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目的:建立尼达尼布的有关物质测定方法,并进行方法学验证。方法:采用XBridge RP-C_(18)色谱柱(250 mm×4.6 mm,3.5μm),以甲醇-0.1%三氟乙酸为流动相进行梯度洗脱,流速为1.0 ml·min~(-1),检测波长为287 nm,柱温为35℃,进样量为10ul。结果:主成分与各杂质峰分离度良好,杂质1~4分别在0.103 0~1.030 4μg·ml~(-1)(r=0.999 5),0.202 9~1.014 5μg·ml~(-1)(r=0.999 7),0.199 9~0.999 6μg·ml~(-1)(r=0.999 9),0.200 6~1.002 9μg·ml~(-1)(r=0.998 4)范围内线性关系良好,检测限分别为0.31,0.61,0.60,0.60 ng;平均回收率分别为98.3%、99.3%、97.9%、99.8%,RSD分别为2.1%、2.1%、3.0%、1.1%。结论:该方法简便,准确,灵敏度高,专属性强,适用于本品有关物质的测定。
OBJECTIVE: To establish a method for the determination of nadinib and to verify the methodology. METHODS: The gradient elution was performed on a XBridge RP-C 18 column (250 mm × 4.6 mm, 3.5 μm) using methanol-0.1% trifluoroacetic acid as the mobile phase at a flow rate of 1.0 ml · min -1 , The detection wavelength was 287 nm, the column temperature was 35 ℃, the injection volume was 10ul. Results: The main components and impurity peaks were separated well. The impurity contents ranged from 0.103 0 to 1.030 4 μg · ml -1 (r = 0.999 5) and from 0.202 9 to 1.014 5 μg · ml -1 (r = 0.999 7), 0.199 9-0.999 6 μg · ml -1 (r = 0.999 9), 0.200 6-1.002 9 μg · ml -1 (r = 0.998 4) The average recovery rates were 98.3%, 99.3%, 97.9% and 99.8%, respectively. The RSDs were 2.1%, 2.1%, 3.0% and 1.1% respectively. Conclusion: The method is simple, accurate, sensitive, specific and applicable to the determination of related substances in this product.