CN112587601A - Improved cold medicine composition and its prepn - Google Patents
Improved cold medicine composition and its prepn Download PDFInfo
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
- A61K36/237—Notopterygium
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
- A61K36/232—Angelica
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Abstract
The invention relates to a preparation method of an improved cold pharmaceutical composition, which comprises 82.3g of notopterygium root, 164.6g of ephedra herb, 123.4g of cassia twig, 123.4g of schizonepeta spike, 82.3g of divaricate saposhnikovia root, 82.3g of angelica dahurica, 82.3g of szechuan lovage rhizome, 41.1g of grassleaf sweelflag rhizome, 123.4g of kudzuvine root, 41.1g of mint, 164.6g of bitter apricot seed, 82.3g of Chinese angelica, 164.6g of baical skullcap root and 82.3g of platycodon root, and is prepared2The preparation method comprises supercritical extraction and ethanol extraction, and solves the technical problems of low extraction rate of volatile oil, heavy deformation of dripping pills, round shape, tailing and adhesion.
Description
Technical Field
The invention relates to the field of medicine preparation, in particular to a preparation method of an improved cold medicine composition.
Background
A Chinese medicinal dripping pill for treating common cold is prepared from Notopterygii rhizoma, herba Ephedrae, ramulus Cinnamomi, herba Schizonepetae, radix Saposhnikoviae, and radix Angelicae Dahuricae. Has effects of dispelling pathogenic wind and relieving fever. Can be used for treating headache, fever, nasal obstruction, watery nasal discharge, aversion to cold, anhidrosis, soreness of joint, and sore throat due to affection of exogenous wind-cold.
During the production process, the problems that the extraction rate of the volatile oil is not high, the weight of the dripping pill is deformed, the dripping pill is approximately round, slightly tailing and slightly sticky are found.
Chinese invention CN200910307435.X, a cold drop pill for treating common cold and its preparation method, (1) extracting volatile oil from herba Schizonepetae and herba Menthae with 8-12 times of water for 2-4 hr, filtering to obtain medicinal liquid; heating and refluxing the other twelve raw medicinal materials by using 80% ethanol in an amount which is 8-12 times that of the raw medicinal materials for 2 times, wherein the first time is 1-4 hours, the second time is 1-2 hours, filtering, combining filtrates, recovering ethanol until no ethanol smell exists, combining the filtrates with the filtrates of the schizonepeta spike and the mint, and concentrating to obtain a thick paste with the relative density of 1.30 measured at 50 ℃; (3) adding the above soft extract into volatile oil, mixing, adding polyethylene glycol, and stirring to obtain molten solution containing medicinal extract and matrix; (4) adjusting the diameter of a dripper of the dripping pill machine, wherein the inner diameter is 1-5 mm, and the outer diameter is 2-10 mm; heating the dripping head of the pill dripping machine and keeping the temperature at 60-100 ℃; cooling and keeping the condensing agent at the temperature of 20 ℃ to-10 ℃; (5) putting the molten liquid containing the medicine extract and the matrix into a storage tank of a pill dropping machine; (6) dripping the molten solution containing the medicinal extract and matrix into condensing agent, and making into pill.
The preparation method is also an invention patent of Guizhou Jianxing pharmaceutical industry Co., Ltd, but in the using process, the volatile oil is extracted by water originally, so that the extraction rate of the volatile oil is low; in addition, the addition amount of polyethylene glycol, the dripping distance and the dripping speed are not determined, which leads to the problems of weight deformation, round shape, tailing and adhesion of the dripping pills.
In order to solve the problems, the applicant improves the original preparation method through long-term grope tests, and solves the technical problems of low extraction rate of volatile oil, heavy deformation of the dripping pill, approximately round shape, slight tailing, slight adhesion and the like.
Disclosure of Invention
The invention aims to provide an improved preparation method of a cold medicine composition.
