CN105624222A - Method for preparing chlortetracycline hydrochloride - Google Patents
Method for preparing chlortetracycline hydrochloride Download PDFInfo
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Abstract
The invention discloses a method for preparing chlortetracycline hydrochloride and belongs to the field of medicine synthesis. The method aims to solve the problems that at present, a second solvent crystallization method is mostly adopted for producing chlortetracycline hydrochloride in China, the secondary crystallization process is long, much solvent waste liquid is generated by production, and product quality and active ingredients are low. According to the method, strains in aureomycin fungus residues are extracted for culture, then a modified additive solution is utilized to conduct screening modification on cultured strains, meanwhile fermentation is conducted under the acidic condition, the content of aureomycin in the fermentation process is raised so that the aureomycin can be acidized easily, finally adsorption is conducted through attapulgite, the ultrasonic stripping is conducted, concentration and drying are conducted, and the chlortetracycline hydrochloride high in quality and activity is obtained.
Description
Technical field
The present invention discloses the preparation method of a kind of Isphamycin, belongs to pharmaceutical synthesis field.
Background technology
Duomycin is the activeconstituents of streptomyces aureus (Streptomycesaureofaciens) biosynthesizing, is tetracycline antibiotics. Isphamycin is the hydrochloride of duomycin, for golden yellow or yellow crystal, without smelly, bitter, meets photochromic gradual change dark, micro-molten in water or ethanol, in acetone, ether or trichloromethane almost insoluble, now it is mainly used in treatment conjunctivitis and trachoma as people's medication, now it is mainly used in treating the diseases such as the typhoid fever of livestock and poultry, dysentery characterized by white mucous stool as veterinary medicine, it is possible to use as livestock and poultry growth promoter. Further developing along with livestock industry in recent years, the market demand of Isphamycin constantly expands, external client is also more and more higher to its specification of quality, and product price is directly related with active component content, therefore, the preparation method being necessary Improvement and perfection Isphamycin, to improve the quality of products and active component content.
Current domestic manufacturer all adopts two solvent crystallizations to produce, and secondary crystal operation is long, and the solvent waste liquid produced is many, and therefore existing production method has a lot of problem in economy, security, environmental protection.
Summary of the invention
The technical problem that the present invention mainly solves: produce with two solvent crystallizations for the many employings of current domestic production Isphamycin, secondary crystal operation is long, the solvent waste liquid produced is many, and quality product and the low problem of activeconstituents, the bacterial classification of the present invention by extracting in duomycin bacterium slag, cultivate, carrying out screening modification to the bacterial classification in cultivation by modification annex solution, ferment in acid condition simultaneously, promote the content of duomycin in fermentation and make it be easy to by acidifying, adsorb finally by attapulgite, again through ultrasonic de-attached, concentrate drying, obtain quality and the high Isphamycin of activity.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) hundred parts of ratios are counted by weight, get 40��50 parts of dregs of beans, 13��15 parts of agar, 6��8 parts of blood meals, 22��25 portions of sucrose, 8��10 parts of massfractions be the sodium chloride solution of 12%, 0.8��1.2 part of dipotassium hydrogen phosphate and 0.2��0.8 part of potassium primary phosphate, after stirring evenly at 115��120 DEG C, sterilizing 30��40min, functional quality mark is hydrochloric acid soln adjustment pH to 5.5��6.0 of 10%, obtains substratum;
(2) substratum measuring the above-mentioned preparation of 30��40mL puts into 250mL triangular flask, stirrer is put into after being mixed by the glucose solution that duomycin bacterium slag and massfraction are 20��25% by solid-to-liquid ratio 1:3 again, after leaving standstill 10��15min after stirring 30��40min with 600��800r/min, collect 70��90mL supernatant liquid and put into Erlenmeyer flask, for subsequent use;
