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目的建立以毛细管气相色谱法测定利伐沙班原料药中乙醇、二氯甲烷、四氢呋喃、三乙胺、吡啶、乙酸、N,N-二甲基甲酰胺(DMF)7种有机溶剂残留量的方法。方法采用Agilent DB-624(30.0 m×0.32 mm,1.8μm)毛细管柱,载气为氮气,采用氢火焰离子化检测器(FID),进样口温度为200℃,检测器温度为240℃,柱温采用程序升温,流速为2.0 m L·min?1,进样量1μL。结果无水乙醇、二氯甲烷、四氢呋喃、三乙胺、吡啶、乙酸、DMF均能得到较好的分离,呈现良好的线性关系,平均回收率分别为102.4%,100.1%,96.5%,91.6%,103.6%,106.6%,102.5%,RSD均<5.0%。结论本方法简便、快速、准确性好、灵敏度高,可用于利伐沙班原料药中残留溶剂的测定。
OBJECTIVE To establish a method for the determination of the residues of 7 organic solvents of ethanol, dichloromethane, tetrahydrofuran, triethylamine, pyridine, acetic acid and N, N-dimethylformamide in rivaroxaban hydrochloride by capillary gas chromatography method. Methods A capillary column with an Agilent DB-624 (30.0 m × 0.32 mm, 1.8 μm) was used. The carrier gas was nitrogen and hydrogen flame ionization detector (FID) was used. The inlet temperature was 200 ° C and the detector temperature was 240 ° C. The column temperature was programmed temperature, flow rate 2.0 m L · min -1, injection volume 1μL. The results showed that ethanol, dichloromethane, tetrahydrofuran, triethylamine, pyridine, acetic acid and DMF could all be separated well with a good linear relationship. The average recoveries were 102.4%, 100.1%, 96.5% and 91.6% , 103.6%, 106.6% and 102.5%, respectively. The RSDs were all less than 5.0%. Conclusion The method is simple, rapid, accurate, sensitive and can be used for the determination of residual solvents in rivaroxaban APIs.