CN1593422A - Method for preparing freeze dried cefathiamidine - Google Patents
Method for preparing freeze dried cefathiamidine Download PDFInfo
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- CN1593422A CN1593422A CN 03146824 CN03146824A CN1593422A CN 1593422 A CN1593422 A CN 1593422A CN 03146824 CN03146824 CN 03146824 CN 03146824 A CN03146824 A CN 03146824A CN 1593422 A CN1593422 A CN 1593422A
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- cefathiamidine
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Abstract
The invention provides a method for preparing freeze dried cefathiamidine which comprises the steps of, dissolving the purified crude product of cefathiamidine with water, adjusting pH to be 4.0-6.0, filtering, washing with slight amount of water, cooling the solution to -60 - -20 deg. C for solidifying, then slowly elevating temperature to 0-60 deg. C under high vacuum so as to gasify the moisture, and strictly controlling the freeze-drying curves.
Description
Technical field
The present invention relates to the freeze-drying method of cefathiamidine, particularly relating to water is solvent, makes the cryodesiccated method of cefathiamidine from-60 ℃ to 60 ℃.
Background technology
Cefathiamidine is chemical to be called (6R, 7R)-the 3[(acetyl group) methyl]-7-[α-(N, N '-diisopropylamidinateand sulfenyl)-acetamido]-8-oxo-5-thia-1-azabicyclo [4,2,0]-oct-2-ene-2-formic acid betaine.Molecular formula is C
19H
28N
4O
6S
2
Cefathiamidine is a beta-lactam antibiotic, antimicrobial spectrum is similar to cefalotin, stronger to staphylococcus aureus, Streptococcus viridans, pneumococcal effect, enterococcus there is unique antibacterial activity, to Hemolytic streptococcus, hemophilus influenza, viridans streptococci, diphtheria corynebacterium, clostridium tetani, escherichia coli, proteus mirabilis etc. also have certain effect in addition.This medicine is oral not to be absorbed, and the serum albumin combination rate is low, and it is the highest with bile to distribute in the body, and concentration is lower in the cerebral tissue.Not metabolism in the body is mainly discharged by urine.Cefathiamidine is mainly used in infection such as respiratory tract infection due to staphylococcus aureus, streptococcus pneumoniae and the streptococcus, biliary tract infection, urinary tract infection, gynecological infection, septicemia, pneumonia, meningitis.Use cefathiamidine aseptic crystallization powder clinically.
Cefathiamidine has the unique molecular structure of amphion inner salt, case of thermal instability, the main at present method preparation of adopting solvent crystallization.The know-why of this method is that the cefathiamidine crude product is adopted solvent processing, through nucleation, and control saturation history and rate of crystalline growth and make cefathiamidine crystal and reach the purpose of purification.The crystallization process advantage is a lower cost, and quality is better relatively; Shortcoming is to have used a large amount of solvents in crystallization process, thereby has formed the environmental pollution threat, and the cefathiamidine dissolution velocity of crystallization process preparation simultaneously is not good.
The purpose of this invention is to provide the freeze dried manufacture method of a kind of cefathiamidine, be cefathiamidine dissolving crude product that purification is crossed in water, generate the process of cefathiamidine crystal powder through lyophilization.
Summary of the invention
Technical solution of the present invention is the cefathiamidine dissolving crude product that water is crossed purification, after transferring pH to be 4.0～6.0, filter, with the low amounts of water washing, solution is cooled to-60～-20 ℃ and makes it to solidify, then under fine vacuum, slowly be warming up to 0～60 ℃ stage by stage, make the moisture gasification, strict simultaneously control freeze-drying curve finally obtains the cefathiamidine crystal powder that lyophilization prepares.
This freeze drying process still is lyophilizing operations such as bottle lyophilizing regardless of lyophilizing in batches, can implement.
The present invention drops into the cefathiamidine crude product that purification is crossed in reaction bulb, with stirring and dissolving under the purified water room temperature, be 5.3 with ammonia regulator solution pH, adds the 1g active carbon and stirs decolouring 30 minutes, filters, and washes with water; To put into the freeze dryer charging tray after filtrate and the washing liquid mixing, be cooled to-60 ℃ rapidly--20 ℃ make it to solidify, start freeze dryer, in-1.0 * 10
-2Slowly heat up under the crust vacuum, slowly heat up again after keeping lyophilizing.Slowly intensification 5-10 hour to 0 ℃-10 ℃, keep 0 ℃-10 ℃ slowly heated up again in lyophilizing 3-5 hour 2-4 hour to 35 ℃-40 ℃, kept 35 ℃ of-40 ℃ of continuation vacuum dryings 5-6 hour.
