气相色谱法测定利伐沙班原药中N,N-二异丙基乙胺的残留量  

Determination of N,N-diisopropylethylamine residues in rivaroxaban APIs by gas chromatography

作　　者：马苗[1,2] 骆雪芳[1] 秦辉 王珺 朱谧 徐丹 钟文英[1] 

机构地区：[1]中国药科大学分析化学教研室,南京市210009 [2]南京正大天晴制药有限公司,南京市210038

出　　处：《临床合理用药杂志》2017年第13期1-3,共3页Chinese Journal of Clinical Rational Drug Use

摘　　要：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 gas chromatography method for the determination of residual N,N-diisopropylethylamine in rivaroxaban APIs.Methods An Agilent DB-624 capillary column（30 m×0.53 mm,3.0 μm） was adopted and the temperature of FID was 250 ℃ and the inlet temperature was 200 ℃.The temperature program method was adopted and nitrogen was used as carrier.The flow rate was 4 ml/min and the injection volumn was 1 μl.Results N,N-diisopropylethylamine and other residual organic solvents in rivaroxaban were completely separated by the method.The limit of quantification was 2.53 μg/ml.Good linearity of N,N-diisopropylethylamine was obtained within the range of 5.12~76.73 μg/ml（r=0.9992）.The average recovery was 100.6% and the RSD was 1.6%.Conclusion The established method is simple,sensitive and accurate and can be used for the determination of residual N,N-diisopropylethylamine in rivaroxaban APIs.

关 键 词：气相色谱法 N N-二异丙基乙胺 利伐沙班 残留量 

分 类 号：R927.2[医药卫生—药学]