(3) 1:8 in mass ratio, Poria cocos and the Radix Astragali are put into pulverizer pulverize, cross 200 order sieves, particle after sieving is put into container, add the hydrochloric acid soln that massfraction is 5% wherein, flood particle 6��8cm, container is heated to 80��90 DEG C, after stirring 8��10h with rotating speed 120r/min, stop stirring heating, leave standstill 30��40mim, carry out filtration under diminished pressure, collect filtered liquid, 9:2:1 by volume again, by filtered liquid, massfraction be 10% magnesium nitrate solution and massfraction be that 15% ferric chloride Solution stirs evenly, functional quality mark is hydrochloric acid soln adjustment pH to 5.0��5.5 of 15%, it is prepared into modification annex solution,
(4) triangular flask for subsequent use in step (2) is put into microwave oscillator, at 400��600MHz, at 28��32 DEG C, after vibration 20��22h, by inoculum size 5��7%, culturing mixt in triangular flask is put into fermentation bottle, air flow is set as 1:1.2��1.8, and temperature is set as 28��32 DEG C, and rotating speed is 120��150r/min, fermentation 36��42h, every 7��8h add the modification annex solution of the above-mentioned preparation of culturing mixt volume 3��4% in fermentation bottle wherein;
(5) after above-mentioned fermentation ends, fermented liquid is collected, the massfraction adding fermentating liquid volume 2��4% wherein is the oxalic acid solution of 30%, functional quality mark is hydrochloric acid soln adjustment pH to 4.0��4.5 of 30%, again the fermented liquid after adjustment is put into whizzer centrifugation 2��5min under 600��700r/min, collect supernatant liquor and put into container, stir the 150 order attapulgites adding fermented liquid quality 15��20% after evenly wherein, 1��2h is left standstill after stirring 20��30min, filter, collect filtrate;
(6) filtrate by above-mentioned gained mixes by solid-to-liquid ratio 1:3 with dehydrated alcohol, filter after mixture is placed in ultrasonic cleaning instrument vibration 1��2h that frequency is 23��25KHz again, collection filtered liquid is put into concentration tank and is concentrated 40��50% to original volume, subsequently concentrated solution is put into spray-drier and carry out spraying dry, Isphamycin can be obtained.
The Isphamycin of gained of the present invention obtains after testing: actual the tiring of fermented liquid is 24620��27130 �� g/mL, the content that Ledermycins is less than 0.8%, dehydration tetracycline content is less than 0.4%, and the content of Isphamycin reaches more than 94%, and duomycin content is less than 3%.
The useful effect of the present invention:
(1) the present invention pollutes few in preparation process, and security height and cost are low;
(2) Isphamycin prepared by the present invention is active high, and the content of Isphamycin reaches more than 94%.
Embodiment
Hundred parts of ratio meters by weight, get 40��50 parts of dregs of beans, 13��15 parts of agar, 6��8 parts of blood meals, 22��25 portions of sucrose, 8��10 parts of massfractions be the sodium chloride solution of 12%, 0.8��1.2 part of dipotassium hydrogen phosphate and 0.2��0.8 part of potassium primary phosphate, after stirring evenly at 115��120 DEG C, sterilizing 30��40min, functional quality mark is hydrochloric acid soln adjustment pH to 5.5��6.0 of 10%, obtains substratum, the substratum measuring the above-mentioned preparation of 30��40mL puts into 250mL triangular flask, stirrer is put into after being mixed by the glucose solution that duomycin bacterium slag and massfraction are 20��25% by solid-to-liquid ratio 1:3 again, after leaving standstill 10��15min after stirring 30��40min with 600��800r/min, collect 70��90mL supernatant liquid and put into Erlenmeyer flask, for subsequent use, 1:8 in mass ratio, Poria cocos and the Radix Astragali are put into pulverizer pulverize, cross 200 order sieves, particle after sieving is put into container, add the hydrochloric acid soln that massfraction is 5% wherein, flood particle 6��8cm, container is heated to 80��90 DEG C, after stirring 8��10h with rotating speed 120r/min, stop stirring heating, leave standstill 30��40mim, carry out filtration under diminished pressure, collect filtered liquid, 9:2:1 by volume again, by filtered liquid, massfraction be 10% magnesium nitrate solution and massfraction be that 15% ferric chloride Solution stirs evenly, functional quality mark is hydrochloric acid soln adjustment pH to 5.0��5.5 of 15%, it is prepared into modification annex