The pharmaceutical composition of the invention comprises 82.3g of notopterygium root, 164.6g of ephedra herb, 123.4g of cassia twig, 123.4g of schizonepeta spike, 82.3g of divaricate saposhnikovia root, 82.3g of angelica dahurica, 82.3g of szechuan lovage rhizome, 41.1g of grassleaf sweelflag rhizome, 123.4g of kudzuvine root, 41.1g of mint, 164.6g of bitter apricot kernel, 82.3g of angelica, 164.6g of baical skullcap root and 82.3g of platycodon grandiflorum, and the preparation:
1) pulverizing herba Menthae, rhizoma Acori Graminei and ramulus Cinnamomi into coarse powder, and adding CO2Performing supercritical extraction, wherein the extraction pressure is 30-50 MPa, the extraction temperature is 35-55 ℃, the extraction flow rate is 10-19L/h, the extraction time is 1-2.5 h, and the extract is reserved;
2) extracting the rest materials with 10 times of 80% ethanol under reflux for 2 times, 2 hr for the first time and 1 hr for the second time, mixing decoctions, filtering, and concentrating at 50 deg.C to obtain soft extract with relative density of 1.30;
3) mixing the soft extract of step 2) with the extract of step 1), adding polyethylene glycol 6000, and stirring to obtain molten liquid containing the medicinal extract and matrix;
4) adjusting the caliber of a dripper of the pill dropping machine, wherein the inner diameter is 2mm and the outer diameter is 5 mm; heating and keeping the temperature of a dripping head of the pill dripping machine at 75 ℃; cooling the condensing agent and keeping the temperature at-2-6 ℃; putting the obtained molten liquid containing the medicine extract and the matrix into a material storage tank of a pill dropping machine;
5) dripping the drug extract and the matrix molten liquid in a storage tank of a pill dropping machine into liquid paraffin at a dripping distance of 4-5 cm; and (4) contracting into pills at the dripping speed of 52-60 drops/min.
Preferably, the extraction pressure of the method is 35-45 MPa.
Preferably, the extraction pressure of the invention is 40 MPa.
Preferably, the extraction temperature is 40-50 ℃.
Preferably, the extraction temperature of the method is 45 ℃.
Preferably, the extraction flow rate of the invention is 15L/h.
Preferably, the extraction time of the invention is 2 h.
Preferably, the amount of the polyethylene glycol 6000 in the invention is 4 times.
The preparation provided by the invention is a solid preparation or a liquid preparation.
The solid preparation is granules, capsules, tablets, pills, powder and freeze-dried powder injection; the liquid preparation is mixture, injection preparation and oral liquid.
Has the advantages that:
1. the prior art has the problem that the extraction rate of volatile oil is not high by extracting volatile oil with water; the invention adopts CO for mint, grassleaf sweelflag rhizome and cassia twig2Supercritical extraction, and experiments prove that the highest yield of the volatile oil reaches 4.48 percent.
2. The prior art does not clearly determine the adding amount of polyethylene glycol, the dropping distance and the dropping speed, and leads to the problems of heavy weight deformation, approximately round shape, slight tailing, slight adhesion and the like of the dropping pill. The invention determines the adding amount of polyethylene glycol, the dropping distance and the dropping speed by adjusting, and the molding condition is as follows: better, less streaking, and less sticking problems.
Detailed Description
The technical solution of the present invention will be further specifically described below by way of specific examples.
Example 1
The formula is as follows: 82.3g of notopterygium root, 164.6g of ephedra herb, 123.4g of cassia twig, 123.4g of schizonepeta spike, 82.3g of divaricate saposhnikovia root, 82.3g of angelica dahurica, 82.3g of szechuan lovage rhizome, 41.1g of grassleaf sweelflag rhizome, 123.4g of kudzuvine root, 41.1g of mint, 164.6g of bitter apricot seed, 82.3g of Chinese angelica, 164.6g of baical skullcap root and 82.3g of platycodon root.