The present invention can will filtrate and washing liquid put into the freeze dryer charging tray after mixing, slowly cool to-20 ℃--30 ℃ make it primary solidification, are cooled to-45 ° more rapidly--60 ℃ make it full solidification.Start freeze dryer, in-1.0 * 10
-2Under the crust vacuum slowly intensification 4-8 hour to-10 ℃--20 ℃, keep-10 ℃--20 ℃ slowly heated up again in lyophilizing 3-5 hour 3-8 hour to 0 ℃-60 ℃, keep 0 ℃-15 ℃ after lyophilizing 1-6 hour, slowly heat up again 3-8 hour to 25 ℃-60 ℃ continued dry 1-6 hour.
The present invention cannot drop into the cefathiamidine crude product that purification is crossed in reaction bulb, in-10～5 ℃ of following stirring and dissolving, be 5.3 with ammonia regulator solution pH with purified water, adds the 1g active carbon and stirs decolouring 30 minutes, filters, and washes with water; To put into the freeze dryer charging tray after filtrate and the washing liquid mixing, be cooled to-50 ℃ rapidly--30 ℃ make it to solidify, start freeze dryer, in-1.0 * 10
-2Slowly heat up under the crust vacuum, slowly heat up again after keeping lyophilizing.Slowly intensification 7-15 hour to-10 ℃-10 ℃, keep-10 ℃-10 ℃ slowly heated up again in lyophilizing 3-8 hour 2-5 hour to 25 ℃-50 ℃, kept 25 ℃ of-50 ℃ of continuation vacuum dryings 1.5-8 hour.
Advantage of the present invention is that cost is cheaper than crystallization process, yield is high than crystallization process, because the cefathiamidine crude product has passed through purification, end product quality is guaranteed equally, and the lyophilizing overall process only is solvent with water, environment is not constituted any pollution threat, adopt the cefathiamidine of lyophilization preparation faster simultaneously than the dissolution velocity of crystallization process preparation.
The specific embodiment
Embodiment one
Dropping into the cefathiamidine crude product that the 60g purification is crossed in the 250ml reaction bulb, with stirring and dissolving under the 90ml purified water room temperature, is 5.3 with ammonia regulator solution pH, adds the 1g active carbon and stirs decolouring 30 minutes, filters, and uses the 10ml water washing.To put into the freeze dryer charging tray after filtrate and the washing liquid mixing, be cooled to-60 ℃ rapidly and make it to solidify, start freeze dryer, in-1.0 * 10
-2Slowly heated up 10 hours to 0 ℃ under the crust vacuum, keep 0 ℃ of lyophilizing and slowly heated up again in 5 hours 4 hours to 35 ℃, kept 35 ℃ of continuation vacuum dryings 5 hours, get cefathiamidine freeze-dried powder 58.2 grams.
Embodiment two
Dropping into the cefathiamidine crude product that the 60g purification is crossed in the 250ml reaction bulb, with stirring and dissolving under the 90ml purified water room temperature, is 5.3 with ammonia regulator solution pH, adds the 1g active carbon and stirs decolouring 30 minutes, filters, and uses the 10ml water washing.To put into the freeze dryer charging tray after filtrate and the washing liquid mixing, be cooled to-40 ℃ rapidly and make it to solidify, start freeze dryer, in-1.0 * 10
-2Slowly heated up 5 hours to 10 ℃ under the crust vacuum, keep 10 ℃ of lyophilizing and slowly heated up again in 3 hours 2 hours to 40 ℃, kept 40 ℃ of continuation vacuum dryings 6 hours, get cefathiamidine freeze-dried powder 57.8 grams.
Embodiment three
Dropping into the cefathiamidine crude product that the 60g purification is crossed in the 250ml reaction bulb, in 0～5 ℃ of following stirring and dissolving, is 5.3 with ammonia regulator solution pH with the 100ml purified water, adds the 1g active carbon and stirs decolouring 30 minutes, filters, and uses the 15ml water washing.To put into the freeze dryer charging tray after filtrate and the washing liquid mixing, be cooled to-30 ℃ rapidly and make it to solidify, start freeze dryer, in-1.0 * 10
-2Cling under the vacuum and slowly heated up 15 hours to 5 ℃, keep 5 ℃ of lyophilizing and slowly heated up again in 7 hours 2 hours to 25 ℃, keep 25 ℃ and continued dry 8 hours, get cefathiamidine freeze-dried powder 58.5 grams.