solution, triangular flask for subsequent use is put into microwave oscillator, at 400��600MHz, at 28��32 DEG C, after vibration 20��22h, by inoculum size 5��7%, culturing mixt in triangular flask is put into fermentation bottle, air flow is set as 1:1.2��1.8, and temperature is set as 28��32 DEG C, and rotating speed is 120��150r/min, fermentation 36��42h, every 7��8h add the modification annex solution of the above-mentioned preparation of culturing mixt volume 3��4% in fermentation bottle wherein, fermented liquid is collected after above-mentioned fermentation ends, the massfraction adding fermentating liquid volume 2��4% wherein is the oxalic acid solution of 30%, functional quality mark is hydrochloric acid soln adjustment pH to 4.0��4.5 of 30%, again the fermented liquid after adjustment is put into whizzer centrifugation 2��5min under 600��700r/min, collect supernatant liquor and put into container, stir the 150 order attapulgites adding fermented liquid quality 15��20% after evenly wherein, 1��2h is left standstill after stirring 20��30min, filter, collect filtrate, the filtrate of above-mentioned gained is mixed by solid-to-liquid ratio 1:3 with dehydrated alcohol, filter after mixture is placed in ultrasonic cleaning instrument vibration 1��2h that frequency is 23��25KHz again, collection filtered liquid is put into concentration tank and is concentrated 40��50% to original volume, subsequently concentrated solution is put into spray-drier and carry out spraying dry, Isphamycin can be obtained.
Example 1
Hundred parts of ratio meters by weight, get 43 parts of dregs of beans, 14 parts of agar, 7 parts of blood meals, 24 portions of sucrose, 10 parts of massfractions be the sodium chloride solution of 12%, 1.2 parts of dipotassium hydrogen phosphates and 0.8 part of potassium primary phosphate, after stirring evenly at 118 DEG C, sterilizing 35min, functional quality mark is the hydrochloric acid soln adjustment pH to 5.5 of 10%, obtains substratum, the substratum measuring the above-mentioned preparation of 35mL puts into 250mL triangular flask, stirrer is put into after being mixed by the glucose solution that duomycin bacterium slag and massfraction are 22% by solid-to-liquid ratio 1:3 again, after leaving standstill 12min after stirring 35min with 700r/min, collect 80mL supernatant liquid and put into Erlenmeyer flask, for subsequent use, 1:8 in mass ratio, Poria cocos and the Radix Astragali are put into pulverizer pulverize, cross 200 order sieves, particle after sieving is put into container, add the hydrochloric acid soln that massfraction is 5% wherein, flood particle 7cm, container is heated to 85 DEG C, after stirring 9h with rotating speed 120r/min, stop stirring heating, leave standstill 35mim, carry out filtration under diminished pressure, collect filtered liquid, 9:2:1 by volume again, by filtered liquid, massfraction be 10% magnesium nitrate solution and massfraction be that 15% ferric chloride Solution stirs evenly, functional quality mark is the hydrochloric acid soln adjustment pH to 5.0 of 15%, it is prepared into modification annex solution, triangular flask for subsequent use is put into microwave oscillator, at 500MHz, at 30 DEG C, after vibration 20h, by inoculum size 6%, culturing mixt in triangular flask is put into fermentation bottle, air flow is set as 1:1.5, and temperature is set as 30 DEG C, and rotating speed is 130r/min, fermentation 40h, every 7h add the modification annex solution of the above-mentioned preparation of culturing mixt volume 3% in fermentation bottle wherein, fermented liquid is collected after above-mentioned fermentation ends, the massfraction adding fermentating liquid volume 3% wherein is the oxalic acid solution of 30%, functional quality mark is the hydrochloric acid soln adjustment pH to 4.0 of 30%, again the fermented liquid after adjustment is put into whizzer centrifugation 4min under 650r/min, collect supernatant liquor and put into container, stir the 150 order attapulgites adding fermented liquid quality 18% after evenly wherein, after stirring 25min, leave standstill 2h, filter, collect filtrate, the filtrate of above-mentioned gained is mixed by solid-to-liquid ratio 1:3 with dehydrated alcohol, mixture is placed in ultrasonic cleaning instrument that frequency is 24KHz again vibrate and filter after 1.5h, collection filtered liquid is put into concentration tank and is concentrated 45% to original volume, subsequently concentrated solution is put into spray-drier and carry out spraying dry, Isphamycin can be obtained.
