Preparation method of ceftriaxone sodium crystal and evaluation method of ceftriaxone sodium aqueous solution turbidity

A technology of ceftriaxone sodium and aqueous solution, which is applied in the field of preparation and evaluation of ceftriaxone sodium, can solve the problems of uncertain crystal form, uncontrollable quality and stability, and achieves mild conditions, good clarity, and occurrence of allergic reactions. low rate effect

Active Publication Date: 2013-03-27
YOUCARE PHARMA GROUP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to overcome the defect that the crystal form is uncertain in the preparation process of the existing ceftriaxone sodium crystal, resulting in uncontrollable quality and stability, an object of the present invention is to provide a method for preparing ceftriaxone sodium crystal, which can obtain the definite crystal type of crystal

Method used

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  • Preparation method of ceftriaxone sodium crystal and evaluation method of ceftriaxone sodium aqueous solution turbidity
  • Preparation method of ceftriaxone sodium crystal and evaluation method of ceftriaxone sodium aqueous solution turbidity
  • Preparation method of ceftriaxone sodium crystal and evaluation method of ceftriaxone sodium aqueous solution turbidity

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Experimental program
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Embodiment 1

[0038] Get the raw material of ceftriaxone sodium (the condensation product sodium salt of 7-ACT and AE-active ester, without further purification) and prepare an aqueous solution, wherein the raw material of ceftriaxone sodium is 5 g and 40 ml of deionized water. Control the temperature of the aqueous solution at about 13°C, then add 4.1 g of sodium isooctanoate to the aqueous solution, stir the solution until it becomes clear, add 10 wt% dilute hydrochloric acid to adjust the pH value of the solution to 7.00, and continue stirring for 30 minutes to obtain the crude product of ceftriaxone sodium aqueous solution.

[0039] Get the above-mentioned crude product aqueous solution of ceftriaxone sodium, slowly add dehydrated ethanol therein under stirring, stop stirring just when turbidity occurs, and let stand for 25 minutes; then slowly add remaining dehydrated alcohol until a large amount of crystals are formed, The total amount is about 150ml.

[0040] The resulting crystals ...

Embodiment 2

[0042] The raw material of ceftriaxone sodium (the condensation product sodium salt of 7-ACT and AE-active ester, without further purification) was prepared into an aqueous solution, wherein the raw material of ceftriaxone sodium was 5 g and 15 ml of deionized water. Control the temperature of the aqueous solution at about 15°C, then add 10.0 g of sodium isooctanoate to the aqueous solution, stir the solution until it becomes clear, add 10 wt% dilute hydrochloric acid to adjust the pH value of the solution to 8.04, and continue stirring for 25 minutes to obtain the crude product of ceftriaxone sodium aqueous solution.

[0043]Get the above-mentioned ceftriaxone sodium crude product aqueous solution, slowly add acetone therein under stirring, stop stirring just when turbidity appears, and let it stand for 30 minutes; then slowly add remaining acetone until a large amount of crystals are formed, the total amount of acetone is about 180ml.

[0044] The resulting crystals are filt...

Embodiment 3

[0046] Using powder X-ray diffraction technology combined with cluster analysis method, more than 160 batches of ceftriaxone sodium samples for injection in the market were classified.

[0047] Powder X-ray diffraction experiment conditions are as follows:

[0048] Instrument: Rigaku Corporation D / max-2200 powder X-ray diffractometer.

[0049] Parameter setting: X-ray: CuK α1 Target; voltage 40KV; current 40mA. Slit width: 1deg, 1deg, 0.15mm. Scanning speed: 4deg / min. Scanning range (2θ): 2~50deg.

[0050] Analysis software: RINT 2000Series software. Integration conditions: peak width 0.05; minimum peak height 100.

[0051] Sample preparation: Take a sample of ceftriaxone sodium for injection, and press it into tablets by positive pressure on a glass plate.

[0052] The spectrograms of more than 160 batches of experimental samples obtained from powder X-ray diffraction experiments were analyzed with random RISM.Qualitative Analysis software, and the average diffraction ...

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Abstract

The invention relates to a preparation method of ceftriaxone sodium crystal, wherein the obtained ceftriaxone sodium is the crystal of the same subtype, and the subtype crystal has the best clarity, the lowest anaphylaxis occurrence rate and the highest safety in comparison with all crystals. The preparation method is simple in technology and excellent in reproducibility. The invention further relates to an evaluation method of ceftriaxone sodium aqueous solution turbidity, wherein a powder X-ray diffraction technology and a scanning electron microscope technology are used, in combination with statistical methods, a method for evaluating the ceftriaxone sodium crystal form is established, three subtypes of the ceftriaxone sodium crystal form is defined for the first time, and the relation between the subtypes and the aqueous solution turbidity is established, thus, rapid evaluation on crystal form and aqueous solution turbidity of ceftriaxone sodium samples becomes possible, and the method has great practical value.

Description

technical field [0001] The invention relates to the field of preparation and evaluation of ceftriaxone sodium, in particular to a method for preparing ceftriaxone sodium crystals and a method for evaluating the turbidity of its aqueous solution. Background technique [0002] Ceftriaxone sodium, also known as ceftriaxone. It is a semi-synthetic third-generation cephalosporin launched by the Swiss company Roche in the 1980s. It has strong antibacterial activity against most Gram-positive and negative bacteria. The antibacterial spectrum includes Pseudomonas aeruginosa, E. , Haemophilus influenzae, enterobacteria aerogenes, Proteus, diplococcus and Staphylococcus aureus, etc., stable to β-lactamase. Ceftriaxone sodium is a national essential drug. It is mainly used clinically for meningitis, pneumonia, skin and soft tissue infection, peritonitis, urinary system infection, gonorrhea, liver and gallbladder infection, surgical trauma, sepsis and reproductive system infection caus...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36G01N23/20
Inventor 胡昌勤薛晶贾燕花杨磊马志华
Owner YOUCARE PHARMA GROUP
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