The preparation method comprises the following steps:
1) pulverizing herba Menthae, rhizoma Acori Graminei and ramulus Cinnamomi into coarse powder, and adding CO2Performing supercritical extraction, wherein the extraction pressure is 40MPa, the extraction temperature is 45 ℃, the extraction flow rate is 15L/h, the extraction time is 2h, and the extract is reserved;
2) extracting the rest materials with 10 times of 80% ethanol under reflux for 2 times, 2 hr for the first time and 1 hr for the second time, mixing decoctions, filtering, and concentrating at 50 deg.C to obtain soft extract with relative density of 1.30;
3) mixing the soft extract of step 2) with the extract of step 1), adding 4 times of polyethylene glycol 6000, and stirring to obtain molten liquid containing the medicinal extract and matrix;
4) adjusting the caliber of a dripper of the pill dropping machine, wherein the inner diameter is 2mm and the outer diameter is 5 mm; heating and keeping the temperature of a dripping head of the pill dripping machine at 75 ℃; cooling the condensing agent and keeping the temperature at-2-6 ℃; putting the obtained molten liquid containing the medicine extract and the matrix into a material storage tank of a pill dropping machine;
5) dripping the drug extract and the matrix molten liquid in a storage tank of a pill dropping machine into liquid paraffin at a dripping distance of 4-5 cm; and (4) contracting into pills at the dripping speed of 52-60 drops/min.
Example 2
The formula is as follows: 82.3g of notopterygium root, 164.6g of ephedra herb, 123.4g of cassia twig, 123.4g of schizonepeta spike, 82.3g of divaricate saposhnikovia root, 82.3g of angelica dahurica, 82.3g of szechuan lovage rhizome, 41.1g of grassleaf sweelflag rhizome, 123.4g of kudzuvine root, 41.1g of mint, 164.6g of bitter apricot kernel, 82.3g of Chinese angelica, 164.6g of baical skullcap root and 82.3g of platycodon
The preparation method comprises the following steps:
1) pulverizing herba Menthae, rhizoma Acori Graminei and ramulus Cinnamomi into coarse powder, and adding CO2Performing supercritical extraction, wherein the extraction pressure is 30MPa, the extraction temperature is 55 ℃, the extraction flow rate is 19L/h, the extraction time is 1h, and the extract is reserved;
2) extracting the rest materials with 10 times of 80% ethanol under reflux for 2 times, 2 hr for the first time and 1 hr for the second time, mixing decoctions, filtering, and concentrating at 50 deg.C to obtain soft extract with relative density of 1.30;
3) mixing the soft extract of step 2) with the extract of step 1), adding 4 times of polyethylene glycol 6000, and stirring to obtain molten liquid containing the medicinal extract and matrix;
4) adjusting the caliber of a dripper of the pill dropping machine, wherein the inner diameter is 2mm and the outer diameter is 5 mm; heating and keeping the temperature of a dripping head of the pill dripping machine at 75 ℃; cooling the condensing agent and keeping the temperature at-2-6 ℃; putting the obtained molten liquid containing the medicine extract and the matrix into a material storage tank of a pill dropping machine;
5) dripping the drug extract and the matrix molten liquid in a storage tank of a pill dropping machine into liquid paraffin at a dripping distance of 4-5 cm; and (4) contracting into pills at the dripping speed of 52-60 drops/min.
Example 3
The formula is as follows: 82.3g of notopterygium root, 164.6g of ephedra herb, 123.4g of cassia twig, 123.4g of schizonepeta spike, 82.3g of divaricate saposhnikovia root, 82.3g of angelica dahurica, 82.3g of szechuan lovage rhizome, 41.1g of grassleaf sweelflag rhizome, 123.4g of kudzuvine root, 41.1g of mint, 164.6g of bitter apricot kernel, 82.3g of Chinese angelica, 164.6g of baical skullcap root and 82.3g of platycodon
The preparation method comprises the following steps:
1) pulverizing herba Menthae, rhizoma Acori Graminei and ramulus Cinnamomi into coarse powder, and adding CO2Performing supercritical extraction, wherein the extraction pressure is 50MPa, the extraction temperature is 35 ℃, the extraction flow rate is 10L/h, the extraction time is 1.5h, and the extract is reserved;
2) extracting the rest materials with 10 times of 80% ethanol under reflux for 2 times, 2 hr for the first time and 1 hr for the second time, mixing decoctions, filtering, and concentrating at 50 deg.C to obtain soft extract with relative density of 1.30;
3) mixing the soft extract of step 2) with the extract of step 1), adding 4 times of polyethylene glycol 6000, and stirring to obtain molten liquid containing the medicinal extract and matrix;
4) adjusting the caliber of a dripper of the pill dropping machine, wherein the inner diameter is 2mm and the outer diameter is 5 mm; heating and keeping the temperature of a dripping head of the pill dripping machine at 75 ℃; cooling the condensing agent and keeping the temperature at-2-6 ℃; putting the obtained molten liquid containing the medicine extract and the matrix into a material storage tank of a pill dropping machine;
5) dripping the drug extract and the matrix molten liquid in a storage tank of a pill dropping machine into liquid paraffin at a dripping distance of 4-5 cm; and (4) contracting into pills at the dripping speed of 52-60 drops/min.