Embodiment four
Dropping into the cefathiamidine crude product that the 60g purification is crossed in the 250ml reaction bulb, in 0～5 ℃ of following stirring and dissolving, is 5.3 with ammonia regulator solution pH with the 100ml purified water, adds the 1g active carbon and stirs decolouring 30 minutes, filters, and uses the 15ml water washing.To put into the freeze dryer charging tray after filtrate and the washing liquid mixing, be cooled to-50 ℃ rapidly and make it to solidify, start freeze dryer, in-1.0 * 10
-2Cling under the vacuum and slowly heated up 7 hours to-10 ℃, keep-10 ℃ of lyophilizing and slowly heated up again in 3 hours 5 hours to 45 ℃, keep 45 ℃ and continued dry 2 hours, get cefathiamidine freeze-dried powder 57.3 grams.
Embodiment five
Dropping into the cefathiamidine crude product that the 60g purification is crossed in the 250ml reaction bulb, in-10～-5 ℃ of following stirring and dissolving, is 5.3 with ammonia regulator solution pH with the 120ml purified water, adds the 1g active carbon and stirs decolouring 30 minutes, filters, and uses the 15ml water washing.To put into the freeze dryer charging tray after filtrate and the washing liquid mixing, be cooled to-40 ℃ rapidly and make it to solidify, start freeze dryer, in-1.0 * 10
-2Cling under the vacuum and slowly heated up 12 hours to 10 ℃, keep 10 ℃ of lyophilizing and slowly heated up again in 8 hours 5 hours to 50 ℃, keep 50 ℃ and continued dry 1.5 hours, get cefathiamidine freeze-dried powder 58.1 grams.
Embodiment six
Dropping into the cefathiamidine crude product that the 60g purification is crossed in the 250ml reaction bulb, with 120ml purified water stirring and dissolving under room temperature, is 5.3 with ammonia regulator solution pH, adds the 1g active carbon and stirs decolouring 30 minutes, filters, and uses the 10ml water washing.With putting into the freeze dryer charging tray after filtrate and the washing liquid mixing, slowly cool to-20 ℃ and make it primary solidification, be cooled to-60 ℃ more rapidly and make it full solidification, start freeze dryer, in-1.0 * 10
-2Slowly heated up 6 hours to-15 ℃ under the crust vacuum, keep-15 ℃ of lyophilizing and slowly heated up again in 5 hours 3 hours to 0 ℃, keep 0 ℃ of lyophilizing and slowly heated up again after 3 hours 3 hours to 25 ℃ and continued dry 6 hours, cefathiamidine freeze-dried powder 58.7 restrains.
Embodiment seven
Dropping into the cefathiamidine crude product that the 60g purification is crossed in the 250ml reaction bulb, with 90ml purified water stirring and dissolving under room temperature, is 5.3 with ammonia regulator solution pH, adds the 1g active carbon and stirs decolouring 30 minutes, filters, and uses the 20ml water washing.With putting into the freeze dryer charging tray after filtrate and the washing liquid mixing, slowly cool to-30 ℃ and make it primary solidification, be cooled to-60 ℃ more rapidly and make it full solidification, start freeze dryer, in-1.0 * 10
-2Slowly heated up 4 hours to-20 ℃ under the crust vacuum, keep-20 ℃ of lyophilizing and slowly heated up again in 3 hours 3 hours to 10 ℃, keep 10 ℃ of lyophilizing and slowly heated up again after 5 hours 8 hours to 60 ℃ and continued dry 1 hour, cefathiamidine freeze-dried powder 57.7 restrains.
Embodiment eight
Dropping into the cefathiamidine crude product that the 60g purification is crossed in the 250ml reaction bulb, with 100ml purified water stirring and dissolving under room temperature, is 5.3 with ammonia regulator solution pH, adds the 1g active carbon and stirs decolouring 30 minutes, filters, and uses the 20ml water washing.With putting into the freeze dryer charging tray after filtrate and the washing liquid mixing, slowly cool to-20 ℃ and make it primary solidification, be cooled to-45 ℃ more rapidly and make it full solidification, start freeze dryer, in-1.0 * 10
-2Slowly heated up 8 hours to-10 ℃ under the crust vacuum, keep-10 ℃ of lyophilizing and slowly heated up again in 4 hours 6 hours to 15 ℃, keep 15 ℃ of lyophilizing and slowly heated up again after 5 hours 5 hours to 35 ℃ and continued dry 3 hours, cefathiamidine freeze-dried powder 58.0 restrains.
