Determination of 8 Residual Organic Solvents in Spironolactone by Capillary GC
- VernacularTitle:毛细管气相色谱法测定螺内酯中8种有机溶剂的残留量
- Author:
Xiaojing ZHANG
;
Yingying WANG
;
Jun LI
- Publication Type:Journal Article
- Keywords:
Capillary GC;
Spironolactone;
Residual organic solvent
- From:
China Pharmacist
2014;(12):2145-2148
- CountryChina
- Language:Chinese
-
Abstract:
Objective:To establish a determination method for 8 residual organic solvents in spironolactone by capillary GC. Methods:The determination of methanol, ethanol, acetone and tetrahydrofuran in spironolactone dissolved in dimethyl sulfoxide was carried out on a DB-624 column. The inlet temperature was 200℃ and the FID detector temperature was 250℃. The constant pressure was 2. 5psi. The column temperature was raised by program. The vial temperature was 85℃ and the time was 30min. The determination of triethylamine, pyridine, N,N-dimethylformamide and dimethyl sulfoxide in spironolactone dissolved in chloroform was carried out on an HP-1 column. The inlet temperature was 220℃ and the FID detector temperature was 250℃. The column temperature was raised by program. The flow rate of carrier gas was 3. 0ml·min-1. Results: All peaks could be separated from each other with promising resolution. The linearity of the eight solvents was fairly good(r > 0. 999). The average recovery ranged from 90. 9%-94. 3% with RSD of 1. 1%-3. 3% (n = 9). The limit of detection for methanol, ethanol, acetone, tetrahydrofuran, triethylamine, pyridine, N,N-dimethylformamide and dimethyl sulfoxide was 0. 60, 0. 67, 0. 20, 0. 15, 0. 64, 0. 36, 0. 89 and 0. 82 μg · ml-1 , respectively. Conclusion: The methods can be applied in the determination of 8 residual organic solvents in spironolactone.
