CN111196818A - Preparation method of ceftazidime for injection - Google Patents
Preparation method of ceftazidime for injection Download PDFInfo
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- CN111196818A CN111196818A CN201811376030.7A CN201811376030A CN111196818A CN 111196818 A CN111196818 A CN 111196818A CN 201811376030 A CN201811376030 A CN 201811376030A CN 111196818 A CN111196818 A CN 111196818A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D501/00—Heterocyclic compounds containing 5-thia-1-azabicyclo [4.2.0] octane ring systems, i.e. compounds containing a ring system of the formula:, e.g. cephalosporins; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
- C07D501/14—Compounds having a nitrogen atom directly attached in position 7
- C07D501/16—Compounds having a nitrogen atom directly attached in position 7 with a double bond between positions 2 and 3
- C07D501/20—7-Acylaminocephalosporanic or substituted 7-acylaminocephalosporanic acids in which the acyl radicals are derived from carboxylic acids
- C07D501/24—7-Acylaminocephalosporanic or substituted 7-acylaminocephalosporanic acids in which the acyl radicals are derived from carboxylic acids with hydrocarbon radicals, substituted by hetero atoms or hetero rings, attached in position 3
- C07D501/38—Methylene radicals, substituted by nitrogen atoms; Lactams thereof with the 2-carboxyl group; Methylene radicals substituted by nitrogen-containing hetero rings attached by the ring nitrogen atom; Quaternary compounds thereof
- C07D501/46—Methylene radicals, substituted by nitrogen atoms; Lactams thereof with the 2-carboxyl group; Methylene radicals substituted by nitrogen-containing hetero rings attached by the ring nitrogen atom; Quaternary compounds thereof with the 7-amino radical acylated by carboxylic acids containing hetero rings
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D501/00—Heterocyclic compounds containing 5-thia-1-azabicyclo [4.2.0] octane ring systems, i.e. compounds containing a ring system of the formula:, e.g. cephalosporins; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
- C07D501/02—Preparation
- C07D501/12—Separation; Purification
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- Cephalosporin Compounds (AREA)
Abstract
The invention discloses a preparation method of ceftazidime for injection, which comprises the following steps: adding the ceftazidime crude product into water for injection, adjusting the pH value, and stirring until the ceftazidime crude product is dissolved to obtain a ceftazidime solution 1; adding activated carbon into the ceftazidime solution 1, preserving heat, decoloring and filtering to obtain a ceftazidime solution 2; a part of the ceftazidime solution 2 is precipitated by a solvent-antisolvent to obtain a ceftazidime suspension; filtering to obtain a wet ceftazidime product; and adjusting the pH value of the ceftazidime solution 2 to 3.5-4.0 to obtain a ceftazidime solution 3; adding the ceftazidime wet product, crystallizing and filtering to obtain the ceftazidime for injection.
Description
Technical Field
The invention belongs to the technical field of medicine; relates to a preparation method of ceftazidime, in particular to a preparation method of ceftazidime for injection.
Background
Ceftazidime is a third generation cephalosporin. The chemical name of ceftazidime is: 1- [ [7- (2-amino-4-thiazolyl) - [ (1-carboxy-1-methylethoxy) imine ] acetyl ] amino ] -2-carboxy-8-oxo-5-thia-1-azabicyclo [4,2,0] -2-octen-3-yl ] methyl ] pyridinium hydroxide inner salt having a molecular weight of 546.6. Ceftazidime is a white or off-white crystalline powder, slightly soluble in water or methanol, and insoluble in acetone or chloroform. Ceftazidime for injection and ceftazidime raw materials have been collected in the second part of the chinese pharmacopoeia, 2000 edition, 2005 edition, 2010 edition and 2015 edition.
The ceftazidime has wide antibacterial spectrum and high antibacterial activity, is stable to various β -lactamase and has high activity to pseudomonas aeruginosa, and in addition, the ceftazidime is also effective to gram-positive bacilli and gram-negative bacilli and is suitable for single infection and mixed infection caused by sensitive bacteria.