Claims (10)
1, the freeze dried manufacture method of a kind of cefathiamidine, with cefathiamidine crude product solvent processing, it is characterized in that the cefathiamidine dissolving crude product that water is crossed purification, after accent pH is 4.0～6.0, filter, with the low amounts of water washing, solution is cooled to-60～-20 ℃ and makes it to solidify, then under fine vacuum, slowly be warming up to 0～60 ℃ stage by stage, make the moisture gasification, control freeze-drying curve simultaneously, obtain the cefathiamidine crystal powder of lyophilization preparation.
2, the freeze dried manufacture method of cefathiamidine according to claim 1 is characterized in that described freeze drying process adopts lyophilizing operational approach in batches or bottle lyophilizing operational approach.
3, the freeze dried manufacture method of cefathiamidine according to claim 1 and 2, it is characterized in that in reaction bulb, dropping into the cefathiamidine crude product that purification is crossed, with stirring and dissolving under the purified water room temperature, with ammonia regulator solution pH is 5.3, add the 1g active carbon and stir decolouring 30 minutes, filter, wash with water; To put into the freeze dryer charging tray after filtrate and the washing liquid mixing, be cooled to-60 ℃ rapidly--20 ℃ make it to solidify, start freeze dryer, in-1.0 * 10
-2Slowly heat up under the crust vacuum, slowly heat up again after keeping lyophilizing.
4, the freeze dried manufacture method of cefathiamidine according to claim 3 is characterized in that starting freeze dryer, in-1.0 * 10
-2Under the crust vacuum slowly intensification 5-10 hour to 0 ℃-10 ℃, keep 0 ℃-10 ℃ slowly heated up again in lyophilizing 3-5 hour 2-4 hour to 35 ℃-40 ℃, kept 35 ℃ of-40 ℃ of continuation vacuum dryings 5-6 hour.
5, the freeze dried manufacture method of cefathiamidine according to claim 3, it is characterized in that will filtrate and washing liquid put into the freeze dryer charging tray after mixing, slowly cool to-20 ℃--30 ℃ make it primary solidification, are cooled to rapidly-45--60 ℃ makes it full solidification again.
6, the freeze dried manufacture method of cefathiamidine according to claim 5 is characterized in that starting freeze dryer, in-1.0 * 10
-2Under the crust vacuum slowly intensification 4-8 hour to-10 ℃--20 ℃, keep-10 ℃--20 ℃ slowly heated up again in lyophilizing 3-5 hour 3-8 hour to 0 ℃-60 ℃, keep 0 ℃-15 ℃ after lyophilizing 1-6 hour, slowly heat up again 3-8 hour to 25 ℃-60 ℃ continued dry 1-6 hour.
7, the freeze dried manufacture method of cefathiamidine according to claim 1 and 2, it is characterized in that in reaction bulb, dropping into the cefathiamidine crude product that purification is crossed, with purified water in-10～5 ℃ of following stirring and dissolving, with ammonia regulator solution pH is 5.3, add the 1g active carbon and stir decolouring 30 minutes, filter, wash with water; To put into the freeze dryer charging tray after filtrate and the washing liquid mixing, be cooled to-50 ℃ rapidly--30 ℃ make it to solidify, start freeze dryer, in-1.0 * 10
-2Slowly heat up under the crust vacuum, slowly heat up again after keeping lyophilizing.
8, the freeze dried manufacture method of cefathiamidine according to claim 7 is characterized in that starting freeze dryer, in-1.0 * 10
-2Under the crust vacuum slowly intensification 7-15 hour to-10 ℃-10 ℃, keep-10 ℃-10 ℃ slowly heated up again in lyophilizing 3-8 hour 2-5 hour to 25 ℃-50 ℃, kept 25 ℃ of-50 ℃ of continuation vacuum dryings 1.5-8 hour.
9, the freeze dried manufacture method of cefathiamidine according to claim 8 is characterized in that starting freeze dryer, in-1.0 * 10
-2Slowly heated up 7 hours to-10 ℃ under the crust vacuum, keep-10 ℃ of lyophilizing and slowly heated up again in 3 hours 5 hours to 45 ℃, keep 45 ℃ and continued dry 2 hours.
