Development and Validation of a Gas Chromatography Method for Quality Control of Residual Solvents in Azilsartan Bulk Drugs.

Autor: Guan J; School of Applied Chemistry, Shenyang University of Chemical Technology, Economic and Technological Development Zone 11th street, Shenyang City, Liaoning Province, People's Republic of China., Min J; School of Applied Chemistry, Shenyang University of Chemical Technology, Economic and Technological Development Zone 11th street, Shenyang City, Liaoning Province, People's Republic of China., Yan F; School of Applied Chemistry, Shenyang University of Chemical Technology, Economic and Technological Development Zone 11th street, Shenyang City, Liaoning Province, People's Republic of China., Xu WY; School of Applied Chemistry, Shenyang University of Chemical Technology, Economic and Technological Development Zone 11th street, Shenyang City, Liaoning Province, People's Republic of China., Shi S; School of Applied Chemistry, Shenyang University of Chemical Technology, Economic and Technological Development Zone 11th street, Shenyang City, Liaoning Province, People's Republic of China., Wang SL; School of Applied Chemistry, Shenyang University of Chemical Technology, Economic and Technological Development Zone 11th street, Shenyang City, Liaoning Province, People's Republic of China.
Jazyk: angličtina
Zdroj: Journal of chromatographic science [J Chromatogr Sci] 2017 Apr 01; Vol. 55 (4), pp. 393-397.
DOI: 10.1093/chromsci/bmw192
Abstrakt: A new gas chromatographic method for the simultaneous determination of six organic residual solvents (acetonitrile, tetrahydrofuran, ethanol, acetone, 2-propanol and ethyl acetate) in azilsartan bulk drug is described. The chromatographic determination was achieved on an OV-624 capillary column employing programmed temperature within 21 min. The validation was carried out according to International Conference on Harmonization validation guidelines. The method was shown to be specific (no interference in the blank solution), sensitive (Limit of detection can achieve 1.5 μg/mL), precise (relative standard deviation of repeatability and intermediate precision ≤5.0%), linear (r≥ 0.999), accurate (recoveries range from 98.8% to 107.8%) and robust (carrier gas flow from 2.7 to 3.3 mL/min, initial oven temperature from 35°C to 45°C, temperature ramping rate from 19°C/min to 21°C/min, final oven temperature from 145°C to 155°C, injector temperature from 190°C to 210°C and detector temperature from 240°C to 260°C did not significantly affect the system suitability, test parameters and peak areas). This extensively validated method has been applied to the determination of residual solvents in real azilsartan bulk samples.
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Databáze: MEDLINE
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