However, the ceftazidime raw material is easily affected by environmental factors (pH value, temperature and illumination), ring opening, degradation and polymerization reaction are easily generated after long-time storage or placement, color change is caused, and related substances, ceftazidime polymer and other impurities are generated. It is currently the prevailing view that these impurities, especially the ceftazidime polymer, are allergens responsible for the allergic reactions of ceftazidime drugs. Therefore, various means have been adopted to improve the purity of ceftazidime as a raw material.
For example, british patent GB2063871A discloses a process for the preparation of ceftazidime by dissolving ceftazidime hydrochloride in water, adjusting the pH to 3.3-4.0 with a base and then crystallizing to obtain ceftazidime pentahydrate crystals. US patent US4954624A discloses a process for the crystallization of ceftazidime. Dissolving ceftazidime hydrochloride in ice water, adjusting the pH value to be 0.7-0.8, and crystallizing after adjusting the pH value to be 4.0 by using sodium hydroxide at the temperature of below 10 ℃. After 2 hours of crystallization, the pH value is adjusted to 3.6, and then the ceftazidime pentahydrate crystal is obtained after 3 hours of crystallization at 5 ℃.
Chinese patent CN1328281C discloses a method for purifying ceftazidime. Adding ceftazidime pentahydrate with high impure polymer content into water, adding acid to dissolve the ceftazidime pentahydrate, and then adjusting the pH value to 1.5-2.5; precipitating, filtering, and adjusting pH of the filtrate to 3.5-4.8 with alkali; and crystallizing to obtain the ceftazidime pentahydrate.
However, if direct crystallization is selected, the purity of the ceftazidime pentahydrate is low, and the content of related substances and polymers is high. If recrystallization is to be carried out by adjusting the pH with an acid, an additional preparation of an acid solution is required, and the yield is lowered. In conclusion, the above-mentioned means still do not solve the problem of impurities generated by environmental factors after long-term storage or storage of ceftazidime well.
On the other hand, there are increasing reports of microchannel reactors in the preparation of nanoparticles. Compared with the conventional reaction system, the microchannel reactor has incomparable advantages of high mass transfer rate, rapid and uniform mixing, narrow residence time distribution and the like. However, the microchannel reactor is mainly used to control the size of nanoparticles and their distribution, and is less reported to be used in a purification process of drugs.
Therefore, a preparation method of ceftazidime for injection is needed, and the method can improve the yield and purity of ceftazidime for injection.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of ceftazidime for injection, which has high yield and purity.
To achieve the above objects, in one aspect, the present invention provides a method for preparing ceftazidime for injection, the method comprising:
(1) adding the ceftazidime crude product into water for injection, adding acid at 0-5 ℃ to adjust the pH value to 1.5-2.5, and stirring until the ceftazidime crude product is dissolved to obtain a ceftazidime solution 1;
(2) adding activated carbon into the ceftazidime solution 1, preserving heat, decoloring and filtering to obtain a ceftazidime solution 2;
(3) a part of the ceftazidime solution 2 is precipitated by a solvent-antisolvent to obtain a ceftazidime suspension;
(4) filtering the ceftazidime suspension to obtain a wet ceftazidime product; and the number of the first and second groups,
(5) adding alkali into the ceftazidime solution 2 to adjust the pH value to 3.5-4.0 at 0-5 ℃ to obtain a ceftazidime solution 3; adding a wet ceftazidime product into the mixture, crystallizing and filtering to obtain the ceftazidime for injection.
The preparation method according to the present invention, wherein the acid of step (1) is selected from concentrated hydrochloric acid, concentrated sulfuric acid, concentrated hydrobromic acid and concentrated phosphoric acid, preferably selected from concentrated hydrochloric acid, concentrated sulfuric acid and concentrated phosphoric acid, and more preferably selected from concentrated hydrochloric acid and concentrated sulfuric acid.
In a particular embodiment, the acid of step (1) is selected from concentrated 35wt% hydrochloric acid.
