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高效液相色谱法测定扎那米韦含量及有关物质
高效液相色谱法测定扎那米韦含量及有关物质
董 虹1,张欢欢2,黄 晴2,曹日昇3,周 雅2,胡一桥1

1 南京大学医学院,南京 210093;2 南京大学生命科学院,南京 210093;3 江苏省人民医院,南京 210008
HPLC determination of zanamivir content and the related substances
(1 Medical School of Nanjing University, Nanjing 210093, China; 2 School of Life Sciences, Nanjing University, Nanjing 210093, China; 3 Jiangsu Province Hospital, Nanjing 210008, China)

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起始页:31

摘要:[摘要] 目的:建立测定扎那米韦的含量和有关物质的高效液相方法。方法:采用NH2P-50色谱柱(250 mm×4.6 mm,5 μm),流动相为乙腈-5 mmol?L-1硫酸溶液(60∶40)[用氨水调节pH至(6.2±0.05)];检测波长为234和210 nm;流速为1.0 mL?min-1,柱温为30 ℃。同时采用液质联用对各杂质进行了结构确证。结果:主药与各杂质、各杂质之间分离度良好,各杂质能有效检出。在100.10~1 001.0 μg?mL-1浓度范围内,扎那米韦与其峰面积呈良好的线性关系(r=0.999 9,n=5),最小检测限为25.0 ng?mL-1,含量测定及有关物质检查的中间精密度RSD分别为0.24%(n=6)与1.24%(n=6)。结论:本法简便、精密、专属、灵敏,可用于扎那米韦含量和有关物质测定。

关键词:[关键词] 扎那米韦;含量;有关物质;高效液相色谱

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Abstract:[Abstract] Objective: To develop an HPLC method for simultaneously determining zanamivir content and its related substances for quality control. Methods: The method was performed on an Asahipak NH2P-50 column (250 mm×4.6 mm, 5 μm) with acetonitrile-5 mmol?L-1 sulphuric acid (60∶40) [adjusting pH to (6.2±0.05) with ammonia solution] as the mobile phase. The flow rate was 1.0 mL?min-1. The detection wavelength was 234 and 210 nm, and the column temperature was set at 30 ℃. Meanwhile, the structure of each impurity was confirmed by LCMS. Results: Zanamivir was completely separated from the related substances. The calibration curve of zanamivir was linear (r=0.999 9, n=5) in the range of 100.10~1 001.0 μg?mL-1; detection limit was 25.0 ng?mL-1; the intermediate precisions RSD were 0.24% and 1.24% (n=6) in the content and related substance determination. Conclusion: The method is simple, accurate, specific and sensitive for simultaneously determining the content and its related substances of zanamivir.

Key words:[Key words] zanamivir; content; related substances; HPLC

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