CN113082069A - Novel process for preparing single square sweet wormwood powder for chicken - Google Patents
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Abstract
The invention provides a novel process for preparing single square artemisia apiacea powder for chickens, and relates to the technical field of veterinary medicines. The novel process for preparing the sweet wormwood powder for the mono-square chicken comprises the following steps: 1) selecting a sweet wormwood medicinal material, and coarsely crushing; 2) extracting the sweet wormwood herb material, concentrating the sweet wormwood herb material into paste under reduced pressure, extracting the sweet wormwood herb material for three times, combining extracting solutions, filtering the extracting solutions, and then concentrating the extracting solutions under reduced pressure into paste; 3) mixing the prepared paste with auxiliary materials, granulating and sieving, wherein the mass ratio of the auxiliary materials to the paste is 1: 1; 4) drying, granulating, pulverizing, and packaging. The single-component powder has the characteristics of rapid action, convenient administration, safety and effectiveness, can directly act on focus, reduces gastrointestinal mucosa injury, and plays a role in killing coccidium.
Description
Technical Field
The invention relates to the technical field of veterinary drugs, in particular to a novel process for preparing single square artemisia apiacea powder for chickens.
Background
The existing products for treating the coccidiosis in chicken, which are introduced in the markets at home and abroad, mainly comprise compound powder (pulvis) and oral liquid. The main components of the oral liquid are chemical drugs, namely water-soluble antibiotic drugs, which have short administration period and quick response, but have serious residue problem and need a long withdrawal period; the powder (pulvis) is mainly a traditional Chinese veterinary medicine product in the domestic market, most of the products are insoluble in water, and can be administered in a mode of mixing feed with feed, so that the effect of preventing and treating chicken coccidiosis can be achieved, but the administration period is longer.
Because the sweet wormwood extract, namely sweet wormwood extract, has high viscosity and strong hygroscopicity, the content of artemisinin is higher for clinical application, and dilution and dispersion and reduction of hygroscopicity are needed.
The artemisia apiacea powder prepared by the existing preparation process has long acting period, low artemisia apiacea extraction rate and higher manufacturing cost.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a novel process for preparing the sweet wormwood powder for the mono-square chicken, and solves the problems of long action cycle, low sweet wormwood extraction rate and higher manufacturing cost of the sweet wormwood powder prepared by the existing preparation process.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a new process for preparing the sweet wormwood powder for the mono-square chicken comprises the following steps:
1) selecting a sweet wormwood medicinal material, and coarsely crushing;
2) extracting herba Artemisiae Annuae, and concentrating under reduced pressure to obtain extract
Extracting for three times, mixing the extractive solutions, filtering, and concentrating under reduced pressure to obtain extract;
3) mixing the obtained paste with adjuvants, granulating, and sieving
The mass ratio of the auxiliary materials to the paste is 1: 1;
4) drying, granulating, pulverizing, and packaging.
Preferably, the sweet wormwood herb in the step 1) is a processed sweet wormwood herb, and the sweet wormwood herb is coarsely ground and then screened by a second sieve.
Preferably, the amount of the extract added in the step 2) is 6:4:4 times, the extract is extracted for three times, 2 hours for the first time, 1.5 hours for the second time and 1 hour for the third time at the temperature of 60-90 ℃, and the mass ratio of the extract to the sweet wormwood herb is 1:1 ratio.
Preferably, the 2) is added with the amount of the extract liquid being 6:4:4 times, the extract liquid is extracted for three times, the first time is 2 hours, the second time is 1.5 hours, and the third time is 1 hour at the temperature of below 55 ℃, and the mass ratio of the extract liquid to the sweet wormwood herb material is 1:1 ratio.
Preferably, the extracting solution is petroleum ether.
Preferably, the auxiliary material in 3) is silicon dioxide, and the mixing time is 60 minutes.
Preferably, the sieving in 3) is as follows: sieving with 12 mesh sieve, and granulating.
Preferably, the drying temperature of the 4) is 50-55 ℃, and after drying, the granules are sieved by a 10-mesh sieve.
(III) advantageous effects
The invention provides a novel process for preparing single square sweet wormwood powder for chickens. The method has the following beneficial effects:
1. the novel process for preparing the single-square artemisia apiacea powder for the chicken has the characteristics of quick action, convenient administration, safety and effectiveness, can directly act on focus, reduces gastrointestinal mucosa injury, and plays a role in killing coccidium.