The production method according to the present invention, wherein the pH value in step (1) is preferably 1.6 to 2.4, more preferably 1.7 to 2.3, and, most preferably, 1.8 to 2.2.
In a specific embodiment, said pH of step (1) is 2.0.
The preparation method of the invention, wherein the concentration of the ceftazidime solution 1 is 200-500 mg/mL. Preferably, the concentration of the ceftazidime solution 1 is 250-450 mg/mL; more preferably, the concentration of the ceftazidime solution 1 is 300-400 mg/mL; and, most preferably, the concentration of the ceftazidime solution 1 is 300-350 mg/mL.
In a specific embodiment, the concentration of the ceftazidime solution 1 is 320 mg/mL.
The preparation method according to the present invention, wherein the HPLC purity of the crude ceftazidime in step (1) is not less than 97.0%, preferably not less than 97.5%, and more preferably not less than 98.0%.
In a specific embodiment, the HPLC purity of the crude ceftazidime of step (1) is 98.2%.
The preparation method according to the present invention, wherein the activated carbon of step (2) is added in an amount of 0.1-2.0wt% based on the total weight of the ceftazidime solution 1.
Preferably, the activated carbon of step (2) is added in an amount of 0.2 to 1.8wt%, based on the total weight of the ceftazidime solution 1; more preferably, the activated carbon of step (2) is added in an amount of 0.3 to 1.5wt%, based on the total weight of the ceftazidime solution 1; and, most preferably, said activated carbon of step (2) is added in an amount of 0.4-1.2wt%, based on the total weight of said ceftazidime solution 1.
In a specific embodiment, the activated carbon of step (2) is added in an amount of 0.5wt%, based on the total weight of the ceftazidime solution 1.
The preparation method provided by the invention is characterized in that the decoloring time of the step (2) is 15-60 min. Preferably, the decolorizing time of step (2) is 20-50 min; more preferably, the decolorization time of step (2) is 25 to 45 min; and, most preferably, said decolorizing time of step (2) is 25-40 min.
In a specific embodiment, said decolorizing time of step (2) is 30 min.
The preparation method of the invention, wherein the step (3) is carried out by using a Y-type micromixer.
The preparation method of the invention is characterized in that the specification of the Y-shaped micro mixer is L =50 mm; w =1 mm; h =0.5mm and the inlet angle is 60 °.
In one specific embodiment, the Y-type micromixer is from guizhou micromechelon co.
The preparation method according to the present invention, wherein the solvent of step (3) is the ceftazidime solution 2 of step (2).
The preparation method according to the present invention, wherein the anti-solvent of step (3) is 90v% acetone aqueous solution, and the pH of the acetone aqueous solution is 4.0 to 4.5.
In a specific embodiment, the anti-solvent of step (3) is a 90v% aqueous acetone solution, and the pH of the aqueous acetone solution is 4.2.
The preparation method of the invention comprises the step (3), wherein the flow rate of the solvent is 1-5mL/min, and the flow rate ratio of the solvent to the anti-solvent is 1 (10-30).
Preferably, the flow rate of the solvent is 1-4mL/min, and the flow rate ratio of the solvent to the anti-solvent is 1 (12-28); more preferably, the flow rate of the solvent is 1-3mL/min, and the flow rate ratio of the solvent to the anti-solvent is 1 (15-25); and, most preferably, the solvent flow is 1-2.5mL/min, and the ratio of solvent to anti-solvent flow is 1 (18-22).
In a specific embodiment, the solvent flow is 2mL/min and the ratio of solvent to anti-solvent flow is 1: 20.
The production method according to the present invention, wherein the step (3) is carried out at a temperature of 0 to 5 ℃.
In a particular embodiment, step (3) is carried out at a temperature of 2 ℃.
The preparation method comprises the following steps (4): the ceftazidime suspension was filtered and washed several times with ice water to give a wet ceftazidime product.
In a specific embodiment, the step (4) is: the ceftazidime suspension was filtered and washed twice with ice water to give a wet ceftazidime product.