Example 4
The formula is as follows: 82.3g of notopterygium root, 164.6g of ephedra herb, 123.4g of cassia twig, 123.4g of schizonepeta spike, 82.3g of divaricate saposhnikovia root, 82.3g of angelica dahurica, 82.3g of szechuan lovage rhizome, 41.1g of grassleaf sweelflag rhizome, 123.4g of kudzuvine root, 41.1g of mint, 164.6g of bitter apricot kernel, 82.3g of Chinese angelica, 164.6g of baical skullcap root and 82.3g of platycodon
The preparation method comprises the following steps:
1) pulverizing herba Menthae, rhizoma Acori Graminei and ramulus Cinnamomi into coarse powder, and adding CO2Supercritical extraction at 35MPa and 40 deg.C and flow rate15L/h, the extraction time is 2h, and the extract is reserved;
2) extracting the rest materials with 10 times of 80% ethanol under reflux for 2 times, 2 hr for the first time and 1 hr for the second time, mixing decoctions, filtering, and concentrating at 50 deg.C to obtain soft extract with relative density of 1.30;
3) mixing the soft extract of step 2) with the extract of step 1), adding 4 times of polyethylene glycol 6000, and stirring to obtain molten liquid containing the medicinal extract and matrix;
4) adjusting the caliber of a dripper of the pill dropping machine, wherein the inner diameter is 2mm and the outer diameter is 5 mm; heating and keeping the temperature of a dripping head of the pill dripping machine at 75 ℃; cooling the condensing agent and keeping the temperature at-2-6 ℃; putting the obtained molten liquid containing the medicine extract and the matrix into a material storage tank of a pill dropping machine;
5) dripping the drug extract and the matrix molten liquid in a storage tank of a pill dropping machine into liquid paraffin at a dripping distance of 4-5 cm; and (4) contracting into pills at the dripping speed of 52-60 drops/min.
Example 5
The formula is as follows: 82.3g of notopterygium root, 164.6g of ephedra herb, 123.4g of cassia twig, 123.4g of schizonepeta spike, 82.3g of divaricate saposhnikovia root, 82.3g of angelica dahurica, 82.3g of szechuan lovage rhizome, 41.1g of grassleaf sweelflag rhizome, 123.4g of kudzuvine root, 41.1g of mint, 164.6g of bitter apricot kernel, 82.3g of Chinese angelica, 164.6g of baical skullcap root and 82.3g of platycodon
The preparation method comprises the following steps:
1) pulverizing herba Menthae, rhizoma Acori Graminei and ramulus Cinnamomi into coarse powder, and adding CO2Performing supercritical extraction, wherein the extraction pressure is 45MPa, the extraction temperature is 50 ℃, the extraction flow rate is 10L/h, the extraction time is 2h, and the extract is reserved;
2) extracting the rest materials with 10 times of 80% ethanol under reflux for 2 times, 2 hr for the first time and 1 hr for the second time, mixing decoctions, filtering, and concentrating at 50 deg.C to obtain soft extract with relative density of 1.30;
3) mixing the soft extract of step 2) with the extract of step 1), adding 4 times of polyethylene glycol 6000, and stirring to obtain molten liquid containing the medicinal extract and matrix;
4) adjusting the caliber of a dripper of the pill dropping machine, wherein the inner diameter is 2mm and the outer diameter is 5 mm; heating and keeping the temperature of a dripping head of the pill dripping machine at 75 ℃; cooling the condensing agent and keeping the temperature at-2-6 ℃; putting the obtained molten liquid containing the medicine extract and the matrix into a material storage tank of a pill dropping machine;
5) dripping the drug extract and the matrix molten liquid in a storage tank of a pill dropping machine into liquid paraffin at a dripping distance of 4-5 cm; and (4) contracting into pills at the dripping speed of 52-60 drops/min.
