OBJECTIVE: To establish a method for simultaneous determination of 5 kinds residual ethanol, acetone, ethylacetate, N,N-diisopropylethylamine and toluene in favipiravir. METHODS: Headspace GC was adopted. The determination was performed on DB-624 capillary column, temperature programmed. The inlet temperature was 220 ℃, and detector was flame ionization detector with temperature of 250 ℃. Nitrogen was used as carrier gas at flow rate of 2.0 mL/min, split ratio was 10 ∶ 1, headspace equilibrium temperature was 80 ℃, equilibrium time was 20 min and headspace sample size was 1 mL. RESULTS: The linear range was 10.0-501.4 μg/mL for ethanol(r=0.999 9),10.0-501.4 μg/mL for acetone(r=0.999 9),10.1-502.6 μg/mL for ethylacetate(r=0.999 9),0.2-11.4 μg/mL for N,N-diisopropylethylamine(r=0.999 9)and 1.8-89.4 μg/mL for acetone(r=0.999 7). The limits of quantification were 5.3, 3.4, 5.2, 6.1 and 20.4 μg/mL, and the limits of detection were 1.4, 1.1, 1.3, 1.6, 5.9 μg/mL. RSD of precision test was lower than 4.0%, and RSDs of acetone in stability and reproducibility tests were both lower than 4.0%. The recoveries were 96.61%-99.70%(RSD=1.01%,n=9), 95.81%-99.50%(RSD=1.29%,n=9), 96.42%-99.76%(RSD=1.24%,n=9), 96.36%-99.30%(RSD=1.19%,n=9), 97.00%-99.51%(RSD=0.82%,n=9). CONCLUSIONS: The method is simple, accurate, reproducible and can be used for simultaneous determination of 5 organic solvents in favipiravir.
关键词
气相色谱法法匹拉韦有机溶剂残留量乙醇丙酮乙酸乙酯NN-二异丙基乙胺甲苯
Keywords
gas chromatographyFavipiravirOrganic solventsResidualEthanolAcetoneEthylacetateNN-diisopropylethylamineToluene