The Isphamycin of gained of the present invention obtains after testing: actual the tiring of fermented liquid is 24620 �� g/mL, and the content that Ledermycins is 0.6%, and dehydration tetracycline content is 0.32%, and the content of Isphamycin reaches 94.7%, and duomycin content is 2.8%.
Example 2
Hundred parts of ratio meters by weight, get 40 parts of dregs of beans, 15 parts of agar, 8 parts of blood meals, 25 portions of sucrose, 10 parts of massfractions be the sodium chloride solution of 12%, 1.2 parts of dipotassium hydrogen phosphates and 0.8 part of potassium primary phosphate, after stirring evenly at 115 DEG C, sterilizing 30min, functional quality mark is the hydrochloric acid soln adjustment pH to 5.5 of 10%, obtains substratum, the substratum measuring the above-mentioned preparation of 30mL puts into 250mL triangular flask, stirrer is put into after being mixed by the glucose solution that duomycin bacterium slag and massfraction are 20% by solid-to-liquid ratio 1:3 again, after leaving standstill 10min after stirring 30min with 600r/min, collect 70mL supernatant liquid and put into Erlenmeyer flask, for subsequent use, 1:8 in mass ratio, Poria cocos and the Radix Astragali are put into pulverizer pulverize, cross 200 order sieves, particle after sieving is put into container, add the hydrochloric acid soln that massfraction is 5% wherein, flood particle 6cm, container is heated to 80 DEG C, after stirring 8h with rotating speed 120r/min, stop stirring heating, leave standstill 30mim, carry out filtration under diminished pressure, collect filtered liquid, 9:2:1 by volume again, by filtered liquid, massfraction be 10% magnesium nitrate solution and massfraction be that 15% ferric chloride Solution stirs evenly, functional quality mark is the hydrochloric acid soln adjustment pH to 5.0 of 15%, it is prepared into modification annex solution, triangular flask for subsequent use is put into microwave oscillator, at 400MHz, at 28 DEG C, after vibration 20h, by inoculum size 5%, culturing mixt in triangular flask is put into fermentation bottle, air flow is set as 1:1.2, and temperature is set as 28 DEG C, and rotating speed is 120r/min, fermentation 36h, every 7h add the modification annex solution of the above-mentioned preparation of culturing mixt volume 3% in fermentation bottle wherein, fermented liquid is collected after above-mentioned fermentation ends, the massfraction adding fermentating liquid volume 2% wherein is the oxalic acid solution of 30%, functional quality mark is the hydrochloric acid soln adjustment pH to 4.0 of 30%, again the fermented liquid after adjustment is put into whizzer centrifugation 2min under 600r/min, collect supernatant liquor and put into container, stir the 150 order attapulgites adding fermented liquid quality 15% after evenly wherein, after stirring 20min, leave standstill 1h, filter, collect filtrate, the filtrate of above-mentioned gained is mixed by solid-to-liquid ratio 1:3 with dehydrated alcohol, mixture is placed in ultrasonic cleaning instrument that frequency is 23KHz again vibrate and filter after 1h, collection filtered liquid is put into concentration tank and is concentrated 40% to original volume, subsequently concentrated solution is put into spray-drier and carry out spraying dry, Isphamycin can be obtained.
The Isphamycin of gained of the present invention obtains after testing: actual the tiring of fermented liquid is 27130 �� g/mL, and the content that Ledermycins is 0.56%, and dehydration tetracycline content is 0.29%, and the content of Isphamycin reaches 97.5%, and duomycin content is 1.8%.
