摘要
目的:建立能够同时测定恩替卡韦薄膜衣片8种有关物质的高效液相色谱法。方法:参考美国药典40和中美上海施贵宝制药有限公司的恩替卡韦薄膜衣片(博路定)标准(YBH33292005)等,采用WATERS C18色谱柱(250 mm×4.6 mm,5μm),流动相A为水-乙腈-三氟乙酸(990∶10∶1),流动相B为水-乙腈-三氟乙酸(700∶300∶1),梯度洗脱,采用紫外-可见光检测器,检测波长为254 nm,柱温30℃,建立同时测定恩替卡韦薄膜衣片8种有关物质的高效液相色谱法,并对该检测方法进行方法学验证。结果:恩替卡韦与各杂质峰之间的分离度均大于1.5,8种有关物质在线性范围内均与峰面积成良好的线性关系,检测限、定量限、精密度、稳定性、耐用性、专属性等均符合要求。结论:本研究建立的高效液相色谱法可同时检测恩替卡韦薄膜衣片常见的8种有关物质。
Objective:To establish a high performance liquid chromatography method to simultaneously quantify eight related substances in entecavir film-coated tablets.Methods:According to USP40 and YBH33292005 standards,a high performance liquid chromatography(HPLC) method for simultaneous determination of 8 related substance in entecavir film-coated tablets was established and validated.The column was WATERS C18(250 mm×4.6 mm,5 μm),the mobile phase A was water-acetonitrile-trifluoroacetic acid(990:10:1),the mobile phase B was water-acetonitrile-trifluoroacetic acid(700:300:1) with gradient elution and ultraviolet-visible light detector,detection wavelength at 254 nm and column temperature of 30 ℃.Results:The resolution between entecavir and each impurity peak was more than 1.5,and each impurity had a good linear relationship with the peak area in the linear range.The limits of detection and quantification,precision,stability,durability,specificity,met the verification requirements.Conclusion:The HPLC method established in this study can be used for simultaneous determination of 8 related substance in entecavir film-coated tablets.
作者
张翼
袁弘
ZHANG Yi;YUAN Hong(College of Pharmaceutical Sciences,Zhejiang University,Hangzhou 310058,China)
出处
《浙江大学学报（医学版）》
CAS
CSCD
北大核心
2021年第4期529-536,共8页
Journal of Zhejiang University(Medical Sciences)
关键词
色谱法
液相
恩替卡韦
薄膜衣片
紫外-可见光检测器
有关物质
Chromatography,liquid
Entecavir
Film-coated tablet
Ultraviolet-visible light detector
Related substance
