Determination of Residual Organic Solvents in Trepibutone by Headspace Gas Chromatography
10.3870/j.issn.1004-0781.2016.09.021
- VernacularTitle:顶空气相色谱法测定曲匹布通原料药中有机溶剂残留量
- Author:
Chunyan SUN
;
Yaping ZHAO
;
Linning CHEN
;
Ying CHENG
- Publication Type:Journal Article
- Keywords:
Trepibutone;
Residual organic solvent;
Chromatography,gas;
Headspace
- From:
Herald of Medicine
2016;35(9):991-993
- CountryChina
- Language:Chinese
-
Abstract:
Objective To establish a headspace GC method for determination of residual organic solvents as methanol, ethanol,dichloromethane and n-hexane in trepibutone. Methods An external standard method was used. A DB-624 capillary column (75 m× 0.450 mm,2.55 μm) was used with a FID detector. The injector temperature was 200 ℃ and the detector temperature was 250 ℃ .The initial column temperature was 50 ℃ ,kept for 6 min,then raised to 200 ℃ at a rate of 20 ℃ ?min-1 and kept for another 12 min. Nitrogen was used as the carrier gas. The flow rate was 3. 0 mL ? min-1 . The headspace vials equilibrium temperature was 80 ℃ and the balance time was 30 min.The injection volume is 1 mL. Results A1l the solvents could be completely separated with good linear relationships.The average recoveries of the four solvents were 100.4% ( RSD =0.5%), 100.6%(RSD = 0.6%), 99.6% ( RSD = 0.8%), 98.7% ( RSD = 0.7%) ( n = 9),respectively. Conclusion The method is simple and accurate,and can be used in the determination of residual solvents in trepibutone.
