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Preparation of impurity in cefetecol disodium and structure confirmation method

A technology of cefotetan disodium and cefotetan, which is applied in the field of preparation and structure confirmation of impurities in cefotetan disodium, and can solve the problems of limitation, influence on safety, and many clinical side effects.

Active Publication Date: 2015-09-16
CHENGDU UNIV
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Problems solved by technology

[0007] Cefotetan disodium is a raw material for injection, and the impurities contained in it will affect the safety of the product, especially the clinical side effects of cephalosporins are more, so the impurities in the sample should be thoroughly studied and strictly limited.
Existing methods and literature have assigned some of the impurities, but there is still a relatively large impurity that is an unknown impurity

Method used

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  • Preparation of impurity in cefetecol disodium and structure confirmation method
  • Preparation of impurity in cefetecol disodium and structure confirmation method
  • Preparation of impurity in cefetecol disodium and structure confirmation method

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Embodiment 1

[0029] 1. Preparation of impurities

[0030] The chromatographic conditions are as follows: Agilent 1200 high performance liquid chromatography, Unitary C 18 100A (10mm×250mm, 10μm) semi-preparative column, with 0.1% trifluoroacetic acid aqueous solution-methanol-acetonitrile (80:10:10) as the mobile phase, take an appropriate amount of sample, dissolve it in water, and prepare 1.0g / ml impurity preparation For the test solution, the injection volume is 100 μl, the flow rate is 3.0ml / min, the detection wavelength is 254nm, and the column temperature is 30°C. Under the chromatographic conditions, the impurities peaked in about 7 minutes, and the cefotetan disodium peaked in about 20 minutes. After the impurities were detected by the ultraviolet detector, the fractions were collected after the column was started at the peak position, and the samples were enriched.

[0031] The collected fractions were concentrated under reduced pressure (15° C.) by a rotary evaporator for about ...

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Abstract

The invention discloses preparation of an impurity in cefetecol disodium and a structure confirmation method, and belongs to the pharmaceutical analysis technology field. Literature reports that a HPLC-MS method to carry out structure derivation of an impurity in a sample, but aimed to the impurity with a small content, satisfied results are difficult to obtain through the HPLC-MS method, and literature and patent reports related to the impurity are not discovered. Aimed to the above problem, separation is carried out by utilization of a preparation column, enrichment of the target impurity is carried out, further separation and purification are carried out, and finally the impurity monomer is obtained. Confirmation is carried out and the chemical structure of the impurity is obtained. The method is simple, the result is accurate, and the method can be used for impurity analysis control of cephalosporin samples.

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 impurities in cefotetan disodium. Background technique [0002] Cefotetan disodium chemical name: (6R,7S)-7-[4-(2-amino-1-carboxy-2-oxoethylene)-1,3-dithietane-2- Formylamino]-7-methoxy-3-[1-methyl-1H-tetrazolium-5-thiomethyl]-8-oxo-5-thia-1-azabicyclo[4.2 .0] Oct-2-ene-2-carboxylic acid disodium salt. [0003] Chemical Structure: [0004] [0005] Cefotetan Disodium (Cefotetan Disodium) is the second-generation cephalosporin antibiotics for injection, which has the characteristics of a broad antibacterial spectrum of the third-generation cephalosporins. It was first launched in Japan in 1993. The product with the same name was approved by the FDA in 2003 to be listed in the United States, and my country has not yet imported this product. According to the provisions of my country's drug registration management met...

Claims

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Application Information

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IPC IPC(8): C07D501/57C07D501/12
CPCC07D501/12C07D501/57
Inventor 王宇驰唐克慧孙样曹胜华张春然张静霞李强赵经纬徐明琴李喆宇杨晨李成龙邓思思
Owner CHENGDU UNIV
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