixing machine, mixing for 15 minutes, and granulating by using a dry granulating machine to obtain 100kg of lotus seed yellow granules.

Example two

s1, taking 240kg of fresh purslane, cleaning to remove impurities such as silt, cutting into pieces with the length of about 1cm, putting the pieces into a pulping machine, adding 480kg of purified water, and preparing into pulp. Filtering with 200 mesh filter cloth, collecting filtrate, filtering with disc centrifuge, and collecting supernatant; concentrating the supernatant with RO reverse osmosis membrane, collecting concentrated water, controlling the ratio of the concentrated water to the discarded water to be 1.

S2, weighing 18kg of common andrographis herb, 18kg of Chinese pulsatilla root, 12kg of myrobalan and 12kg of ash bark, adding 600kg of 70% ethanol for percolation, collecting percolate, recovering ethanol at 70 ℃ under reduced pressure until no ethanol smell exists, performing spray drying, and preparing ethanol extraction dry powder B at 165 ℃ air inlet temperature and 80 ℃ air outlet temperature, wherein 3.4kg of ethanol extraction dry powder B is prepared.

S3, adding 1260kg of water into the percolated medicinal materials in the step S2, then adding 12kg of garden burnet and 12kg of liquorice, heating to 80 ℃, adding 18kg of scutellaria baicalensis, heating to 100 ℃, performing reflux dynamic extraction, and extracting for 2 hours; adding 1040kg of water, heating to 100 ℃, refluxing and dynamically extracting for 2 hours; collecting the two extractive solutions, concentrating to relative density of 1.10, filtering with 200 mesh filter cloth, spray drying at air inlet temperature of 180 deg.C and air outlet temperature of 80 deg.C to obtain dry powder C (8.5 kg);

and S4, adding 64.125kg of cane sugar and 21.375kg of dextrin into the mixture of the dry powder A, the dry powder B and the dry powder C, placing the mixture into a trough-shaped mixer, mixing for 15 minutes, and granulating by using a dry granulator to obtain 100kg of coptis chinensis granules.

Comparative example 1

(2017 edition animal remedy quality standard Chinese medicine roll preparation method)

A preparation method of veterinary coptis chinensis granules comprises the following steps:

s1, taking 18kg of scutellaria baicalensis, adding purified water, decocting for 2 times, mixing decoctions, filtering, adjusting the pH of the collected filtrate to be =1-2 by using hydrochloric acid, heating to 80 ℃, keeping the temperature for 30 minutes, standing and centrifuging; adding water into the precipitate, stirring, adjusting pH to =7 with 40% sodium hydroxide, adding appropriate amount of ethanol, filtering, adding hydrochloric acid into the collected filtrate to adjust pH to =1-2, stirring, heating to 80 deg.C, keeping the temperature for 30 min, and filtering; washing the precipitate with 50% ethanol, and drying at 60 deg.C under reduced pressure to obtain Scutellariae radix powder 0.18 kg.

S2, weighing 18kg of common andrographis herb, 18kg of Chinese pulsatilla root, 12kg of myrobalan, 12kg of ash bark, 12kg of garden burnet root, 12kg of liquorice and 24kg of purslane, adding water, decocting for 2 times, mixing decoctions, filtering, concentrating the filtrate to obtain clear paste with the relative density of 1.32 (70-80 ℃), and preparing 18kg of clear paste.

And S3, adding the radix scutellariae powder, uniformly mixing with 70.365kg of sucrose powder and 23.455kg of dextrin, granulating, drying under reduced pressure at 65 ℃, and finishing granules to obtain 100kg of coptis chinensis granules.

Comparative example No. two

s1, adding purified water with the mass being 10 times that of 24kg of purslane, decocting for 2 times, mixing decoctions, concentrating to the relative density of 1.15-1.18, and performing spray drying to obtain 1.7kg of dry powder A in total.

And S4, adding 64.8kg of cane sugar and 21.6kg of dextrin into the mixture of the dry powder A, the dry powder B and the dry powder C, placing the mixture into a groove-shaped mixing machine, mixing for 15 minutes, and granulating by using a dry granulating machine to obtain 100kg of coptis chinensis granules.

Comparative example No. three

S2, weighing 18kg of common andrographis herb, 18kg of Chinese pulsatilla root, 12kg of myrobalan and 12kg of ash bark, adding 600kg of 50% ethanol for percolation, collecting percolate, recovering ethanol at 70 ℃ under reduced pressure until no ethanol smell exists, performing spray drying, and preparing ethanol extraction dry powder B at 165 ℃ of air inlet temperature and 80 ℃ of air outlet temperature, wherein the total amount is 1.2kg.

S3, adding 1260kg of water into the percolated medicinal materials in the step S2, then adding 12kg of garden burnet and 12kg of liquorice, adding scutellaria baicalensis when heating to 80 ℃, heating to 100 ℃, performing reflux dynamic extraction, and extracting for 2 hours; adding 1040kg of water, heating to 100 ℃, refluxing and dynamically extracting for 2 hours; collecting the two extractive solutions, concentrating to relative density of 1.10, filtering with 200 mesh filter cloth, spray drying at air inlet temperature of 180 deg.C and air outlet temperature of 80 deg.C to obtain dry powder C (8.6 kg).

And S4, adding 66.375kg of cane sugar and 22.125kg of dextrin into the mixture of the dry powder A, the dry powder B and the dry powder C, placing the mixture into a groove-shaped mixer, mixing for 15 minutes, and granulating by using a dry granulator to obtain 100kg of coptis chinensis granules.

