CN104163774A - Method for improving output of aureomycin calcium salt - Google Patents

Method for improving output of aureomycin calcium salt Download PDF

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Publication number
CN104163774A
CN104163774A CN201410368510.4A CN201410368510A CN104163774A CN 104163774 A CN104163774 A CN 104163774A CN 201410368510 A CN201410368510 A CN 201410368510A CN 104163774 A CN104163774 A CN 104163774A
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aureomycin
calcium salt
duomycin
solution
output
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CN104163774B (en
Inventor
张雪峥
李书至
方孝武
马德寿
孙庆峰
常坤
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ZHUMADIAN HUAZHONG CHIA TAI CO Ltd
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ZHUMADIAN HUAZHONG CHIA TAI CO Ltd
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Abstract

The invention belongs to the technical field of preparation of aureomycin, and concretely relates to an improvement technology for improving the output of an aureomycin semi-finished product, namely an aureomycin calcium salt. The method comprises: using a sodium hydroxide solution to adjust pH of an aureomycin fermentation solution, adding calcium carbonate, performing routine production, and the like. Compared with a conventional aureomycin calcium salt production technology, the method belongs to an improvement production technology. Through multi-time experiments for adjusting, an optimum pH value of the aureomycin fermentation solution is explored, and the solubility of calcium carbonate is furthest reduced, so that the output of the aureomycin calcium salt is improved, and the quality of the obtained finished product accords with correlated quality standard requirements. Also, through the improvement production technology, the content of aureomycin in discharged waste water is reduced to about 30%, and reducing of sewage processing cost and environment protection are facilitated. Therefore, the method possesses relatively good economic and social benefit.

