摘要
目的建立亲水柱-高效液相色谱法(HILIC-HPLC)测定吉非替尼原料药中的酸降解杂质X的检测方法。方法采用Waters Xbridge HILIC柱(4.6 mm×250 mm,5μm)为色谱柱,以乙腈-0.05mol·L^(-1)的甲酸铵缓冲液(用甲酸调节p H至4.0)(85∶15,v/v)为流动相,流速1.0 m L·min^(-1),柱温25℃,检测波长240 nm。结果杂质X在9.8 min左右出峰。吉非替尼与杂质X之间的分离度大于2.0。杂质X在0.10~1.0μg·m L^(-1)与峰面积呈良好的线性关系(r=1.000,n=6),相对校正因子为0.4,定量限和检测限分别为0.08 ng和0.02 ng,回收率在99.7%~100.5%内,RSD均<1.5%(n=3)。结论经方法学验证表明,该方法的专属性、线性关系等良好,可采用加校正因子的主成分自身对照法对本品的杂质X进行控制。
Objective To establish a hydrophilic interaction chromatography-high performance liquid chro- matography （HILIC-HPLC） method for the determination of impurity X in gefitinib raw materials. Methods HPLC was adopted on a Waters Xbridge HILIC （4.6 mm × 250 mm, 5 μm） using a mobile phase consisting of acetonitrile-0.05 mol · L ^- 1 formic acid buffer solution （pH adjusted to 4.0 with formic acid, 85 ： 15, v/v） at 1.0 mL · min ^- 1. The column temperature was 25℃ , and the detection wavelength was 240 nm. Results The reso- lution between gefitinib and impurity X was greater than 2.0. The calibration curve of impurity X was linear at 0.10 -- 1.0 μg · mL ^- 1 （r = 1.000, n = 6）. The relative correction factors were 0.4 for impurity X. The deter- mination limit and detection limit were 0.08 ng and 0.02 ng. The recovery was at 99.7% -- 100.5% （RSD 〈 1.5%, n = 3）. Conclusion The method has good specificity and linearity, which is suitable for the quality control of impurity X.
出处
《中南药学》
CAS
2017年第2期217-220,共4页
Central South Pharmacy