10, the freeze dried manufacture method of cefathiamidine according to claim 8 is characterized in that starting freeze dryer, in-1.0 * 10
-2Slowly heated up 12 hours to 10 ℃ under the crust vacuum, keep 10 ℃ of lyophilizing and slowly heated up again in 8 hours 5 hours to 50 ℃, keep 50 ℃ and continued dry 1.5 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031468241A CN100350910C (en) | 2003-09-10 | 2003-09-10 | Method for preparing freeze dried cefathiamidine |
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|---|---|---|---|
| CNB031468241A CN100350910C (en) | 2003-09-10 | 2003-09-10 | Method for preparing freeze dried cefathiamidine |
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| CN1593422A true CN1593422A (en) | 2005-03-16 |
| CN100350910C CN100350910C (en) | 2007-11-28 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010031262A1 (en) * | 2008-09-17 | 2010-03-25 | 上海天伟生物制药有限公司 | A glycoprotein composition almost containing no subunit and preparation method thereof |
| CN102319221A (en) * | 2009-08-31 | 2012-01-18 | 重庆福安药业(集团)股份有限公司 | Cefsulodin sodium lyophilized powder, cefsulodin sodium lyophilized powder preparation and their preparation method |
| CN104059088A (en) * | 2014-07-07 | 2014-09-24 | 江苏汉斯通药业有限公司 | Preparation technology for cefathiamidine |
| CN104530083A (en) * | 2014-12-31 | 2015-04-22 | 天津大学 | New form crystal of cefathiamidine compound and preparation method of new crystal-form crystal |
| CN104524585A (en) * | 2014-12-08 | 2015-04-22 | 悦康药业集团有限公司 | Cefathiamidine composition |
| CN105646534A (en) * | 2016-02-18 | 2016-06-08 | 海南灵康制药有限公司 | Novel-crystal-form cefathiamidine compound adopting crystal product molecular assembly and form optimization technology in particle process and preparation |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0782149A (en) * | 1993-06-30 | 1995-03-28 | Kaken Pharmaceut Co Ltd | Stabilized preparation of cephem-based antibiotic |
| JPH0725875A (en) * | 1993-07-15 | 1995-01-27 | Taisho Pharmaceut Co Ltd | Aromatic alkaloid compound |
| JP2678737B2 (en) * | 1994-10-06 | 1997-11-17 | セイコーエプソン株式会社 | Organozinc compound |
| CN1385434A (en) * | 2002-06-10 | 2002-12-18 | 广州白云山制药股份有限公司广州白云山化学制药厂 | Method for making cefathiamidine crystal |
| CN1209364C (en) * | 2003-01-28 | 2005-07-06 | 广州白云山制药股份有限公司 | Amine salt of cefathiamiding, its preparing method and application |
-
2003
- 2003-09-10 CN CNB031468241A patent/CN100350910C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010031262A1 (en) * | 2008-09-17 | 2010-03-25 | 上海天伟生物制药有限公司 | A glycoprotein composition almost containing no subunit and preparation method thereof |
| CN102319221A (en) * | 2009-08-31 | 2012-01-18 | 重庆福安药业(集团)股份有限公司 | Cefsulodin sodium lyophilized powder, cefsulodin sodium lyophilized powder preparation and their preparation method |
| CN104059088A (en) * | 2014-07-07 | 2014-09-24 | 江苏汉斯通药业有限公司 | Preparation technology for cefathiamidine |
| CN104524585A (en) * | 2014-12-08 | 2015-04-22 | 悦康药业集团有限公司 | Cefathiamidine composition |
| CN104524585B (en) * | 2014-12-08 | 2018-11-09 | 悦康药业集团有限公司 | Cefathiamidine composition |
| CN104530083A (en) * | 2014-12-31 | 2015-04-22 | 天津大学 | New form crystal of cefathiamidine compound and preparation method of new crystal-form crystal |
| CN105646534A (en) * | 2016-02-18 | 2016-06-08 | 海南灵康制药有限公司 | Novel-crystal-form cefathiamidine compound adopting crystal product molecular assembly and form optimization technology in particle process and preparation |
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|---|---|
| CN100350910C (en) | 2007-11-28 |
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Assignee: Guangdong Liguo Pharmacy Co., Ltd. Assignor: Shenzhen Liguo Drug Research Co., Ltd. Contract fulfillment period: 2008.7.11 to 2014.7.10 contract change Contract record no.: 2008440000243 Denomination of invention: Method for preparing freeze dried cefathiamidine Granted publication date: 20071128 License type: Exclusive license Record date: 2008.9.22 |
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Free format text: EXCLUSIVE LICENCE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.7.11 TO 2014.7.10 Name of requester: GUANGDONG LIGUO PHARMACY CO., LTD. Effective date: 20080922 |
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Granted publication date: 20071128 Termination date: 20100910 |