Example 3
Hundred parts of ratio meters by weight, get 50 parts of dregs of beans, 13 parts of agar, 6 parts of blood meals, 22 portions of sucrose, 8 parts of massfractions be the sodium chloride solution of 12%, 0.8 part of dipotassium hydrogen phosphate and 0.2 part of potassium primary phosphate, after stirring evenly at 120 DEG C, sterilizing 40min, functional quality mark is the hydrochloric acid soln adjustment pH to 6.0 of 10%, obtains substratum, the substratum measuring the above-mentioned preparation of 40mL puts into 250mL triangular flask, stirrer is put into after being mixed by the glucose solution that duomycin bacterium slag and massfraction are 25% by solid-to-liquid ratio 1:3 again, after leaving standstill 15min after stirring 40min with 800r/min, collect 90mL supernatant liquid and put into Erlenmeyer flask, for subsequent use, 1:8 in mass ratio, Poria cocos and the Radix Astragali are put into pulverizer pulverize, cross 200 order sieves, particle after sieving is put into container, add the hydrochloric acid soln that massfraction is 5% wherein, flood particle 8cm, container is heated to 90 DEG C, after stirring 10h with rotating speed 120r/min, stop stirring heating, leave standstill 40mim, carry out filtration under diminished pressure, collect filtered liquid, 9:2:1 by volume again, by filtered liquid, massfraction be 10% magnesium nitrate solution and massfraction be that 15% ferric chloride Solution stirs evenly, functional quality mark is the hydrochloric acid soln adjustment pH to 5.5 of 15%, it is prepared into modification annex solution, triangular flask for subsequent use is put into microwave oscillator, at 600MHz, at 32 DEG C, after vibration 22h, by inoculum size 7%, culturing mixt in triangular flask is put into fermentation bottle, air flow is set as 1:1.8, and temperature is set as 32 DEG C, and rotating speed is 150r/min, fermentation 42h, every 8h add the modification annex solution of the above-mentioned preparation of culturing mixt volume 4% in fermentation bottle wherein, fermented liquid is collected after above-mentioned fermentation ends, the massfraction adding fermentating liquid volume 4% wherein is the oxalic acid solution of 30%, functional quality mark is the hydrochloric acid soln adjustment pH to 4.5 of 30%, again the fermented liquid after adjustment is put into whizzer centrifugation 5min under 700r/min, collect supernatant liquor and put into container, stir the 150 order attapulgites adding fermented liquid quality 20% after evenly wherein, after stirring 30min, leave standstill 2h, filter, collect filtrate, the filtrate of above-mentioned gained is mixed by solid-to-liquid ratio 1:3 with dehydrated alcohol, mixture is placed in ultrasonic cleaning instrument that frequency is 25KHz again vibrate and filter after 2h, collection filtered liquid is put into concentration tank and is concentrated 50% to original volume, subsequently concentrated solution is put into spray-drier and carry out spraying dry, Isphamycin can be obtained.
The Isphamycin of gained of the present invention obtains after testing: actual the tiring of fermented liquid is 26530 �� g/mL, and Ledermycin content 0.36%, dehydration tetracycline content 0.18%, and the content of Isphamycin reaches 98.9%, duomycin content 1.2%.
Claims (1)
1. the preparation method of an Isphamycin, it is characterised in that concrete preparation process is:
(1) hundred parts of ratios are counted by weight, get 40��50 parts of dregs of beans, 13��15 parts of agar, 6��8 parts of blood meals, 22��25 portions of sucrose, 8��10 parts of massfractions be the sodium chloride solution of 12%, 0.8��1.2 part of dipotassium hydrogen phosphate and 0.2��0.8 part of potassium primary phosphate, after stirring evenly at 115��120 DEG C, sterilizing 30��40min, functional quality mark is hydrochloric acid soln adjustment pH to 5.5��6.0 of 10%, obtains substratum;
(2) substratum measuring the above-mentioned preparation of 30��40mL puts into 250mL triangular flask, stirrer is put into after being mixed by the glucose solution that duomycin bacterium slag and massfraction are 20��25% by solid-to-liquid ratio 1:3 again, after leaving standstill 10��15min after stirring 30��40min with 600��800r/min, collect 70��90mL supernatant liquid and put into Erlenmeyer flask, for subsequent use;
