克拉霉素缓释片中骨架辅料羟丙甲纤维素含量的HPLC-RID测定

Assay of hydroxypropyl methyl cellulose as the skeleton excipient in clarithromycin sustained-release tablets by HPLC-RID method

目的:建立HPLC-RID法测定和比较不同企业生产的克拉霉素缓释片中骨架辅料羟丙甲纤维素(HPMC)的含量,同时评价该辅料与释放度之间可能存在的相关性。方法:采用TSK-Gel 3000色谱柱(300 mm×7.5 mm,10μm),以50 mmol·L^(-1)氯化钠溶液为流动相进行洗脱,流速0.7 m L·min^(-1),柱温30℃,检测温度30℃,进样量5μL。结果:本法可以有效测定HPMC且与其它峰能良好分离,溶液在24 h内稳定;样品中的HPMC含量为标示量的85%~107%。结论:本方法可以有效地测定克拉霉素缓释片中HPMC含量,同时该辅料含量与该药品的体外释放存在一定的相关性。

Objective： To establish an HPLC-RID method for the assay and comparison of hydroxypropyl methyl cellulose （ HPMC ） as skeleton excipient in clarithromycin sustained-release tablets from different manufacturers, and to evaluate the correlation between the excipient contents and the sustained-release features. Methods： The separation was performed on a TSK-Gel 3000 column （ 300 mm× 7.5 mm, 10 μm ）, with a mobile phase of 50 mmol · L^-1 sodium chloride at a flow rate of 0.7 mL· min^-1. Both the column and the detector temperature were set at 30 ℃, and a 5 μL aliquot was injected into HPLC for the assay. Results： HPMC was well separated from other components and the assay was accurate. The test solution was stable in 24 hours. The contents of HPMC in the tested samples were found to be in the range from 85% to 107% of labeled amount. Conclusion： The method was validated to be suitable for the assay of HPMC in clarithromycin sustained-release tablets. There was obvious correlation between the contents of HPMC in the clarithromycin sustained-release tablets and the in vitro drug release characteristics.