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Simultaneous determination of related substances in entecavir film-coated tablet by high performance liquid chromatography |
ZHANG Yi( ),YUAN Hong( ) |
College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310058, China |
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Abstract 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.
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Received: 10 April 2021
Published: 01 November 2021
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Corresponding Authors:
YUAN Hong
E-mail: zyi0571@sina.com;yuanhong70@zju.edu.cn
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利用高效液相色谱法同时检测恩替卡韦薄膜衣片中的有关物质
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,5?μm),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。
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
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