The preparation method according to the present invention, wherein the base of step (5) is a sodium hydroxide solution.
In a specific embodiment, the base of step (5) is 2mol/L sodium hydroxide solution.
The preparation method according to the present invention, wherein the wet ceftazidime in step (5) is added in an amount of 0.01-0.1wt% based on the total weight of the ceftazidime solution 3. Preferably, the wet ceftazidime in step (5) is added in an amount of 0.02 to 0.09wt% based on the total weight of the ceftazidime solution 3; more preferably, the wet ceftazidime in step (5) is added in an amount of 0.03 to 0.08wt% based on the total weight of the ceftazidime solution 3; and, most preferably, said wet ceftazidime of step (5) is added in an amount of 0.04 to 0.06wt% based on the total weight of said ceftazidime solution 3.
In a specific embodiment, the wet ceftazidime in step (5) is added in an amount of 0.05wt% based on the total weight of the ceftazidime solution 3.
The preparation method provided by the invention is characterized in that the crystallization time of the step (5) is 0.5-24 h. Preferably, the crystallization time of step (5) is 1 to 12 h; more preferably, said crystallization time of step (5) is from 1.5 to 8 h; and, most preferably, said crystallization time of step (5) is 2-6 h.
In a specific embodiment, said crystallization time of step (5) is 3 h.
The inventor finds that when a Y-type micro mixer is used for solvent-antisolvent precipitation, the pH value and the temperature condition in the preparation method are controlled simultaneously, so that the obtained ceftazidime has uniform granularity and high purity, and is suitable for being used as a seed crystal of ceftazidime crystals for injection. Finally, the purity of the ceftazidime for injection is obviously improved, and the contents of related substances and ceftazidime polymers are reduced. Without wishing to be bound by any theory, the micromixing process used in the present invention and the specific control of pH and temperature conditions have a significant impact on the improvement of ceftazidime yield and purity of the present invention. The content of impurities generated after the ceftazidime for injection is influenced by environmental factors after being stored and placed for a long time is still within an allowable range.
Compared with the prior art, the invention has the following beneficial technical effects:
i) the ceftazidime for injection has higher yield and purity.
ii) the content of the related substances produced by ceftazidime for injection after long-term storage and placement under the action of environmental factors is still within the allowable range.
iii) the preparation method is simple and easy to implement, has good repeatability, and does not need other auxiliary materials; the equipment cost is low and no pollution is caused; can generate huge social benefit and economic benefit, and is suitable for being widely popularized and used.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications can be made by those skilled in the art after reading the contents of the present invention, and those equivalents also fall within the scope of the invention defined by the appended claims.
The following examples will aid understanding of the present invention, but are not intended to limit the scope of the present invention. In each example, the water used was purified water, and the purity of the starting material was not indicated as being chromatographically pure.
Example 1:
the HPLC purity of the crude ceftazidime was 98.2%. Adding the ceftazidime crude product into water for injection, adding 35wt% concentrated hydrochloric acid at 2 ℃ to adjust the pH value to 2.0, and stirring until the ceftazidime crude product is dissolved to obtain a ceftazidime solution 1; the concentration of the ceftazidime solution 1 is 320 mg/mL. Adding activated carbon into the ceftazidime solution 1, preserving heat and decoloring for 30min, and filtering to obtain a ceftazidime solution 2; the activated carbon was added in an amount of 0.5wt% based on the total weight of the ceftazidime solution 1. A small amount (about 5 mL) of ceftazidime solution 2 was used as solvent, while a 90v% aqueous acetone solution was used as anti-solvent, and the pH of the aqueous acetone solution was 4.2. Solvent-antisolvent precipitation was performed in a Y-type micromixer, model MCT micromixer, guizhou micromechem ltd. The specification of the Y-shaped micro mixer is L =50 mm; w =1 mm; h =0.5mm and the inlet angle is 60 °. The flow rate of the solvent is 2mL/min, and the flow rate ratio of the solvent to the anti-solvent is 1: 20; at a temperature of 2 ℃. The ceftazidime suspension was then filtered and washed twice with ice water to give a wet ceftazidime product. Adding 2mol/L sodium hydroxide solution into the ceftazidime solution 2 at the temperature of 2 ℃ to adjust the pH value to 3.6, so as to obtain a ceftazidime solution 3; to this was added a wet ceftazidime in an amount of 0.05wt% based on the total weight of the ceftazidime solution 3. Crystallizing for 3h, filtering, and washing with acetone twice to obtain ceftazidime for injection.
