气相色谱法测定阿哌沙班中8种残留溶剂

Detection of Residual Organic Solvent in Apixaban by Gas Chromatography

建立了气相色谱法测定阿哌沙班中残留溶剂的方法,以二甲基亚砜为溶剂配制对照溶液及供试品溶液,采用DB-624(30 m×0.32 mm×1.8μm)的毛细管柱程序升温,以氮气为载气,顶空进样,FID为检测器,进样口温度为250℃,检测器温度为300℃,对阿哌沙班中8种残留溶剂进行了测定。结果表明,样品中甲醇、二氯甲烷、叔丁醇、乙酸乙酯、四氢呋喃、三乙胺、N,N-二甲基甲酰胺、1,2-丙二醇相互间的分离度及检测灵敏度均符合要求。该方法简便、快速、灵敏、结果准确可靠,可用于阿哌沙班中残留有机溶剂的测定。

To detect the residues of eight kinds of organic solvent in Apixaban,a gaschromatography method was established. The detector was FID. The analytical column was DB-624（ 30 m × 0. 32 mm,1. 8 μm）. The temperature of injector was 250 ℃,and300 ℃ to the detector. The column temperature was programmed raised. N2 was used as the carrier gas. The eight kinds of residual organic solvent（ methyl alcohol,dichloromethane,t-butanol,ethyl acetate,tetrahydrofuran,triethylamine,N,N-dimethylformamide,1,2-propanediol） in Apixaban sample were separated completely. The resolution and sensitivity were acceptable. This method was simple,sensitive,accurate,and can be used for detection of eight kinds of residual solvent in Apixaban.