Drawings
FIG. 1 is a flow chart of the new process of the present invention;
FIG. 2 is a graph showing the effect of the first extraction of sweet wormwood herb coarse powder and petroleum ether according to the present invention;
FIG. 3 is a graph showing the effect of the second extraction of sweet wormwood herb coarse powder and petroleum ether according to the present invention;
FIG. 4 is a graph showing the effect of the third extraction rate of sweet wormwood herb coarse powder and petroleum ether;
FIG. 5 is a time chart of the extraction of artemisinin by petroleum ether according to the invention;
FIG. 6 is a temperature diagram of the extraction of artemisinin by petroleum ether according to the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
the embodiment of the invention provides a novel process for preparing single square artemisia apiacea powder for chickens, which comprises the following steps: weighing 3000g of sweet wormwood herb coarse powder according to the formula amount, weighing three parts, adding petroleum ether according to the ratio of 6:4:4, extracting for three times at the temperature of below 55 ℃, extracting for 2 hours for the first time, 1.5 hours for the second time and 1 hour for the third time, combining extracting solutions, filtering, recovering a solvent from a filtrate, concentrating under reduced pressure to obtain an ointment, and adding silicon dioxide according to the ratio of 1: 1;
extracting with 1:1 petroleum ether extract;
taking extract extracted from sweet wormwood as a main drug, selecting silicon dioxide as an auxiliary material, mixing and granulating according to a ratio of 1:1, sieving with a 12-mesh sieve, drying at low temperature, crushing after finishing granules, and bagging; the ratio of the extract to the auxiliary materials is 1:1, and the mixing time is 60 minutes, which is the best mixing condition of the forming process;
mixing with silicon dioxide at a ratio of 1:1, granulating, sieving with 12 mesh sieve, drying at 55 deg.C, granulating, pulverizing, and packaging, wherein the ratio of extract to adjuvant is 1:1, and the mixing time is 60 min.
Example two:
the embodiment of the invention provides a novel process for preparing single square artemisia apiacea powder for chickens, which comprises the following steps: weighing 31250g of processed herba Artemisiae Annuae, pulverizing into coarse powder, and sieving with a second sieve;
preparing an extract, namely crushing 5 times of a medicinal material sweet wormwood herb into a coarse powder fruit sieve, adding petroleum ether (60-90 ℃) for extraction for three times, wherein the amount of the petroleum ether is 6 times of that of the first time, and extracting for 2 hours; extracting for 1.5h in 4 times of the amount of the extract; extracting for 1 hour in an amount which is 4 times that of the extract for the third time, filtering, combining the extracting solutions, recovering petroleum ether from the filtrate, and concentrating under reduced pressure to obtain paste (the relative density is 1.15-1.25 at the temperature of 25 ℃).
The preparation method comprises weighing herba Artemisiae Annuae extract, mixing with adjuvant silicon dioxide at a ratio of 1:1, granulating, drying at low temperature (below 55 deg.C), pulverizing, and packaging to 5000 g.
Example three:
weighing 1000g of a pure sweet wormwood herb according to the prescription amount, weighing three parts, respectively crushing, sieving by a 30-mesh sieve to obtain coarse powder, weighing, and calculating the powder yield. Mixing the three coarse powders for later use.
And X1, and determining the content of the sweet wormwood coarse powder by referring to high performance liquid chromatography (supplement 0512 of the second division of the 2010 version of Chinese animal pharmacopoeia).
X2, octadecyl bonded silica gel is used as a filling agent; acetonitrile: 0.1% glacial acetic acid is taken as a mobile phase, 50: 50; the flow rate was 1.0ml/min, and the detection wavelength was 210 nm. The column temperature is 35 ℃, and the theoretical number of pedals is not lower than 3000 according to the peak of artemisinin. A chromatographic column: 4.6mm × 250 mm; 5 μm or C18 with equivalent column efficiency.
X3, preparation of control solution. Accurately weighing artemisinin reference 10.00mg, placing in 10ml measuring flask, adding mobile phase for decomposition, diluting to scale, shaking, filtering, and making into 1mg per 1ml solution as reference solution.
X4, preparation of test solution: weighing herba Artemisiae Annuae coarse powder, sieving with No. 4 sieve, precisely sieving with a proper amount (containing artemisinin 10mg), placing in a 10ml measuring flask, adding a proper amount of mobile phase, ultrasonically dissolving artemisinin, cooling, diluting with mobile phase to scale, shaking, and filtering to obtain test solution.
X5, assay: precisely measuring 10 μ l of each of the sample solution and the reference solution, injecting into a liquid chromatograph, recording chromatogram, and calculating according to external standard method with chromatographic peak area.
