Method for determining mesalazine related substances by high performance liquid chromatography

Abstract

The invention relates to a method for determining mesalazine related substances by high performance liquid chromatography. The chromatographic conditions are as follows: the high performance liquid chromatography is adopted; octadecyl silica gel bonded silica gel is used as a filler (Gemimi C185mu m 150mm*4.6 mm); the volume ratio of a phosphate buffer to a TABH solution to a methanol to a water in a mixed solution serving as a mobile phase A is 250: 50: 260: 440; the volume ratio of a phosphate buffer to a TABH solution to methanol to water in a mixed solution serving as a mobile phase B is 250: 50: 500: 200; and gradient elution is performed, the flow rate is 1.1 ml / min, the column temperature is 35 DEG C, and the detection wavelength is 230 nm. According to the determination method of the related substances, main peaks and various impurities can be effectively separated, and the blank gradient does not interfere with the determination of the impurity H and the impurity N. Methodological verification is carried out on the determination conditions of the related substances, and the separation degree and the detection sensitivity meet the requirements.

Description

technical field [0001] The invention relates to a high-efficiency liquid phase detection method for related substances, in particular to a detection method for mesalazine related substances, and belongs to the technical field of medicine. Background technique [0002] Mesalazine is a non-steroidal anti-inflammatory drug used for the treatment of ulcerative colitis and Crohn's disease (crohn's disease) in the acute attack stage. Considering the portability and ease of use of its enteric-coated tablets, Chinese pharmaceutical companies developed Mesalazine with reference to the mesalazine enteric-coated tablets imported from Dr. Qin enteric-coated tablets. As a synthetic drug, mesalazine is prone to produce a series of process impurities and degraded impurities during the synthesis process of its raw materials. In order to effectively detect each impurity, the detection of related substances is carried out. The impurities that must be inspected in my country are as follows: ...

AI Technical Summary

Problems solved by technology

[0004] The existing internal control standards for mesalazine raw materials have the following defects: (1) Elution ability: the impurity H cannot be effectively eluted; (2) Separation ability: the separation degree between mesalazine, impurity A, and impurity F Not up to the requirements; the separation between impurity D and impurity K is not up to the requirements; (3) peak shape: the peak shapes of impurities A, B, C, D, E, F, G are poor (symmetry factors are all lower than Small), the peak is prone to split

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