Liquid phase detection method of cefdinir reaction terminal point

Abstract

A liquid phase detection method of cefdinir reaction terminal point comprises the following steps: 1) dilution of a reaction liquid, filtering; 2) configuration of a mobile phase, to be more specific, mobile phase A is an aqueous solution with 26mL of 10% tetrabutyl ammonium hydroxide contained in 1000mL of aqueous phase, the pH is adjusted to 5 by phosphoric acid, and mobile phase B is acetonitrile; 3) the volume ratio of the mobile phase A:B of 525-600:475-400, the flow rate of 1mL / min, C18 filler, column temperature of 25 DEG C, the detection wavelength of 210-300nm, and the injection volume of 10 muL; and 4) taking the peak area less than 0.5% of 7-AVCA (7-amino-3-vinyl-3-cephem-4-carboxylic acid) in liquid chromatography as the reaction terminal point. The beneficial effects of the liquid phase detection method are that: without changing other chromatographic conditions, the proportion of each component of the mixed mobile phase is adjusted, the separation degree of the 7-AVCA and adjacent coexistence matters is greater than 1.5 to achieve complete baseline separation, the reaction terminal point can be accurately judged, the method is simple, and the operability is strong.

Description

technical field [0001] The invention relates to an analysis and detection method, in particular to a liquid phase detection method for the reaction end point of cefdinir. Background technique [0002] The synthetic steps of cefdinir include: condensation, deprotection and refining three steps. In one step of the condensation reaction, cefdinir is produced from the intermediate 7-AVCA and the active ester. The reaction solution was detected by HPLC, and when 7-AVCA<0.5%, it was judged as the end point of the reaction. When the sources of active esters are from different manufacturers, the impurities brought into the reaction solution are also different. When 7-AVCA forms triplet peaks with two adjacent impurities, the content of 7-AVCA cannot be accurately integrated, that is, 7-AVCA is always greater than 0.5%. It is impossible to accurately judge whether the reaction reaches the end point, which directly affects the purity and quality of the product. Convenient and qu...

AI Technical Summary

Problems solved by technology

When the sources of active esters are from different manufacturers, the impurities brought into the reaction solution are also different. When 7-AVCA forms triplet peaks with two adjacent impurities, the content of 7-AVCA cannot be accurately integrated, that is, 7-AVCA is always greater than 0.5%. It is impossible to accurately judge whether the reaction has reached the end point, which directly affects the purity and quality of the product