HPLC法测定卤米松乳膏中有关物质  

Determination of related substances in halomethasone ointment by HPLC

作　　者：安明 常珍 吕宁 郎昌野 孙静芬 AN Ming;CHANG Zhen;LV Ning;LANG Chang-ye;SUN Jing-fen(Beijing Horicin Biotechnology Co.,Ltd.,Beijing 100023,China)

机构地区：[1]北京华睿鼎信科技有限公司,100023

出　　处：《中国医药生物技术》2022年第1期25-34,共10页Chinese Medicinal Biotechnology

摘　　要：目的建立HPLC法检测卤米松乳膏中的有关物质。方法采用AgilentZORBAXSB-C18色谱柱(4.6mm×250 mm,5μm);以0.03%冰醋酸为流动相A,乙腈为流动相B,按一定程序进行梯度洗脱;流速为0.8 ml/min;检测波长为238 nm;柱温为35℃;进样体积为20μl。结果该法专属性良好;干扰性符合相关规定,卤米松与相邻杂质以及各已知杂质之间的分离度均良好(R> 1.5);卤米松和各已知杂质的浓度与峰面积之间线性关系良好(r≥0.9992),精密度良好;准确度良好(在50%、100%和150%限度浓度下,制剂中各杂质回收率均在92%~105%之间);校正因子耐用性和方法耐用性均良好;卤米松乳膏3批自制品与2批参比制剂的杂质谱基本一致,各批样品均符合制订质量标准的规定。结论所建立的方法可用于简便、快速、准确地检测卤米松乳膏中的有关物质。Objective To establish a method for determination of the related substances in halomethasone ointment by HPLC.Methods The condition of the chromatographic system was as follows: the column used was Agilent ZORBAX SB-C18(4.6 mm ×250 mm, 5 μm);the mobile phase A was 0.03% glacial acetic acid and the mobile phase B was acetonitrile;gradient elution was performed according to a certain procedure;the flow rate was 0.8 ml/min and the detection wavelength was 238 nm;the column temperature was 35℃ and the injection volume was 20 μl.Results The validation demonstrated that the established method possessed good specificity, satisfactory interference, and there was a good separation between halomethasone and adjacent impuritie and known impurities(R > 1.5). The linear relationship between the concentration and corresponding peak area of all related substances were ideal(r ≥ 0.9992), the precision, accuracy and durability of correction factor and method were fine, and the recoveries of impurities in the preparation were 92% ~ 105% at the limit concentration of 50%, 100% and 150%. The impurity spectra of 3 batches of self-made preparations and 2 batches of reference preparations of halomethasone ointment were basically consistent, complying with the established quality standards.Conclusion The established method is simple, prompt, and accurate, which can be used to determine the related substances in halomethasone ointment.

关 键 词：卤米松 乳膏 高效液相色谱法 有关物质 

分 类 号：O657.72[理学—分析化学] TQ460.72[理学—化学]