TABLE 1 test result table of powder yield of sweet wormwood herb
The product is soluble in acetone, ethyl acetate, and chloroform, soluble in methanol, ethanol, diluted ethanol, diethyl ether and petroleum ether, and insoluble in water; it is soluble in glacial acetic acid. In order to extract the medicinal components completely as much as possible, the artemisinin and the sweet wormwood oil are extracted, and the synergistic effect of the components of the sweet wormwood is fully exerted. An organic solvent extraction method is selected, and three solvents of methanol, ethanol and petroleum ether (60-90 ℃) are respectively selected for investigation. The petroleum ether is most suitable to be used as an artemisinin extraction solvent, the artemisinin is a non-polar substance and is easily caused by overhigh temperature, the petroleum ether is a non-polar solvent, the content of the artemisinin in the extract is highest, the extraction is complete, and finally the petroleum ether is determined to be used as the extraction solvent of the sweet wormwood herb.
Investigation of solvent content of extraction process. Weighing the pure sweet wormwood medicinal material according to the prescription amount, adding petroleum ether respectively, extracting for three times, combining extracting solutions, recovering a solvent, concentrating to a proper amount, and adding auxiliary materials to prepare the sweet wormwood health-care tea. The petroleum ether addition is inspected, the extract yield and the artemisinin content are respectively used as evaluation indexes, data analysis is carried out on comprehensive scoring, the weight coefficients are that the extract yield is 0.4, the artemisinin content is 0.6, and the inspection method and the results are as follows:
x1, and optimizing the adding solvent amount. The material ratio is the ratio of the feeding (kg) of the sweet wormwood coarse powder to the volume (L) of the added solvent. The optimized petroleum ether dosage of the feed-liquid ratio is too low (1:6 or 1:7), the artemisinin in the sweet wormwood leaves can not be completely extracted, when the feed-liquid ratio is 1:8(kg: L), the artemisinin extraction rate reaches the maximum (1.00 percent), the petroleum ether dosage is continuously increased, and the artemisinin extraction rate is basically kept unchanged.
X2, weighing 1000g of sweet wormwood herb according to the prescription amount, weighing three parts, adding petroleum ether according to the design of the following table, extracting for three times at the temperature of below 55 ℃, 2h for the first time, 1.5h for the second time and 1h for the third time, combining the extracting solutions, filtering, recovering the solvent from the filtrate, and concentrating under reduced pressure to obtain the ointment. Respectively weighing, calculating the yield of the extract, and determining the content of artemisinin in the extract.
And X3, selecting 6, 4 and 4 times of petroleum ether as the optimal extraction conditions from the aspects of saving energy and reducing production cost.
TABLE 2 sweet wormwood herb extraction solvent selection and investigation result-methanol result table
TABLE 3 sweet wormwood herb extraction solvent selection and investigation result-ethanol result table
TABLE 4 sweet wormwood herb extraction solvent selection and investigation result-petroleum ether result table
TABLE 5 Experimental results of the amount of solvent added to Artemisia annua
Investigation of extraction time of extraction Process. Weighing 1000g of sweet wormwood herb according to the prescription amount, weighing three parts, respectively adding 6, 4 and 4 times of petroleum ether (60-90 ℃), designing the extraction time according to the following table, extracting for three times at the temperature of below 55 ℃, combining the extracting solutions, filtering, recovering the solvent from the filtrate, and concentrating under reduced pressure to obtain the paste. Respectively weighing, calculating the yield of the extract, and determining the content of artemisinin in the extract.
And X1, and time optimization is respectively carried out on three extractions in the production process. When the extraction time is 2h, the artemisinin extraction rate reaches the highest, and then the extraction time is prolonged, and the extraction rate is basically unchanged; the second extraction time is 1.5h, the artemisinin extraction rate reaches the highest; the third extraction time is 1h, and the artemisinin yield reaches the highest. Therefore, the optimized conditions are that the first extraction time is 2h, the second extraction time is 1.5h, and the third extraction time is 1 h.
And X2, taking the extraction time of 2, 1.5 and 1 hour as the extraction conditions from the aspects of saving energy and reducing production cost.
TABLE 6 Experimental result table of the extraction time of Artemisia apiacea medicinal materials
And (4) examining the extraction temperature of the extraction process. Weighing 1000g of sweet wormwood herb according to the prescription amount, weighing three parts, adding petroleum ether (60-90 ℃) in 6, 4 and 4 times of the amount of the sweet wormwood herb 0 respectively, extracting for 2, 1.5 and 1 hour, designing the extraction temperature according to the following table, extracting for three times, combining the extracting solutions, filtering, recovering the solvent from the filtrate, and concentrating under reduced pressure to obtain the ointment. Respectively weighing, calculating the yield of the extract, and determining the content of artemisinin in the extract.