Comparative example No. four

s1, weighing 24kg of purslane, adding purified water with the mass being 10 times that of the purslane, decocting for 2 times, mixing decoctions, concentrating to the relative density of 1.15-1.18, and performing spray drying to obtain 1.7kg of dry powder A.

S2, weighing 18kg of common andrographis herb, 18kg of Chinese pulsatilla root, 12kg of myrobalan, 12kg of ash bark, 12kg of garden burnet root and 12kg of liquorice, adding 840kg of 70% ethanol for percolation, collecting percolate, recovering ethanol under reduced pressure at 70 ℃ until no alcohol smell exists, and carrying out spray drying at the air inlet temperature of 165 ℃ and the air outlet temperature of 80 ℃ to obtain 3.2kg of dry alcohol extraction powder B.

S3, adding 1260kg of water into the percolated medicinal materials in the step S2, adding the scutellaria baicalensis when the temperature is heated to 80 ℃, heating to 100 ℃, performing reflux dynamic extraction, and extracting for 2 hours; adding 1040kg of water, heating to 100 ℃, refluxing and dynamically extracting for 2 hours; collecting the two extractive solutions, concentrating to relative density of 1.10, filtering with 200 mesh filter cloth, spray drying at air inlet temperature of 180 deg.C and air outlet temperature of 80 deg.C to obtain dry powder C (4.6 kg).

And S4, adding 67.875kg of sucrose and 22.625kg of dextrin into the mixture of the dry powder A, the dry powder B and the dry powder C, placing the mixture into a groove-shaped mixer, mixing for 15 minutes, and granulating by using a dry granulator to obtain 100kg of coptis chinensis granules.

Experimental testing

2000 white feather broilers of 35 days old are selected, the white feather broilers are naturally attacked, yellow mucus-containing excrement is obvious, loose excrement is adhered to the anus, feed is obvious, and the anus is red and swollen. The veterinary clinical diagnosis is summer heat damp heat dysentery, and the Chinese medicinal granules are clinically applicable.

Randomly divided into 8 groups of 250 chickens each. The groups are blank control group, drug control group, example group, comparative example group, and comparative example group. The blank control group was not added with any drug, the drug control group was given with 20% neomycin sulfate soluble powder 0.125g per chicken per day, the other groups were given with the corresponding lotus yellow granules, and each chicken was given 0.25g per day. After 5 days of continuous use, feces, feed intake and death were observed.

TABLE 1 Table of white feather broilers of different groups

As a result, the results of the first and second examples are superior to those of the comparative example in both the dry powder drug yield and the clinical use effect. The veterinary coptis chinensis particle adopts the fresh purslane in the preparation process, and the protein is not denatured at high temperature in the processing process, so the dysentery stopping effect is obviously better than that of the dry purslane by decoction. And the method adopts the steps of firstly percolating the alcohol with proper concentration according to varieties and then decocting the alcohol with water for extraction, so that the antibacterial and toxin expelling effects are improved. In addition, the sanguisorba and the liquorice are added firstly, and then the scutellaria is added at 80 ℃, so that the method effectively increases the powder yield of the three medicines and obviously improves the effect of astringing intestines to stop diarrhea.

Therefore, the preparation method of the veterinary coptis chinensis granules extracted from all components is simple to operate, and has the characteristics of adopting different extraction methods according to different medicines, retaining effective medicinal components to the maximum extent, reducing impurity removal, improving the conversion rate and the like. Not only the components which are easy to be damaged by high temperature are obtained, but also the fat-soluble and water-soluble components are increased, and the content of organic acid and alkaloid in the finished product is increased, so the method has the characteristics of full components and obtains better clinical application effect.

Finally, it should be noted that: the above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.

Claims

1. A preparation method of veterinary lotus seed and coptis chinensis granules extracted from all components is characterized by comprising the following steps:

s1, cleaning 240kg of collected fresh purslane, adding water for pulping, filtering, centrifuging, taking supernate, concentrating the supernate through an RO reverse osmosis membrane, drying the concentrated liquid under reduced pressure in an environment at 60 ℃, and crushing to obtain dry powder A;

s2, percolating and extracting 18kg of common andrographis herb, 18kg of Chinese pulsatilla root, 12kg of myrobalan and 12kg of ash bark by using 70-75% ethanol solution, recovering ethanol from percolate until no alcohol smell exists, and performing spray drying to obtain dry alcohol extract powder B, wherein the air inlet temperature of the spray drying is 165 ℃ and the air outlet temperature is 80 ℃;

s3, adding the percolated medicinal materials in the step S2 into a traditional Chinese medicine extraction tank, adding 12kg of garden burnet and 12kg of liquorice, heating to 80 ℃, adding 18kg of scutellaria baicalensis, heating to 100 ℃, performing reflux dynamic extraction for 2 hours, and performing spray drying to obtain water extraction dry powder C;

2. The preparation method of the full ingredient extracted veterinary coptis chinensis granules according to claim 1, which is characterized by comprising the following steps of: in the step S1, pure water is added in an amount which is 2 times of the mass of the fresh purslane, a filter screen is 200 meshes, the centrifugal rate is 3000r/min, and the concentration ratio of supernatant concentrated by an RO reverse osmosis membrane is 4.

3. The preparation method of the full ingredient extracted veterinary coptis chinensis granules according to claim 2, characterized by comprising the following steps: after the primary extraction, adding water with the weight of 8 times that of the medicinal materials, heating to 100 ℃, and performing reflux dynamic extraction for 2 hours;

4. The preparation method of the full ingredient extracted veterinary coptis chinensis granules according to claim 1, which is characterized by comprising the following steps of: in step S4, the mass ratio of sucrose to dextrin is 3.