期刊论文

Determination of residual solvents in rabeprazole sodium raw material by headspace gas chromatography

中文

长沙理工大学学报(自然科学版)

1672-9331

2016

13

1

93-98

10.3969/j.issn.1672-9331.2016.01.015

湖南省教育厅科研资助项目（14A012）；

本校为第一机构

利用气相色谱法测定雷贝拉唑钠原料药中丙酮、乙腈、二氯甲烷、乙酸乙酯和甲苯5种有机溶剂残留量,通过优化实验条件建立了一种有效的测定有机溶剂残留量的方法。采用顶空毛细管气相色谱法,检测器为氢火焰离子化检测器,色谱柱为 DB-624石英毛细管柱,以氮气为载气,流速为2.0 mL/min；柱温采取程序升温方式,于40℃保持8 min,然后以每分钟20℃的速率升温至240℃,并保持20 min；顶空平衡温度为90℃,平衡时间为30 min；进样口温度为200℃,检测温度为250℃；进样体积为1 mL,分流比为5∶1。5种有机溶剂在该色谱条件下均能有效分离,峰面积与浓度呈现良好的线性关系,相关系数 R 圴大于0.990,检出限(3S/N)分...

A gas chromatography(GC)method was developed for the determination of five residual solvents including acetone,acetonitrile,dichloromethane,ethyl acetate and toluene in rabeprazole sodium raw material.Based on the optimized experimental conditions,an ef-fective method for determining the residual amount of organic solvent was established.A headspace capillary GC with FID detector was selected to determine 5 kinds of organic as ac-etone,acetonitrile,dichloromethane,ethyl acetate and toluene.The determination was per-formed on DB-624 capillary co...