Description

A kind of method that improves duomycin calcium salt output
Technical field
The invention belongs to duomycin preparing technical field, be specifically related to a kind of improvement technique that duomycin work in-process are duomycin calcium salt output that improves.
Background technology
Duomycin is a kind of tetracycline antibiotics, is also important a member in such microbiotic, and its chemical name is 6-methyl-4-dimethylamino-3,6,10,12,12a-penta hydroxy group-1, the chloro-Isosorbide-5-Nitrae in 11-dioxo-7,4a, 5,5a, 6,11,12a-octahydro-2-tetracene methane amide, it finds to have had the history of more than 60 year apart from modern.
In prior art, the general fermentative Production that adopts of duomycin preparation, wherein duomycin calcium salt is that Aureomycin fermentation liquor adds after calcium carbonate pre-treatment, carries out filter press, dry gained duomycin work in-process.Because Aureomycin fermentation liquor pH is in 6.0 left and right, be acid, and calcium carbonate is alkalescence, therefore often cause calcium ion to run off preparing when duomycin work in-process are duomycin calcium salt, cause the loss of duomycin calcium salt, thereby reduced the output of duomycin.
Summary of the invention
The object of the invention is to provide that a kind of to improve duomycin work in-process in duomycin preparation process be the improvement technique of duomycin calcium salt output.
The technical scheme that the present invention takes is as follows:
A method that improves duomycin calcium salt output, comprises the following steps:
(1) get solution after Ferment of DM, add sodium hydroxide solution to adjust pH to 7.3;
(2) step (1) is regulated the rear solution of pH value add calcium carbonate, stir;
(3) step (2) solution is carried out to Plate Filtration, after filtering, filtration cakes torrefaction obtains duomycin calcium salt finished product.
Sodium hydroxide solution in step (1) adopts the sodium hydroxide solution that massfraction is 30%.
The present invention is compared to existing aureomycin calcium technology of threonates, belong to a kind of follow-on production technique, by many experiments, adjust, explore and adjust Aureomycin fermentation liquor optimal ph, can reduce to greatest extent the solubleness of calcium carbonate, thereby improve the output of duomycin calcium salt, and the quality of gained finished product meets correlated quality standard-required; The present invention simultaneously, by improvement of production process, makes the duomycin content in institute's waste discharge reduce by 30% left and right, is conducive to reduce cost of sewage disposal and environment protection.Thereby in general, the present invention has good economic and social profit.
Embodiment
Below in conjunction with embodiment the present invention will be further explained explanation.
embodiment 1
The method of raising duomycin calcium salt output provided by the present invention, comprises the following steps:
(1) get solution after Ferment of DM, add sodium hydroxide solution to adjust pH to 7.3;
(2) step (1) is regulated the rear solution of pH value add as calcium carbonate, stir;
(3) step (2) solution is carried out to Plate Filtration, after filtering, filtration cakes torrefaction obtains duomycin calcium salt finished product.
Sodium hydroxide solution in step (1) adopts the sodium hydroxide solution that mass fraction is 30%.
The present embodiment is specific as follows:
(1) get Aureomycin fermentation liquor 52m 3, add 125kg 30% sodium hydroxide and adjust pH to 7.3,
(2) step (1) is regulated to the rear solution of pH value, according to measuring duomycin content 237g/kg, add 300kg calcium carbonate, stir 45min, guarantee to stir;
(3) step (2) solution is carried out to Plate Filtration, filter 70min, after filtering, filter cake enters the dry 1.5h of drying tower, obtain duomycin calcium salt finished product, main detected result is as follows: dry biomass content is 9.38%, amount to 15%CTC(Isphamycin) output 8142kg, activity in filtrate 295u/ml, meets correlated quality standard.
Duomycin activity in filtrate detects as follows and detects: get a certain amount of Aureomycin fermentation liquor, add appropriate oxalic acid acidifying, filtration, utilize spectrophotometer to detect, read absorbancy, calculating is tired.
Duomycin content detects in the following manner: instrument adopts Agilent chromatographic system; Chromatographic condition: pillar: the Welch(month rising sun); Column temperature: 30 ℃; Wavelength: 360nm; Moving phase: oxalic acid: acetonitrile: methyl alcohol=71:16:13; Flow velocity: 1.2ml/min.
For the improved technique effect of explanation the present invention, contriver further be take existing technique as contrast, is not regulating in pH value situation, has carried out experiment and detect under the same terms, and particular case is as follows:
(1) get Aureomycin fermentation liquor 52m 3;
(2) to solution in step (1), according to measuring duomycin content 237g/kg, add 300kg calcium carbonate, stir 45min, guarantee to stir;
(3) step (2) solution is carried out to Plate Filtration, filter 70min, after filtering, filter cake enters the dry 1.5h of drying tower, obtain duomycin calcium salt finished product, main detected result is as follows: dry-matter is 8.38%, amounts to 15%CTC output 7784kg, activity in filtrate 376u/ml, meets correlated quality standard.
From above-mentioned contrast, can find out, with 52m 3aureomycin fermentation liquor is example, adopts after industry of the present invention, amounts to 15%CTC output and has promoted 358Kg, has promoted approximately 4.6% output, thereby has good actual production meaning.
embodiment 2
The present embodiment detailed process is as follows:
(1) get Aureomycin fermentation liquor 51m 3, add 125kg 30% sodium hydroxide and adjust pH to 7.3,
(2) step (1) is regulated to the rear solution of pH value, according to measuring duomycin content 245g/kg, add 300kg calcium carbonate, stir 45min, guarantee to stir;
(3) step (2) solution is carried out to Plate Filtration, filter 70min, after filtering, filter cake enters the dry 1.5h of drying tower, obtain duomycin calcium salt finished product, main detected result is as follows: dry-matter is 9.26%, amounts to 15%CTC output 8042kg, activity in filtrate 305u/ml, meets correlated quality standard.
Take existing industry as contrast, do not regulate in pH value situation,
(1) get Aureomycin fermentation liquor 51m 3;
(2) to solution in step (1), according to measuring duomycin content 245g/kg, add 300kg calcium carbonate, stir 45min, guarantee to stir;
(3) step (2) solution is carried out to Plate Filtration, filter 70min, after filtering, filter cake enters the dry 1.5h of drying tower, obtain duomycin calcium salt finished product, main detected result is as follows: dry-matter is 8.42%, amounts to 15%CTC output 7698kg, activity in filtrate 390u/ml, meets correlated quality standard.
From above-mentioned contrast, can find out, with 51m 3duomycin lotion is example, adopts after industry of the present invention, amounts to 15%CTC output and has promoted 344Kg, has promoted approximately 4.5% output, thereby has good actual production meaning.
embodiment 3
The present embodiment detailed process is as follows:
(1) get Aureomycin fermentation liquor 51.6m 3, add 125kg 30% sodium hydroxide and adjust pH to 7.3;
(2) step (1) is regulated to the rear solution of pH value, according to measuring duomycin content 238g/kg, add 300kg calcium carbonate, stir 45min, guarantee to stir;
(3) step (2) solution is carried out to Plate Filtration, filter 70min, after filtering, filter cake enters the dry 1.5h of drying tower, obtain duomycin calcium salt finished product, main detected result is as follows: dry-matter is 8.95%, amounts to 15%CTC output 8092kg, activity in filtrate 289u/ml, meets correlated quality standard.
Take existing industry as contrast, do not regulate in pH value situation,
(1) get Aureomycin fermentation liquor 51.6m 3;
(2) to solution in step (1), according to measuring duomycin content 238g/kg, add 300kg calcium carbonate, stir 45min, guarantee to stir;
(3) step (2) solution is carried out to Plate Filtration, filter 70min, after filtering, filter cake enters the dry 1.5h of drying tower, obtain duomycin calcium salt finished product, main detected result is as follows: dry-matter is 8.52%, amounts to 15%CTC output 7604kg, activity in filtrate 385u/ml, meets correlated quality standard.
From above-mentioned contrast, can find out, with 51.6m 3aureomycin fermentation liquor is example, adopts after industry of the present invention, amounts to 15%CTC output and has promoted 488Kg, has promoted approximately 6.4% output, thereby has good actual production meaning.
From above-described embodiment, can find out; adopt after the present invention; by adjusting the pH value of Aureomycin fermentation liquor; finally amount to 15%CTC output and all have raising in various degree; and the present invention passes through improvement of production process; make the duomycin content in institute's waste discharge also reduce by 30% left and right, be beneficial to environment protection, thereby the present invention has good social and economic effects.

