The Study OnIbuprofen Ethyl Ester In Ibuprofen And Its Analytical Method

The main analyte of this article, ibuprofen ethyl ester, is an unknown impurity of ibuprofen raw material medicine production found in the inspection process. In the detection of the related substances of ibuprofen API process, the impurities become the main source that the related substances of ibuprofen beyond the limit. National pharmacopoeia, related literature were not included the impurities, no more suitable analysis method for quantitative analysis of it, therefore, to make a thorough study of the impurity, has an important significance to improve the quality, guarantee the safety of using ibuprofen.This paper firstly used preparative chromatography to prepare impurity, then did the structure elucidation and confirmation on it, and then explore the method for analysis of impurities, through the screening of the detection wavelength, chromatographic column, mobile phase chromatographic conditions, find out the optimum chromatographic conditions, and did a comprehensive method validation. On the basis of the above work, further proved the formation principle and source of ibuprofen ethyl ester, and eliminate and reduce process of the impurities were explored, through optimizing the relevant key process parameters on ibuprofen refining process, the content of ibuprofen ethyl ester is simple and effective controlled,Firstly, by preparation chromatography, preparing ibuprofen ethyl ester, followed by means of IR, UV, MS, NMR and other methods for structure elucidation and confirmation of the impurity. The key chromatographic conditions then groped high performance liquid chromatographic method for determination, including the detection wavelength, chromatographic column, mobile phase gradient composition content, finally the optimal chromatographic conditions are determined. In order to verify the applicability of the method of analysis and validity, the specificity, accuracy, repeatability, intermediate precision, linearity, limit of detection and limit of quantification, the solution stability of the method validation and review. The optimal HPLC conditions:the detection wavelength was214nm; chromatographic column:YMC-pack ODS-A C18(4.6×150mm,5μ m); mobile phase:mobile phase A: acetonitrile-water=340:660(adjust pH=3with phosphoric acid), mobile phase B:acetonitrile, and determine the best mobile phase gradient composition. Validation results show that specificity, repeatability, intermediate precision, linearity, accuracy can meet the requirements, The analysis method is high sensitivity, simple, accurate,it is suitable for the detection of ibuprofen ethyl ester and other related substances. play an important role in the quality control of ibuprofen products.Then this paper studied the ibuprofen crude refining process, through the analysis of the crude product, finished product, analysis of the bleaching time, bleaching temperature, ethanol solvent concentration, ethanol recovery of ibuprofen ethyl ester content, determine the principle and source of ibuprofen ethyl ester production, find the factors affecting the content of ethyl ester of ibuprofen.Finally, according to the principle of the esterification reaction, the process parameters and reduce the content of ethyl ester of ibuprofen were screened, and finally the best process parameter determination, to effectively control the content of ethyl ibuprofen ibuprofen in objective.