Method for detecting residual solvent in nilotinib bulk drug

The invention discloses a method for determining the residual amount of a solvent in a nilotinib bulk drug by headspace gas chromatography. The method comprises the following specific steps of (1) preparing a reference substance solution of the residual solvent to be detected, (2) preparing a test solution, and (3) detecting the sample, and calculating and simultaneously detecting seven organic solvents, namely methanol, ethanol, isopropanol, dichloromethane, n-hexane, ethyl acetate and methylbenzene according to an external standard method by utilizing a flame ionization detector (FID) through temperature programming and headspace sampling modes. The method is simple, sensitive, accurate and suitable for quality control of nilotinib raw materials in industrial production. 本发明公开了一种顶空气相色谱法测定尼洛替尼原料药中的溶剂残留量的方法，所述方法具体步骤为：(1)制备待检测残留溶剂对照品溶液；(2)制备供试品溶液；(3)检测样品，利用氢火焰离子化检测器(FID)，经程序升温，顶空进样方式，最后按外标法计算，同时检测甲醇、乙醇、异丙醇、二氯甲烷、正己烷、乙酸乙酯和甲苯7种有机溶剂。本发明方法简单，灵敏准确，适用于工业化生产中尼洛替尼原料的质量控制。