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目的建立气相色谱法测定利伐沙班原药中N,N-二异丙基乙胺残留物含量的方法。方法采用Agilent HP-5(30 m×0.53 mm,5.0μm)毛细管柱,FID检测器,进样口温度200℃,检测器温度250℃,程序升温,载气为氮气,流速为4 ml/min,分流比为10∶1,进样量为1μl。结果 N,N-二异丙基乙胺与样品中其他残留溶剂均能得到有效分离,其定量限为2.53μg/ml,其浓度在5.12~76.73μg/ml(r=0.9992)范围内线性关系良好,平均回收率(n=12)为100.6%,RSD为1.6%。结论该方法简便、专属、灵敏、准确,可用于利伐沙班原药中N,N-二异丙基乙胺的检测。
Objective To establish a method for the determination of N, N-diisopropylethylamine residues in rivaroxaban by gas chromatography. Methods The Agilent HP-5 (30 m × 0.53 mm, 5.0 μm) capillary column and FID detector were used. The inlet temperature was 200 ℃, the detector temperature was 250 ℃, and the temperature was programmed. The carrier gas was nitrogen and the flow rate was 4 ml / min , Split ratio of 10: 1, injection volume of 1μl. Results The N, N-diisopropylethylamine and other residual solvents in the sample could be effectively separated with a limit of quantification of 2.53μg / ml and a linear range of 5.12-76.73μg / ml (r = 0.9992) Good, average recovery (n = 12) was 100.6%, RSD was 1.6%. Conclusion The method is simple, sensitive, accurate and accurate and can be used for the determination of N, N-diisopropylethylamine in rivaroxaban.