Separation preparation method of mezlocillin sodium impurity A

A technology of refining method of mezlocillin sodium, which is applied in the separation and preparation of impurity A of mezlocillin sodium and the refining of impurities of antibiotic drug compounds, which can solve the difficulties in the synthesis of impurity A, low product purity, instability and easy degradation, etc. problems, to achieve the effect of shortening the separation time, simple process and stable product quality

Inactive Publication Date: 2018-12-25
REYOUNG PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no research institution in China that can provide efficient standards and preparation methods of mezlocillin sodium impurity A, but there are problems such as high cost, cumbersome procedures, and long delivery cycle when importing foreign commercially available products.
Moreover, the synthesis of impurity A is difficult, unstable and easy to degrade after synthesis, and a large number of by-products are easily produced during the synthesis process, and the yield is low, resulting in low purity of commercially available products.

Method used

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  • Separation preparation method of mezlocillin sodium impurity A
  • Separation preparation method of mezlocillin sodium impurity A
  • Separation preparation method of mezlocillin sodium impurity A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] At room temperature, add 60 mL of 0.1 mol / mL potassium hydroxide solution to 2.0 g of mezlocillin sodium, stir for 30 minutes, then add 0.5 mol / mL hydrochloric acid solution dropwise to adjust the pH value of the solution to 3, add 20 g of calcium chloride solid was stirred for 5 minutes, filtered, rinsed once with 5 mL of water, then rinsed once with 5 mL of ethanol, and dried at room temperature to obtain 1.1 g of solid. According to the 2015 edition of the Chinese Pharmacopoeia, octadecylsilane bonded silica gel is used as a filler; the mobile phase is a buffer solution (take 4.9 g of potassium dihydrogen phosphate and 0.45 g of dipotassium hydrogen phosphate, dissolve and dilute to 1000 mL with water): acetonitrile, Isocratic elution at a volume ratio of 80:20, flow rate 1.0mL / min; column temperature 30°C, detection wavelength 210nm; retention time 11.1min. The calculated yield was 70%.

Embodiment 2

[0051] At room temperature, add 60 mL of 0.1 mol / mL sodium hydroxide solution to 2.0 g of mezlocillin sodium, stir for 30 min, add phosphoric acid solution drop by drop, adjust the pH value of the solution to 4, add 20 g of calcium chloride solid After stirring for 5 min, filter, rinse once with 5 mL of water, then rinse once with 5 mL of ethanol, and dry at room temperature to obtain 1.1 g of solid. The calculated yield was 67%.

Embodiment 3

[0053] At room temperature, add 60 mL of ammonia water to 2.0 g of mezlocillin sodium, stir for 30 min, then add acetic acid solution drop by drop, adjust the pH value of the solution to 5, then add 15 g of potassium chloride solid and stir for 10 min, filter, and use Rinse twice with 5 mL of acetone and dry at room temperature to obtain 1.2 g of solid with a yield of 52%.

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Abstract

The invention belongs to the technical field of medicine and relates to a refining method of antibiotic drug compound impurities, in particular to a separation preparation method of mezlocillin sodiumimpurity A, comprising the steps of subjecting mezlocillin sodium as a raw material to reaction with an alkaline reagent to obtain mezlocillin sodium impurity A. The mezlocillin sodium impurity A ismade with mezlocillin sodium, an alkaline solution, an acid solution and an inorganic salt at room temperature by filtering, washing and drying. The invention also provides a refining method for separating and purifying mezlocillin sodium impurity A; the mezlocillin sodium impurity A prepared herein has purity of greater than 95% and is applicable to control researches; the invention belongs to the field of medicine.

Description

technical field [0001] The invention relates to a method for refining antibiotic drug compound impurities, in particular to a method for separating and preparing mezlocillin sodium impurity A, and belongs to the technical field of medicine. Background technique [0002] The chemical name of mezlocillin sodium is: (2R,5R,6R)-3,3-Dimethyl-6-[(R)-2[3-(methylsulfonyl)-2-oxo-1-imidazole Alkylcarboxamido]-2-phenylacetamido]-7-oxo-4-thia-1-azabicyclo[3.2.0]-heptane-2-carboxylic acid sodium salt, which has the following structure: [0003] [0004] Mezlocillin sodium is a semi-synthetic penicillin antibiotic, white or off-white powder or crystal; odorless or slightly specific odor, bitter taste. Clinically, Pseudomonas aeruginosa, Escherichia coli, Klebsiella pneumoniae, Proteus, Enterobacter, Citrobacter, Serratia, Acinetobacter and penicillin-sensitive Gram-positive cocci are all Has an inhibitory effect. [0005] Mezlocillin sodium belongs to the β-lactam penicillin antibio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D417/12
CPCC07D417/12
Inventor 苗得足胡清文赵征王志尹诗曾丽丽
Owner REYOUNG PHARMA
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