Determination of 9 Residual Solvents in Irbesartan by GC / 中国药师

ABSTRACT

Objective:To establish a method for the determination of 9 residual solvents including methanol, ethanol, acetone, i-sopropyl alcohol, acetonitrile, dichloromethane, methyl-butyl ether, ethyl acetate and methylbenzene by capillary gas chromatography. Methods:The residual solvents were separated on a Kromat KB-624(30 m × 0. 53 mm,3. 0 μm) capillary chromatographic column with temperature programming. Nitrogen was used as the carrier gas with the flow rate of 5. 0 ml·min-1 . The temperature of injector was 200 ℃. A flame ionization detector was used with the temperature of 250℃. The containers of head-space injector were in equilib-rium at 80℃ for 20 min. Dimethyl sulfoxide was used as the solvent and an external standard method was used for the determination of the 9 residual solvents. The injection volume was 1 ml. Results:Under the above conditions, the 9 solvents were well separated. There was good linear relationship within the concentration range, and the correlation coefficients were no less than 0. 9991. The average re-coveries were 99. 08%-105. 14% with RSD of 1. 1%-3. 3%(n=9). The LOQ was 15. 68, 25. 45, 1. 09, 10. 61, 4. 54, 5. 73, 1. 04, 10. 58 and 1. 89 μg, respectively. Conclusion:The established method is simple, accurate and reproducible, and can be used in the determination of residual solvents in irbesartan API.