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Paeoniflorin crystallization process with controllable crystal form and granularity

A technology of azithromycin and particle size, applied in the field of crystallization process of azithromycin, can solve the problems of inability to meet the requirements of azithromycin polymorphism, large fluctuation of particle size distribution, optimization research of preparation method, etc., and achieve stable preparation of crystal form and good gloss. , the effect of crystal appearance rules

Inactive Publication Date: 2009-04-29
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the common preparation methods of azithromycin are mainly pure water extraction or cooling methods, which lack the control of the preparation process and the optimization of the preparation method, which leads to low stability of the crystal form, low purity, large particle size distribution fluctuations, and hygroscopicity. Strong, unable to meet the requirements of the pharmaceutical industry for polymorphic forms of azithromycin

Method used

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  • Paeoniflorin crystallization process with controllable crystal form and granularity
  • Paeoniflorin crystallization process with controllable crystal form and granularity
  • Paeoniflorin crystallization process with controllable crystal form and granularity

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Dissolve 20g of amorphous azithromycin raw material in 170mL of absolute ethanol, adjust the pH to 10.0, dilute to 200mL and place it in a 1000mL three-necked flask, keep a constant temperature water bath at 40℃, and control the stirring speed to 500r·min -1 , Add 2% sodium chloride of azithromycin quality. Then start to add pure water slowly, and the flow rate is controlled. The hourly dosage is the initial volume of the 20% azithromycin organic solution, which is slightly turbid. After stopping the flow and adding the crystal for 2 hours, continue to maintain the same flow acceleration and continue to flow until the flow is completed. Pure water, suction filtration, vacuum, desiccant anhydrous calcium chloride, drying at 40°C for 4 hours. The finally obtained azithromycin crystal form has good stability (see Table 3 for unit cell parameters), regular appearance, crystal form purity of 99%, main particle size of 40.3 μm, distribution width of 21.5 μm, and water content of ...

Embodiment 2

[0037] Dissolve 24g of amorphous azithromycin raw material into 170mL of ethylene glycol, adjust the pH to 11.0, set the volume to 200mL and put it into a 1000mL three-necked flask, keep a constant temperature water bath at 20℃, and control the stirring speed at 300r·min -1 , Add 2% sodium acetate of the quality of azithromycin. Then start to add pure water slowly, and the flow rate is controlled. The hourly flow rate is the initial volume of 15% azithromycin organic solution, which is slightly turbid. After stopping the flow and adding the crystal for 2 hours, continue to maintain the same flow acceleration and continue to flow until the flow is completed. Pure water, suction filtration, vacuum, drying in the presence of desiccant silica gel, at 40°C for 5 hours. The final crystal form of azithromycin (see Table 3 for unit cell parameters) has regular appearance, purity of crystal form is 99%, main particle size is 72 μm, distribution width is 44.2 μm, and water content is 3.2%. ...

Embodiment 3

[0039] Dissolve 30g of amorphous azithromycin raw material into 170mL tetrahydrofuran, adjust the pH to 8.0, dilute the volume to 200mL and put it into a 1000mL three-necked flask, keep a constant temperature water bath at 30℃, and control the stirring speed at 500r·min -1 , Add 2% sodium chloride of azithromycin quality. Then start to add pure water slowly, and the flow rate is controlled. The hourly flow rate is the initial volume of 15% azithromycin organic solution, which is slightly turbid. After stopping the flow and adding the crystal for 2 hours, continue to maintain the same flow acceleration and continue to flow until the flow is completed. Pure water, suction filtration, vacuum, desiccant anhydrous magnesium nitrate, drying at 40°C for 8 hours. The final crystal form of azithromycin (see Table 3 for unit cell parameters) has regular appearance, purity of crystal form is 99%, main particle size is 32.4 μm, distribution width is 20.2 μm, and water content is 1.7%.

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Abstract

The invention discloses an azithromycin crystallization process with controllable crystal form and grain size. In azithromycin organic solution with the pH value of between 7.0 and 11.0 and the initial concentration of between 80 and 200g.L<-1>, inorganic sodium salt and a solventing-out agent are added, the crystallization temperature is controlled to between 10 and 90 DEG C, the stirring speed is controlled to between 10 and 1,000r.min<-1>, the crystallization is performed by the synergy of elution and salting out, suction filtration is performed after complete crystallization, washing is repeatedly performed by the solventing-out agent, and then vacuum drying is performed. In the process, the aims of stable preparation of crystal form and controllable grain size of the azithromycin are achieved by regulating and controlling preparation conditions. The azithromycin prepared by the crystallization process has the advantages of good stability of crystal form, high purity (more than 99 percent), uniform grain size, good luster, weak hydroscopic property and the like.

Description

Technical field [0001] The invention belongs to the technical field of crystallization, and specifically relates to a crystallization process of azithromycin. Background technique [0002] As the second-generation erythromycin product, azithromycin is the first semi-synthetic aza-fifteen-membered ring macrolide antibiotic. Compared with erythromycin, azithromycin retains the advantages of erythromycin and has a further antibacterial spectrum. Expansion, outstanding antibacterial effect on Chlamydia trachomatis and high tissue concentration. Azithromycin has always been a hot product in the international anti-infective drug market due to its advantages such as long half-life, fewer doses, shorter course of treatment, and low incidence of adverse reactions. The US FDA Anti-Infection Advisory Committee recommends it as a drug for respiratory, genitourinary, skin and soft tissue infections caused by sensitive bacteria. Today, the incidence of sexually transmitted diseases is getting ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08
Inventor 应汉杰黄小权张磊熊健柏建新李振江
Owner NANJING TECH UNIV
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