摘要
目的建立快速、准确的同时测定复方盐酸克林霉素软膏中克林霉素和维A酸含量的HPLC方法,并考察软膏的稳定性。方法采用Waters Nova-PakC18(3.9mm×250mm,4.6μm)柱,流动相为甲醇-磷酸盐缓冲液(0.015mol/LKH2PO4,用1mol/L氢氧化钠调节pH至7.0)(80:20),流速为1.0ml/min,检测波长214nm,进样量20μl;维A酸的主要降解产物异维A酸测定波长为340nm,其它测定条件与维A酸含量测定相同,按维A酸与异维A酸两者面积归一化结果计算异维A酸的量;软膏的稳定性考察采用中国药典2005年版附录中推荐的条件。结果克林霉素和维A酸的色谱峰均能与其它杂质峰较好的分离。克林霉素在0.2119～3.4704mg/ml的浓度范围,维A酸在0.007181～0.2298mg/ml的浓度范围内均呈线性。克林霉素的平均回收率为100.0%,RSD为0.4%(n=9);维A酸的平均回收率为99.9%,RSD为0.4%(n=9)。维A酸与异维A酸的检测限均为0.002μg/ml,定量限均为0.005μg/ml。异维A酸相对维A酸的校正因子为0.9。加速稳定性试验6个月和长期稳定性12个月考察结果表明,软膏中克林霉素稳定,维A酸对热不稳定,且易氧化。结论建立的测定方法简单、快捷,适用于同时测定软膏中的克林霉素和维A酸含量;复方盐酸克林霉素软膏应于凉暗处密闭保存,软膏灌装时应充分充氮除氧。
Objective To establish an HPLC method for determination of clindamycin and tretinon in compound clindamycin hydrochloride ointment simultaneously and to evaluate the ointment＇s stability. Methods A C18 column was used and the mobile phase consisted of 0. 015mol/L potassium dihydrogen phosphate （adjusted with 1mol/L sodium hydroxide to pH7.0） - methanol （80： 20）, the detection wavelength was 214nm, the flow rate was 1.0ml/min and the injection volume was 20μl. The chromatographic conditions of isotretinon were the same as above except that the detection wavelength was 340nm. The amount of isotretinon in the ointment could be calculated by the normalization of chromatographic peak area of tretinon and isotretinon. The stability testing condition of compound clindamycin hydrochloride ointment was confirmed accordding to the guidence of stabihy testing in appendix of CP2005. Results Good separation was achieved between clindamycin, tretinon and the relative impurities. The linearity of clindamycin was obtained in the range of 0. 2119 - 3.4704mg/ml, its average recovery was 100. 0%, RSD for 0.4% （ n = 9）; the linearity of tretinon was obtained in the range of 0. 007181 - 0. 2298mg/ml, its average recovery was 99.9%, RSD for 0. 9% （ n = 9）. LOD of tretinon and isotretinon were both 0. 002μg/ml, and LOQ were both 0. 005μg/ml. The corrected factor was 0. 9. The results of the accelerated stability testing for 6 months duration and the long term stability testing for 12 months duration indicated that clindamycin was stable but tretinon was unstable for heat and prone to oxidize. Conclusion The method established was simple and accurate for simultaneous determination of these two constituents in compound clindamycin hydrochloride ointment. The ointment should be stored in sealing container filled with nitrogen in low temperature.
出处
《中国抗生素杂志》
CAS
CSCD
北大核心
2009年第5期291-293,共3页
Chinese Journal of Antibiotics
关键词
复方盐酸克林霉素软膏
HPLC
含量测定
克林霉素
维A酸
异维A酸
稳定性考察
Compound clindamycin hydrochloride ointment
HPLC
Content determination
Clindamycin hydrochloride
Tretinon
Isotretinon
Stability evaluation.
