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目的建立测定二甲苯磺酸拉帕替尼片有关物质的高效液相色谱法。方法采用Waters Xterra MS C18色谱柱(4.6mm×250 mm,5μm);以0.01 mol.L-1磷酸二氢钠溶液(用磷酸调节pH值至3.2)为流动相A,以乙腈为流动相B,梯度洗脱,流速1.0 mL.min-1;检测波长265 nm,柱温40℃。结果拉帕替尼杂质A、拉帕替尼杂质2和拉帕替尼杂质1分别在0.02～8.08、0.02～8.26和0.02～8.29 mg.mL-1内线性关系良好,r≥0.999 9,定量限分别为1.0、1.4、2.1 ng,杂质高、中、低浓度的平均回收率(n=9)在100.2%～102.9%,RSD(n=9)在0.02%～0.66%,可以满足杂质分析的要求。结论本方法简便、准确、专属性强,可定量测定二甲苯磺酸拉帕替尼片的有关物质。
OBJECTIVE To establish a HPLC method for the determination of related substances in lapatinib ditosylate tablets. Methods A Waters Xterra MS C18 column (4.6 mm × 250 mm, 5 μm) was used. The mobile phase A was consisted of 0.01 mol·L-1 sodium dihydrogen phosphate solution (adjusted to pH 3.2 with phosphoric acid) and acetonitrile as mobile phase B , Gradient elution, flow rate 1.0 mL.min-1; detection wavelength 265 nm, column temperature 40 ℃. Results The linear relationship between lapatinib impurity A, lapatinib impurity 2 and lapatinib impurity 1 was 0.02 ~ 8.08, 0.02 ~ 8.26 and 0.02 ~ 8.29 mg.mL-1 respectively, r≥0.999 9, (N = 9) ranged from 100.2% to 102.9% and RSD (n = 9) ranged from 0.02% to 0.66%, respectively, which could meet the impurity analysis Request. Conclusion The method is simple, accurate and specific, and can quantitatively determine the related substances of lapatinib ditosylate tablets.