更昔洛韦及其注射液杂质分析

目的: 对更昔洛韦原料及注射液中的杂质进行检测、鉴定,并进行方法学研究。方法: 采用Agilent ZORBAX 300-SCX(4.6 mm×250 mm,5 μm)色谱柱,以乙腈-0.05%三氟乙酸(50:50)为流动相,检测波长254 nm,柱温40℃;Q ExactiveTM质谱系统配有HESI源,采用正离子模式,喷雾电压3.0 kV,毛细管温度350℃,雾化器250℃,鞘气0.28 MPa,辅助气0.1 MPa,S-lens RF电压50 V。结果: 更昔洛韦与各杂质及强制破坏产物能完全分离,主峰纯度因子均大于999.0,试验样品最大和次大杂质确证为鸟嘌呤和杂质A,来源为合成引入或工艺杂质。结论: 本法准确、灵敏,杂质检出性强,适用于更昔洛韦及其注射液杂质的测定。

Objective: To detect and identify the impurities in ganciclovir and ganciclovir injection and to validate the method for the determination of impurities. Methods: The analysis was performed on an Agilent ZORBAX 300-SCX (4.6 mm×250 mm,5 μm) column and the mobile phase was acetonitrile-0.05% trifluoroacetic acid (50:50). The detection wavelength was 254 nm,and the column temperature was at 40℃.The target compounds were analyzed with ExactiveTM Q mass spectrometry system with HESI in positive ion mode.The spray voltage was 3.0 kV,the capillary temperature was 350℃,the atomizer was 250℃,the sheath gas was 0.28 MPa,the auxiliary gas was 0.1 MPa,and the S-lens RF voltage was 50 V. Results: Ganciclovir was separated completely from known impurities and degradation products under various conditions with the purity factor greater than 999.0. The largest impurity and the second largest one were guanine and impurity A. It was confirmed that the two major impurities came from synthetic introduction or synthetic process of the material. Conclusion: The method is accurate,sensitive and can be used for determination of the impurities of ganciclovir and ganciclovir injection.

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