Example 2:
the HPLC purity of the crude ceftazidime was 98.0%. Adding the ceftazidime crude product into water for injection, adding 35wt% concentrated hydrochloric acid at 5 ℃ to adjust the pH value to 2.2, and stirring until the ceftazidime crude product is dissolved to obtain a ceftazidime solution 1; the concentration of the ceftazidime solution 1 is 300 mg/mL. Adding activated carbon into the ceftazidime solution 1, keeping the temperature and decoloring for 25min, and filtering to obtain a ceftazidime solution 2; the activated carbon was added in an amount of 0.4wt% based on the total weight of the ceftazidime solution 1. A small amount (about 5 mL) of ceftazidime solution 2 was used as solvent, while a 90v% aqueous acetone solution was used as anti-solvent, and the pH of the aqueous acetone solution was 4.5. Solvent-antisolvent precipitation was performed in a Y-type micromixer, model MCT micromixer, guizhou micromechem ltd. The specification of the Y-shaped micro mixer is L =50 mm; w =1 mm; h =0.5mm and the inlet angle is 60 °. The flow rate of the solvent is 1mL/min, and the flow rate ratio of the solvent to the anti-solvent is 1: 18; at a temperature of 5 ℃. The ceftazidime suspension was then filtered and washed twice with ice water to give a wet ceftazidime product. Adding 2mol/L sodium hydroxide solution into the ceftazidime solution 2 at 5 ℃ to adjust the pH value to 3.8, so as to obtain a ceftazidime solution 3; to this was added a wet ceftazidime in an amount of 0.06wt% based on the total weight of the ceftazidime solution 3. Crystallizing for 4h, filtering, and washing with acetone twice to obtain ceftazidime for injection.
Example 3:
the HPLC purity of the crude ceftazidime was 98.1%. Adding the ceftazidime crude product into water for injection, adding 35wt% concentrated hydrochloric acid at 1 ℃ to adjust the pH value to 1.8, and stirring until the ceftazidime crude product is dissolved to obtain a ceftazidime solution 1; the concentration of the ceftazidime solution 1 is 350 mg/mL. Adding activated carbon into the ceftazidime solution 1, preserving heat and decoloring for 40min, and filtering to obtain a ceftazidime solution 2; the activated carbon was added in an amount of 0.8wt% based on the total weight of the ceftazidime solution 1. A small amount (about 5 mL) of ceftazidime solution 2 was used as solvent, while a 90v% aqueous acetone solution was used as anti-solvent, and the pH of the aqueous acetone solution was 4.0. Solvent-antisolvent precipitation was performed in a Y-type micromixer, model MCT micromixer, guizhou micromechem ltd. The specification of the Y-shaped micro mixer is L =50 mm; w =1 mm; h =0.5mm and the inlet angle is 60 °. The flow rate of the solvent is 3mL/min, and the flow rate ratio of the solvent to the anti-solvent is 1: 22; at a temperature of 1 ℃. The ceftazidime suspension was then filtered and washed twice with ice water to give a wet ceftazidime product. Adding 2mol/L sodium hydroxide solution into the ceftazidime solution 2 at 1 ℃ to adjust the pH value to 3.5 to obtain a ceftazidime solution 3; to this was added a wet ceftazidime in an amount of 0.04wt% based on the total weight of the ceftazidime solution 3. Crystallizing for 2h, filtering, and washing with acetone twice to obtain ceftazidime for injection.