X1, temperature optimization of extraction process without stirring. The extraction temperature is over 55 ℃, the variation of the artemisinin extraction rate is not obvious, the energy consumption is increased by increasing the temperature, and the artemisinin content is slightly reduced. Therefore, the optimal extraction temperature is 50-55 ℃, and the extraction rate of the artemisinin is 99%.
X2, small extraction validation test of extraction process. Weighing 3000g of sweet wormwood herb according to 3 times of the formula, weighing three parts, respectively adding petroleum ether (60-90 ℃) of 6, 4 and 4 times of the formula, extracting for three times at the temperature of below 55 ℃, 2 hours for the first time, 1.5 hours for the second time and 1 hour for the third time, combining extracting solutions, filtering, recovering the petroleum ether from filtrate, and concentrating into paste (the relative density is 1.15-1.25, the temperature is 25 ℃). 6. The experimental results of 4 and 4 times of petroleum ether extraction and verification are close to the experimental results of small-scale investigation, and the optimal petroleum ether amount extracted from the sweet wormwood herb is determined to be 6, 4 and 4 times.
TABLE 7 Experimental results of temperature extraction of sweet wormwood herb
A method for measuring the content of artemisinin in Artemisia annua extract is provided. The measurement is carried out according to high performance liquid chromatography (appendix 0512 of the second part of the 2010 edition of Chinese veterinary pharmacopoeia).
X1, octadecyl bonded silica gel is used as a filling agent; mixing acetonitrile: 0.1% glacial acetic acid (50:50) as mobile phase; the flow rate was 1.0ml/min, and the detection wavelength was 210 nm. The column temperature was 35 ℃. (or column equivalent chromatographic column) the theoretical number of pedals should not be less than 3000 calculated by artemisinin peak.
X2, preparation of control solution. Accurately weighing artemisinin reference 10.00mg, placing in 10ml measuring flask, adding mobile phase for decomposition, diluting to scale, shaking, filtering, and making into 1mg per 1ml solution as reference solution.
X3, preparation of a test solution. Precisely weighing appropriate amount of herba Artemisiae Annuae extract (containing artemisinin 10mg), placing in 10ml measuring flask, adding appropriate amount of mobile phase, ultrasonic dissolving artemisinin, cooling, diluting with mobile phase to scale, shaking, and filtering to obtain sample solution.
X4, assay: precisely measuring 10 μ l of each of the sample solution and the reference solution, injecting into a liquid chromatograph, recording chromatogram, and calculating according to external standard method with chromatographic peak area.
TABLE 8 Experimental results of the Artemisia apiacea herb extraction
And (5) observing a forming process. Referring to the products for treating the coccidiosis in chicken which are currently put out in markets at home and abroad, the dosage forms of the products mainly comprise powder (pulvis) and oral liquid. The main components of the oral liquid are chemical drugs, namely water-soluble antibiotic drugs, which have short administration period and quick response, but have serious residue problem and need a long withdrawal period; the powder (pulvis) is mainly a traditional Chinese veterinary medicine product in the domestic market, is different from water in most cases, can be administrated in a mode of mixing feed with feed, has a long administration period, and can play a role in preventing and treating chicken coccidiosis. The sweet wormwood extract, namely sweet wormwood extract, has high viscosity and strong hygroscopicity, and the content of artemisinin is higher for clinical application, so dilution and dispersion are needed and the hygroscopicity is reduced. The product of the invention is mainly used for treating coccidiosis infected in the growth process of chicken, the main complication part of the coccidiosis is the digestive tract of poultry, and a powder formulation is selected.
X1, determination of the content of main ingredient and the total amount of the final product. The main amount of each prescription is obtained according to the result of a verification experiment, and the crude amount of the sweet wormwood herb, the amount of the sweet wormwood herb and the yield of the coarse powder are 6250g, 99.88 percent and 6242.5 g. The amount of the sweet wormwood herb extracted by petroleum ether is 6250g, multiplied by 7.95 percent, multiplied by 496.88g and approximately 500 g. According to the related requirements and regulations of 'veterinary drug registration management approach' and 'technical requirements for veterinary drug and new drug research', each prescription is designed by taking 1000 as a unit. Therefore, the finished product of the invention is the finished product of the main medicine and the auxiliary materials, and the finished product of each prescription accounts for 1000 g.