(3) 1:8 in mass ratio, Poria cocos and the Radix Astragali are put into pulverizer pulverize, cross 200 order sieves, particle after sieving is put into container, add the hydrochloric acid soln that massfraction is 5% wherein, flood particle 6��8cm, container is heated to 80��90 DEG C, after stirring 8��10h with rotating speed 120r/min, stop stirring heating, leave standstill 30��40mim, carry out filtration under diminished pressure, collect filtered liquid, 9:2:1 by volume again, by filtered liquid, massfraction be 10% magnesium nitrate solution and massfraction be that 15% ferric chloride Solution stirs evenly, functional quality mark is hydrochloric acid soln adjustment pH to 5.0��5.5 of 15%, it is prepared into modification annex solution,
(4) triangular flask for subsequent use in step (2) is put into microwave oscillator, at 400��600MHz, at 28��32 DEG C, after vibration 20��22h, by inoculum size 5��7%, culturing mixt in triangular flask is put into fermentation bottle, air flow is set as 1:1.2��1.8, and temperature is set as 28��32 DEG C, and rotating speed is 120��150r/min, fermentation 36��42h, every 7��8h add the modification annex solution of the above-mentioned preparation of culturing mixt volume 3��4% in fermentation bottle wherein;
(5) after above-mentioned fermentation ends, fermented liquid is collected, adding fermentating liquid volume 2��4% massfraction wherein is the oxalic acid solution of 30%, functional quality mark is hydrochloric acid soln adjustment pH to 4.0��4.5 of 30%, again the fermented liquid after adjustment is put into whizzer, centrifugation 2��5min under 600��700r/min, collect supernatant liquor and put into container, stir the 150 order attapulgites adding fermented liquid quality 15��20% after evenly wherein, 1��2h is left standstill after stirring 20��30min, filter, collect filtrate;
(6) filtrate by above-mentioned gained mixes by solid-to-liquid ratio 1:3 with dehydrated alcohol, after mixture is placed in ultrasonic cleaning instrument vibration 1��2h that frequency is 23��25KHz again, filter, collection filtered liquid is put into concentration tank and is concentrated 40��50% to original volume, subsequently concentrated solution is put into spray-drier and carry out spraying dry, Isphamycin can be obtained.
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| CN201610155479.5A CN105624222A (en) | 2016-03-18 | 2016-03-18 | Method for preparing chlortetracycline hydrochloride |
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| CN201610155479.5A CN105624222A (en) | 2016-03-18 | 2016-03-18 | Method for preparing chlortetracycline hydrochloride |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114105804A (en) * | 2021-12-15 | 2022-03-01 | 浦城正大生化有限公司 | Preparation method of chlortetracycline hydrochloride |
| CN114195669A (en) * | 2021-12-08 | 2022-03-18 | 浦城正大生化有限公司 | Method for co-producing chlortetracycline hydrochloride and chlortetracycline premix |
| CN114276268A (en) * | 2021-08-09 | 2022-04-05 | 浦城正大生化有限公司 | Aureomycin hydrochloride with ultrahigh water solubility and high bioavailability |
| CN114276267A (en) * | 2021-08-09 | 2022-04-05 | 浦城正大生化有限公司 | Preparation method of ultrahigh water-soluble chlortetracycline hydrochloride |
-
2016
- 2016-03-18 CN CN201610155479.5A patent/CN105624222A/en not_active Withdrawn
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114276268A (en) * | 2021-08-09 | 2022-04-05 | 浦城正大生化有限公司 | Aureomycin hydrochloride with ultrahigh water solubility and high bioavailability |
| CN114276267A (en) * | 2021-08-09 | 2022-04-05 | 浦城正大生化有限公司 | Preparation method of ultrahigh water-soluble chlortetracycline hydrochloride |
| CN114276267B (en) * | 2021-08-09 | 2023-11-07 | 浦城正大生化有限公司 | Preparation method of super-high water-soluble aureomycin hydrochloride |
| CN114276268B (en) * | 2021-08-09 | 2023-11-07 | 浦城正大生化有限公司 | Super-high water-solubility and high bioavailability aureomycin hydrochloride |
| CN114195669A (en) * | 2021-12-08 | 2022-03-18 | 浦城正大生化有限公司 | Method for co-producing chlortetracycline hydrochloride and chlortetracycline premix |
| CN114195669B (en) * | 2021-12-08 | 2023-08-22 | 浦城正大生化有限公司 | Method for co-producing aureomycin hydrochloride and aureomycin premix |
| CN114105804A (en) * | 2021-12-15 | 2022-03-01 | 浦城正大生化有限公司 | Preparation method of chlortetracycline hydrochloride |
| CN114105804B (en) * | 2021-12-15 | 2023-09-15 | 浦城正大生化有限公司 | Preparation method of aureomycin hydrochloride |
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