High performance liquid chromatography (HPLC) detecting method of agomelatine and intermediates as well as impurities

Abstract

The invention relates to a liquid chromatography method for effectively separating and analyzing agomelatine and synthetic intermediates as well as impurities. The agomelatine is a melatonin excitant, has a depressive symptom resistance effect and can improve the night sleeping condition under the condition without influencing the daytime activity state. The invention aims at providing the efficient liquid chromatogram method for separating the agomelatine and the synthetic intermediates as well as the impurities. A octadecyl silane bonding silica gel filling chromatographic column is adopted so that a flowing phase A (organic phase) and a flowing phase B (water phase) prepared from buffer solution (with the pH being 6 to 7) and organic solvents according to different proportions are used as flowing phases, the flowing rte is 1.0ml/min, the gradient elution is carried out, and the separation and the analysis determination of the agomelatine and the synthetic intermediates as well as the impurities are realized.

Description

Technical field: [0001] The invention relates to a high-performance liquid chromatography method capable of effectively separating and analyzing agomelatine, synthetic intermediates and various impurities. technical background: [0002] Agomelatine (Agomelatine), chemical name N-[2-(7-methoxynaphthyl-1-yl) ethyl] acetamide, is a melatonin agonist, has the effect of antidepressant symptoms, can Improve nighttime sleep without compromising daytime activity. [0003] The synthesis steps of this product are mentioned in the patent EP0447285, which uses 7-methoxy-1-tetralone as the starting material to react to obtain agomelatine. It is also a common agomelatine preparation process. Tin preparation process. [0004] In the chemical synthesis process of agomelatine, there are several key steps, so the corresponding intermediates may remain in the final product, and many ammonium salts are likely to be produced during the synthesis process, especially in the catalytic hydrogenati...

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Problems solved by technology

[0024] Undoubtedly, the above-mentioned compounds can be separated and detected separately when using different chromatographic conditions, but there is a great waste of manpower and material resources in the selection of multiple chromatographic conditions for separate detection. Through investigation, we have found a suitable chromatographic condition, which can be Effective separation and analysis of the above compounds

[0025] Considering the structures of the above compounds, some of the structures are very similar. From the perspective of polarity, some impurities have great polarity differences with agomelatine. To achieve complete and effective separation of each component on the same chromatographic column is very difficult

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