关于布洛芬片有关物质方法学的研究

Studies on Material Methodology:Ibuprofen Tablets

目的:为了更好地控制布洛芬片生产的稳定性,确定布洛芬片在长期放置过程中是否有新的杂质产生。通过相应的方法学研究,建立了布洛芬片有关物质的测定方法。验证方法:采用YMC色谱柱(4.6 mm×150 mm, 5μm);以0.07%磷酸溶液-乙腈(体积比55∶45)(可根据保留时间适当调节比例)为流动相。柱温30℃;检验波长为214 nm,流速1.0 mL/min。验证结果:定量限及检测限RSD≤5.0%;专属性:辅料不干扰;杂峰与主峰分离良好;重复性及中间精密度RSD均小于1.0%。准确度:向供试品溶液中加入不同浓度的布洛芬,回收率均大于90%。稳定性:对照溶液和供试品溶液在自然条件下,放置8 h,供试溶液无新物质生成,总杂无变化或变化微小,溶液稳定性良好。耐用性:色谱条件在一定的范围内变动时,与标准条件下比较,变化在规定误差范围内,符合系统适用性试验要求。线性和范围:在规定的范围内布洛芬的线性结果与被测样品中的浓度呈线性关系,而且线性的范围能达到精密度和准确度的要求。

Objective:Ibuprofen tablets have been shown to be effective in the treatment of colds,fevers,and joint pain,while ibuprofen tablets have been shown to be effective in the treatment of joint pain.Especially in the new coronavirus infection,can play a very good role in antipyretic.In order to better control the stability of ibuprofen tablets production,to determine whether ibuprofen tablets in the long-term storage process of new impurities produced,a method for the determination of related substances in ibuprofen tablets was established.Methods:YMC column(4.6 mm×150 mm,5μm)was used,0.07%phosphoric acid solution-acetonitrile(55∶45)(the ratio can be adjusted according to the retention time)was used as mobile phase.The column temperature was 30℃,the detection wavelength was 214 nm and the flow rate was 1.0 mL/min.The results showed that the RSD of quantitative limit and detection limit was less than 5.0%;specificity:Excipients did not interfere;the separation between main peak and miscellaneous peak was good.The repeatability and intermediate precision RSD were both less than 1.0%;Accuracy:Different concentrations of ibuprofen are added to the test solution,the recovery rate is more than 90%.Stability:The control solution and test solution under natural conditions,placed for 8 h,test solution no new substances generated,the stability of the solution is good.Durability:When the chromatogram condition changes in a certain range,compared with the standard condition,the change is within the specified error range,in line with the system applicability test requirements.Linear and range:The linear result of ibuprofen is linear with the concentration of the sample in the specified range,and the linear range can meet the requirements of precision and accuracy.