Claims (2)

1. a method that improves duomycin calcium salt output, is characterized in that, the method comprises the following steps:
(1) get solution after Ferment of DM, add sodium hydroxide solution to adjust pH to 7.3;
(2) step (1) is regulated the rear solution of pH value add calcium carbonate, stir;
(3) step (2) solution is carried out to Plate Filtration, after filtering, filtration cakes torrefaction obtains duomycin calcium salt finished product.
2. improve as claimed in claim 1 the method for duomycin calcium salt output, it is characterized in that, the sodium hydroxide solution massfraction in step (1) is 30%.
CN201410368510.4A 2014-07-30 2014-07-30 A kind of method improving aureomycin calcium salt yield Active CN104163774B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114848599A (en) * 2022-06-09 2022-08-05 驻马店华中正大有限公司 High-stability aureomycin premix and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101863797A (en) * 2010-07-07 2010-10-20 福建省福抗药业股份有限公司 New process for preparing chlortetracycline hydrochloride
CN102899377A (en) * 2012-10-31 2013-01-30 金河生物科技股份有限公司 Preparation method of chlortetracycline premix
CN102898326A (en) * 2012-10-31 2013-01-30 金河生物科技股份有限公司 Preparation method of chlortetracycline hydrochloride

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101863797A (en) * 2010-07-07 2010-10-20 福建省福抗药业股份有限公司 New process for preparing chlortetracycline hydrochloride
CN102899377A (en) * 2012-10-31 2013-01-30 金河生物科技股份有限公司 Preparation method of chlortetracycline premix
CN102898326A (en) * 2012-10-31 2013-01-30 金河生物科技股份有限公司 Preparation method of chlortetracycline hydrochloride

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114848599A (en) * 2022-06-09 2022-08-05 驻马店华中正大有限公司 High-stability aureomycin premix and preparation method thereof
CN114848599B (en) * 2022-06-09 2023-10-13 驻马店华中正大有限公司 High-stability aureomycin premix and preparation method thereof

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Inventor after: Zhang Xuezheng

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