X2, selection of auxiliary materials and determination of auxiliary material quantity. The powder is prepared by taking the sweet wormwood herb coarse powder extract and auxiliary materials as contents of the powder and adopting the processes of mixing granulation, drying, granule finishing, crushing, total mixing and internal packaging. According to the technical requirements of powder preparation, the prescription and process research is carried out according to the basic technical guidance principle of natural pharmaceutical preparation research. The auxiliary material silica has been collected in the "medical auxiliary materials Damien". A series of formulas are designed for auxiliary materials with similar purposes, starch, B-cyclodextrin, calcium hydrophosphate and silicon dioxide are respectively selected, and after screening, the sweet wormwood herb is determined to be used as a main drug, and the silicon dioxide is used as a dispersion medium.
X3 and determining the amount of auxiliary materials. The extract extracted from sweet wormwood herb is used as a main drug, and silicon dioxide is used as an auxiliary material. The ratio of the extract to the auxiliary materials is 1: 1.
TABLE 9 Experimental results of the types of the herbs extract and the auxiliary materials
10. Experimental result table of medicinal material extract and auxiliary material amount
TABLE 11 Experimental results of the small dosage of the auxiliary materials in the herba Artemisiae Annuae powder
TABLE 12 Experimental results of mixing time of the herb extracts and adjuvants
TABLE 13 Experimental results of drying temperature after mixing of the herb extract and the adjuvant
TABLE 14 Total mix process test results of Artemisia apiacea powder
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A new process for preparing the sweet wormwood powder for the square chicken is characterized in that: the method comprises the following steps:
1) selecting a sweet wormwood medicinal material, and coarsely crushing;
2) extracting herba Artemisiae Annuae, and concentrating under reduced pressure to obtain extract
Extracting for three times, mixing the extractive solutions, filtering, and concentrating under reduced pressure to obtain extract;
3) mixing the obtained paste with adjuvants, granulating, and sieving
The mass ratio of the auxiliary materials to the paste is 1: 1;
4) drying, granulating, pulverizing, and packaging.
2. The novel process for preparing the sweet wormwood powder for the mono-square chicken as claimed in claim 1, wherein the process comprises the following steps: the sweet wormwood herb in the step 1) is a processed medicinal sweet wormwood herb, and the medicinal sweet wormwood herb is coarsely ground and then screened by a second screen.
3. The novel process for preparing the sweet wormwood powder for the mono-square chicken as claimed in claim 1, wherein the process comprises the following steps: adding the amount of the extracting solution into the mixture obtained in the step 2) according to the ratio of 6:4:4, extracting for three times at 60-90 ℃, wherein the extracting solution is extracted for 2 hours for the first time, 1.5 hours for the second time and 1 hour for the third time, and the mass ratio of the extracting solution to the sweet wormwood herb is 1:1 ratio.
4. The novel process for preparing the sweet wormwood powder for the mono-square chicken as claimed in claim 1, wherein the process comprises the following steps: adding the amount of the extracting solution into the mixture obtained in the step 2) according to the ratio of 6:4:4, extracting for three times at the temperature of below 55 ℃, 2 hours for the first time, 1.5 hours for the second time and 1 hour for the third time, wherein the mass ratio of the extracting solution to the sweet wormwood herb is 1:1 ratio.
5. The novel process for preparing the sweet wormwood powder for the mono-square chicken as claimed in claim 3 or 4, wherein the process comprises the following steps: the extracting solution is petroleum ether.
6. The novel process for preparing the sweet wormwood powder for the mono-square chicken as claimed in claim 1, wherein the process comprises the following steps: the auxiliary material in the step 3) is silicon dioxide, and the mixing time is 60 minutes.
7. The novel process for preparing the sweet wormwood powder for the mono-square chicken as claimed in claim 1, wherein the process comprises the following steps: the sieving in the step 3) is as follows: sieving with 12 mesh sieve.
8. The novel process for preparing the sweet wormwood powder for the mono-square chicken as claimed in claim 1, wherein the process comprises the following steps: and 4) drying at 50-55 ℃, and sieving with a 10-mesh sieve to complete granules after drying.
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| CN114014871A (en) * | 2021-10-25 | 2022-02-08 | 河南天源药物研究有限公司 | Method for extracting artemisinin from sweet wormwood herb |
| CN114432355A (en) * | 2021-11-29 | 2022-05-06 | 河南天源药物研究有限公司 | Compound sweet wormwood powder for chickens and preparation method thereof |
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Application publication date: 20210709 |