Comparative example 1:
the solvent-anti-solvent precipitation was performed in a 500mL beaker, and the conditions were the same as in example 1.
The ceftazidime for injection in the embodiments 1-3 and the comparative example 1 is taken and the content of the related substances is determined according to the test method of the second part of the Chinese pharmacopoeia 2015, page 240-241.
The results of the relevant tests are shown in tables 1 and 2 below:
TABLE 1 Performance index at day 0
| Yield/% | Maximum single impurity/%) | Total impurity content/%) | |
| Example 1 | 94 | 0.18 | 0.58 |
| Example 2 | 91 | 0.23 | 0.72 |
| Example 3 | 92 | 0.21 | 0.65 |
| Comparative example 1 | 86 | 0.47 | 1.43 |
TABLE 2 Performance index at day 10
| Maximum single impurity/%) | Total impurity content/%) | |
| Example 1 | 0.31 | 0.87 |
| Example 2 | 0.43 | 0.92 |
| Example 3 | 0.47 | 1.04 |
| Comparative example 1 | 0.84 | 2.11 |
As can be seen from tables 1 and 2, compared with comparative example 1, ceftazidime for injection in examples 1-3 of the present invention has higher yield and purity; it can be seen that the micromixing process used in the present invention and the control of the specific pH and temperature conditions have a significant impact on the improvement of the ceftazidime yield and purity of the present invention. And the content of the related substances generated after being subjected to the action of environmental factors after being stored and placed for a long time is still within the allowable range.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (10)
1. A process for the preparation of ceftazidime for injection, the process comprising:
(1) adding the ceftazidime crude product into water for injection, adding acid at 0-5 ℃ to adjust the pH value to 1.5-2.5, and stirring until the ceftazidime crude product is dissolved to obtain a ceftazidime solution 1;
(2) adding activated carbon into the ceftazidime solution 1, preserving heat, decoloring and filtering to obtain a ceftazidime solution 2;
(3) a part of the ceftazidime solution 2 is precipitated by a solvent-antisolvent to obtain a ceftazidime suspension;
(4) filtering the ceftazidime suspension to obtain a wet ceftazidime product; and the number of the first and second groups,
(5) adding alkali into the ceftazidime solution 2 to adjust the pH value to 3.5-4.0 at 0-5 ℃ to obtain a ceftazidime solution 3; adding a wet ceftazidime product into the mixture, crystallizing and filtering to obtain the ceftazidime for injection.
2. The preparation method according to claim 1, wherein the concentration of ceftazidime solution 1 is 200-500 mg/mL.
3. The preparation method according to claim 1, wherein the crude ceftazidime has an HPLC purity of not less than 97.0%.
4. The production method according to claim 1, wherein the step (3) is performed using a Y-type micromixer.
5. The preparation method according to claim 4, wherein the specification of the Y-type micromixer is L =50 mm; w =1 mm; h =0.5mm and the inlet angle is 60 °.
6. The preparation method according to claim 1, wherein the solvent of step (2) is ceftazidime solution 2 of step (2); the anti-solvent is 90v% aqueous acetone, and the pH of the aqueous acetone is 4.0-4.5.
7. The process according to claim 6, wherein in the step (3), the flow rate of the solvent is 1 to 5mL/min, and the flow rate ratio of the solvent to the antisolvent is 1 (10 to 30).
8. The production method according to claim 1, wherein the step (3) is carried out at a temperature of 0 to 5 ℃.
9. The preparation method according to claim 1, wherein the wet ceftazidime in step (5) is added in an amount of 0.01 to 0.1wt% based on the total weight of the ceftazidime solution 3.
10. The production method according to claim 1, wherein the crystallization time of step (5) is 0.5 to 24 hours.
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| 刘作华 等: "《流体混沌混合及搅拌过程强化方法》", 30 June 2016, 重庆大学出版社 * |
| 刘煜婷 等: ""头抱他咤五水化合物结晶工艺的改进"", 《黑龙江医药》 * |
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