To further verify the effectiveness of the present invention, the inventors performed a series of verification tests, excerpted as follows:
firstly, determining supercritical carbon dioxide extraction parameters
41.1g of mint, 41.1g of grassleaf sweelflag rhizome and 123.4g of cassia twig are crushed into coarse powder, the investigation of carbon dioxide supercritical extraction parameters is carried out, and according to the report of the existing documents, pressure, temperature, extraction time and flow rate are important parameters in the carbon dioxide supercritical extraction process, so that the pressure (factor A), the temperature (factor B), the extraction time (factor C) and the extraction flow rate (factor D) are taken as experimental investigation factors. Using 4-factor 3 level L9(34) Orthogonal design, see tables 1 and 2.
TABLE 1 level table of orthogonal experimental factors of supercritical carbon dioxide extraction of mint, grassleaved sweetflag rhizome and cassia twig
TABLE 2 orthogonal experimental results of supercritical carbon dioxide extraction of herba Menthae, rhizoma Acori Graminei and ramulus Cinnamomi
The experimental results are as follows: extraction ratio (%)
As can be seen from the above table, the four factors affect the extraction rate in the following order: time of extraction>Pressure of extraction>Temperature of extraction>The extraction flow rate. The optimal combination between factors and levels is A2B2C3D1Pulverizing herba Menthae, rhizoma Acori Graminei and ramulus Cinnamomi into coarse powder, and adding CO2Supercritical extraction at 40MPaThe extraction temperature is 45 ℃, the extraction time is 2 hours, the flow rate is 15L/h, and the extract is reserved.
TABLE 3 analysis of variance in supercritical carbon dioxide extraction orthogonal experiment for peppermint, grassleaf sweelflag rhizome and cassia twig
Factors of the fact | Sum of squares of deviation | Degree of freedom | F ratio | Critical value of F |
A(MPa) | 0.052 | 2 | 1.677 | 19.000 |
B(℃) | 0.052 | 2 | 1.677 | 19.000 |
C(H) | 0.190 | 2 | 6.129 | 19.000 |
D(L/h) | 0.031 | 2 | 1.000 | 19.000 |
Error of the measurement | 0.03 | 2 |
Note: p is more than 0.05.
The analysis result of variance shows that all factors have no significant influence on the extraction rate, and the optimal factor level of the carbon dioxide supercritical extraction is as follows: the extraction pressure is 40MPa, the extraction temperature is 45 ℃, the extraction time is 2h, the flow rate is 15L/h, and the extract is reserved.
1. Carbon dioxide supercritical extraction verification test
In order to verify the optimum process of carbon dioxide supercritical extraction of herba Menthae, rhizoma Acori Graminei and ramulus Cinnamomi, 41.1g of herba Menthae, 41.1g of rhizoma Acori Graminei and 123.4g of ramulus Cinnamomi are pulverized into coarse powder, mixed well, and added in A2B2C3D1And (5) carrying out a carbon dioxide supercritical extraction verification test under the condition. See table 3.
TABLE 3 carbon dioxide supercritical extraction validation test results
Serial number | Yield of essential oil (%) |
1 | 4.43 |
2 | 4.48 |
3 | 4.46 |
As a result: the results of 3 verification tests show that: a. the2B2C3D1The carbon dioxide supercritical extraction conditions are basically consistent with the orthogonal test results, so the optimal carbon dioxide supercritical extraction parameters are as follows: the extraction pressure is 40MPa, the extraction temperature is 45 ℃, the extraction time is 2h, and the flow rate is 15L/h.
