摘要
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 and verify an HPLC method for determining the related substances in nintedanib. Methods： An XBridge RP-Cls （250 mm x4.6 Into,3.5 pLm） column was used, and the column temperature was set at 35~C. The mobile phase was composed of methanol and 0.1% trifluoroaeetic acid with gradient elution. The flow rate was 1.0 ml·min^-1. The detection wavelength was 287 nm. The injection volume was 10μl. Results： Nintedanib and its related substances could be well separated, and impurity 1-4 showed a good linear relationship within the range of 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 ） and 0.200 6-1. 002 9μg·ml^-1（ r = 0.998 4 ）, respectively. The detection limit was 0.31, 0.61, 0.60, 0.60 ng, the average recovery was 98.3%, 99.3%, 97.9% and 99.8%, and RSD was 2.1%, 2.1%, 3.0% and 1.1%, respectively. Conclusion： The method is simple and accurate with high sensitivity and strong specificity, which is suitable for the determination of the relatedsubstances in nintedanib.
出处
《中国药师》
CAS
2016年第11期2188-2192,共5页
China Pharmacist
