摘要
目的建立直接进样毛细管气相色谱法测定JS1-1-01原料药中7种有机溶剂残留量。方法采用DB-5色谱柱(30 mm×0.32 mm,1.0μm),氮气作为载气,氢火焰离子化检测器,采用N,N-二甲基甲酰胺作为溶剂,外标法分析,检测JS1-1-01原料药中残留溶剂。结果甲醇、乙醇、丙酮、二氯甲烷、甲基环己烷、吡啶和甲基吡咯烷酮线性关系良好(r=0.999 5~0.999 8),平均回收率为86.8%~100.7%,定量限分别为3.02、5.00、5.01、12.05、4.79、2.03和、4.26 mg·L-1。结论建立的方法简单、快速、分离效果好,适用于JS1-1-01中7种残留溶剂的同时检测。
Objective To establish a capillary gas chromatography method for the determination of seven kinds of residual solvents in JS1-1-01.Methods The samples were separated on DB-5 capillary column(30 mm×0.32 mm,1.0 μm) and analyzed with FID detector.Nitrogen was used as carrier gas and the method was calculated by external standard with N,N-dimethylformamide as solvent.Results There were good linear relationships in the experimental concentrations of methanol,ethanol,acetone,dichloromethane,methylcyclohexane,pyridine and methylpyrrolidone(r=0.999 5-0.999 8).The average recoveries ranged from 86.8% to 100.7%.The limits of quantification were 3.02,5.00,5.01,12.05,4.79,2.03,4.26 mg·L-1,respectively.Conclusion The method is simple,rapid and accurate and has good separation effect.It is suitable for the simultaneous detection of seven residual solvents in JS1-1-01.
作者
闫丽晔
韩民
马晓慧
赵锦花
于治国
赵云丽
YAN Liye;HAN Min;MA Xiaohui;ZHAO Jinhua;YU Zhiguo;ZHAO Yunli(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China;Chem-Pharm R&D Institute,Tasly Holding Group Company,Tianjin 300402,China)
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2020年第2期148-151,共4页
Journal of Shenyang Pharmaceutical University
关键词
气相色谱法
JS1-1-01
原料药
残留溶剂
同时检测
gas chromatography
JS1-1-01
active pharmaceutical ingredient
residual solvents
simultaneous detection