Second, investigation of forming process
The optimal cold pill production process parameters are screened out by investigating the influence of relevant parameters such as the ingredient proportion, the temperature of a cooling medium, the drop distance, the drop speed and the like on the forming conditions such as the hardness, the roundness, the tailing, the adhesion and the like of the pill and the yield of the pill in the cold pill production process. The current 20 batches of products before and after continuous statistical optimization are subjected to statistical analysis on the yield and the molding condition, and the method comprises the following steps:
the method comprises the following steps: drug to carrier ratio: 1: 2.7; temperature of refrigerant: 2-10 ℃; the dripping distance is not more than 3 cm; the dropping speed is 30-50 drops/min.
The second method comprises the following steps:
the optimized technological parameters are as follows: drug to carrier ratio: 1: 4.0; temperature of refrigerant: -2 ℃ to 6 ℃; the drop distance is 4-5 cm; the dropping speed is 52-60 drops/min.
As can be seen from the table above, the average yield of method two is significantly higher than method one, so the drug to carrier ratio is preferred: 1: 4.0; temperature of refrigerant: -2 ℃ to 6 ℃; the drop distance is 4-5 cm; the dropping speed is 52-60 drops/min.
While the invention has been described in detail in the foregoing by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that certain changes and modifications may be made therein based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. An improved preparation method of a cold pharmaceutical composition is characterized in that the pharmaceutical composition is composed of 82.3g of notopterygium root, 164.6g of ephedra herb, 123.4g of cassia twig, 123.4g of schizonepeta spike, 82.3g of divaricate saposhnikovia root, 82.3g of angelica dahurica, 82.3g of ligusticum wallichii, 41.1g of rhizoma acori graminei, 123.4g of radix puerariae, 41.1g of mint, 164.6g of bitter apricot kernel, 82.3g of angelica, 164.6g of scutellaria baicalensis and 82.3g of platycodon grandiflorum, and the preparation method is as follows:
1) pulverizing herba Menthae, rhizoma Acori Graminei and ramulus Cinnamomi into coarse powder, and adding CO2Performing supercritical extraction, wherein the extraction pressure is 30-50 MPa, the extraction temperature is 35-55 ℃, the extraction flow rate is 10-19L/h, the extraction time is 1-2.5 h, and the extract is reserved;
2) extracting the rest materials with 10 times of 80% ethanol under reflux for 2 times, 2 hr for the first time and 1 hr for the second time, mixing decoctions, filtering, and concentrating at 50 deg.C to obtain soft extract with relative density of 1.30;
3) mixing the soft extract of step 2) with the extract of step 1), adding polyethylene glycol 6000, and stirring to obtain molten liquid containing the medicinal extract and matrix;
4) adjusting the caliber of a dripper of the pill dropping machine, wherein the inner diameter is 2mm and the outer diameter is 5 mm; heating and keeping the temperature of a dripping head of the pill dripping machine at 75 ℃; cooling the condensing agent and keeping the temperature at-2-6 ℃; putting the obtained molten liquid containing the medicine extract and the matrix into a material storage tank of a pill dropping machine;
5) dripping the drug extract and the matrix molten liquid in a storage tank of a pill dropping machine into liquid paraffin at a dripping distance of 4-5 cm; and (4) contracting into pills at the dripping speed of 52-60 drops/min.
2. The method of claim 1, wherein the extraction pressure is 35 to 45 MPa.
3. The method of claim 2, wherein the extraction pressure is 40 MPa.
4. The method according to claim 1, wherein the extraction temperature is 40 to 50 ℃.
5. The method of claim 1, wherein the extraction temperature is 45 ℃.
6. The method of claim 1, wherein the extraction flow rate is 15L/h.
7. The method of claim 1, wherein the extraction time is 2 hours.
8. The preparation method according to claim 1, wherein the amount of polyethylene glycol 6000 is 4 times of the total amount of the thick paste of step 2) and the extract of step 1).
9. The method for producing according to claim 1, wherein the preparation is a solid preparation or a liquid preparation.
10. The preparation method according to claim 8, wherein the solid preparation is granules, capsules, tablets, pills, powder, lyophilized powder for injection; the liquid preparation is mixture, injection preparation and oral liquid.
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