HPLC测定吉非替尼中的有关物质

Determination of the related substances in Gefitinib by HPLC

目的采用HPLC法测定吉非替尼中的有关物质。方法色谱柱为Phenomenex C_(18)柱(250 mm×4.6 mm,5μm),柱温40℃,流速1.0 m L·min^(-1),流动相为乙腈-乙酸铵缓冲液(1.5 g乙酸铵中加入1 L水溶解,加氨水调p H8.50±0.05),梯度洗脱,检测波长247 nm,进样量20μL。结果杂质Ⅰ~Ⅸ的线性范围分别为0.2101~1.2020、0.1940~3.880、0.2000~4.000、0.1920~3.8400、0.1952~3.904、0.2020~4.0400、0.1950~3.900、0.2022~4.0480、0.1920~3.8440μg·m L^(-1);检测限(S/N=3)分别为225、44.5、48.0、59.4、77.6、75.2、72.0、144、291 ng·m L^(-1)。结论所用方法灵敏、专属、准确,适用于吉非替尼有关物质的测定。

OBJECTIVE To establish an HPLC method for the determination of the related substances in Gefitinib. METHODS Analysis was carried out on a Phenomenex C18 column（250 mmx 4.6 mm ,5 μm） using acetonitrile- ammonium acetate buffer（ 1.5 g of ammonium acetate with 1 L water, adding ammonia to adjust the pH to 8.50±0.05） as the mobile phase. The injection volume was 20 μL and the column temperature was 40 ℃. The detection wavelength was 247 nm, and the flow rate was 1.0 mL·min^-1. RESULTS The linear ranges of impurity Ⅰ- Ⅸ were 0. 2101 - 1. 2020 μg·m L^-1,0. 1940 - 3. 880 μg·m L^-1 ,0. 2000 - 4. 000 μg·m L^-1, 0. 1920 - 3. 840 μg·m L^-1 ,0. 1952 - 3. 9040 μg·m L^-1 ,0. 2020 - 4. 0400 μg·m L^-1 ,0. 1950 - 3. 900 μg·m L^-1 ,0. 2022 - 4. 0480 μg·m L^-1 and 0. 1920 - 3. 8440 μg·m L^-1, respectively. The limits of detection （ S/N = 3 ） was 225,44.5,48.0,59.4,77.6,75.2,72. 0,144 and 291 ng·m L^-1,respectively. CONCLUSION The method is sensitive, exclusive, accurate and suitable for the determination of the related substances in Gefitinib.