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Preparation and structure confirmation method of lactone impurities in flomoxef sodium

A technology of fluoxefom sodium and impurities, which is applied in the field of preparation and structure confirmation of lactone impurities in fluoxefom sodium

Pending Publication Date: 2019-06-14
SHANDONG RUIYING PIONEER PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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There is no relevant report on the preparation and confirmation method of the impurity of the present invention

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  • Preparation and structure confirmation method of lactone impurities in flomoxef sodium
  • Preparation and structure confirmation method of lactone impurities in flomoxef sodium
  • Preparation and structure confirmation method of lactone impurities in flomoxef sodium

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Embodiment 1

[0028] 1. Preparation of impurities

[0029] The chromatographic conditions are as follows: Agilent 1200 high-performance liquid chromatography, octadecylsilane bonded silica gel as a semi-preparative column (10mm × 250mm, 10 μm) as a filler, 5mmol / L ammonium acetate solution-methanol (the volume ratio of the two 700-900:300-100) as the mobile phase, take an appropriate amount of sample, dissolve it in water, and prepare the test solution for 10-200mg / ml impurities, the injection volume is 100μl, the flow rate is 1-3ml / min, and the detection wavelength is 246nm. The column temperature is 30°C. Under the chromatographic conditions, the fluoxetal sodium peaks out in about 10 minutes, and the impurities peak out in about 17 minutes. After the impurities are detected by the ultraviolet detector, the fractions are collected after the column is started at the peak position, and the samples are enriched.

[0030] Take the collected fractions and concentrate them under reduced pressu...

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Abstract

The invention discloses a preparation and structure confirmation method of impurities in flomoxef sodium, which is characterized by comprising the following steps: (1) preparing a flomoxef sodium sample, increasing impurities under an acidic condition, and regulating the pH value to be neutral by using a dilute alkali solution; (2) applying the solution obtained in the step (1) to a high performance liquid chromatograph, collecting fractions and enriching a sample; (3) conducting reduce-pressure concentration on the collected fractions by using a rotary evaporator; (4) performing repeated enrichment to obtain a concentrated solution, removing an organic solvent from the concentrated solution by using a rotary evaporator, and performing freeze-drying treatment on the residual solution to obtain an impurity monomer; and (5) analyzing and confirming the impurity structure of a single impurity through a mass spectrum and a nuclear magnetic resonance spectrum. The method is used for detecting related substances of flomoxef sodium and preparations of flomoxef sodium, a theoretical basis is provided for safe use of the medicine, effective data support can be provided for improving the quality standard of flomoxef sodium, and an effective guarantee is provided for clinical safe use of flomoxef sodium.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for preparing and confirming the structure of lactone impurities in fluoxyceph sodium. Background technique [0002] The chemical name of fluoxetal sodium is: (6R,7R)-7-[2-(difluoromethylthio)acetamido]-7-methoxy-3-{[1-(2-hydroxyethyl) Sodium -1H-tetrazol-5-yl]thiomethyl}-8-oxo-5-oxa-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate. [0003] The chemical structural formula is: [0004] . [0005] Flomoxef Sodium (Flomoxef Sodium) was successfully developed by Shionogi Pharmaceutical Co., Ltd. in Japan, and was first listed in Japan under the trade name Flumarin in 1988 as an injection of Oxycephalosporin antibiotics. Fluoxefor sodium is a broad-spectrum oxycephem (oxacephalosporin) antibacterial drug, which is very stable to β-lactamase. The antibacterial performance is similar to that of the fourth generation cephalosporins. [0006] At present, it has been repor...

Claims

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Application Information

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IPC IPC(8): C07D505/02C07D505/20G01N24/08G01N30/06
CPCY02A90/30
Inventor 彭继先宁小荣袁继鲁付洪荣
Owner SHANDONG RUIYING PIONEER PHARMA
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