Determination of Residual Solvents in Tulobuterol by Gas Chromatography
10.3870/j.issn.1004-0781.2018.11.020
- VernacularTitle:气相色谱法测定妥洛特罗中有机溶剂残留量
- Author:
Zhiqiang WANG
1
;
Yongzhuo LI
;
Huajin TAN
;
Hui SONG
;
Ya MENG
;
Yujia ZHANG
;
Jinsong LIU
;
Wensheng ZHENG
Author Information
1. 安徽中医药大学药学院
- Keywords:
Tulobuterol;
Residual solvent;
Chromatography,capillary gas;
Purification of crude product
- From:
Herald of Medicine
2018;37(11):1377-1380
- CountryChina
- Language:Chinese
-
Abstract:
Objective To establish a method for the determination of residual solvents in tulobuterol by GC and optimize the purified process of crude tulobuterol product by this method. Methods The analysis was performed on Agilent DB-624 capillary column (30 m×0.32 mm,1.8 μm).The carrier gas was nitrogen at 1 mL·min-1.The injector temperature was 250 ℃.Detector was FID with hydrogen at 45 mL·min-1and air at 450 mL·min-1.The detector temperature was 250 ℃.The column temperature program was used.And the flow ratio was 10:1.Dimethyl sulfoxide (DMSO) was used as solvent of reference and test solution. Results Ethanol,tert-butylamine,dichloromethane,tert-butyl-methyl ether,n-hexane and 1,4-dioxane were completely separated.The calibration curve of each solvent showed good linear correlation. The RSD of precision was less than 5.0% and the average recovery ranged from 97.0% to 104.0% (RSD<5%).By optimizing the purification process of toloterol,the residue of organic solvent in the preparation of tolobuterol was in accordance with the Chinese Pharmacopoeia ( 2015) limit. Conclusion Validated by methodology,this simple,rapid and precise method can be used for the test of residual solvents in tulobuterol.
