OBJECTIVE: To establish simultaneous determination of 7 kinds of residual solvents in vorapaxar sulfate raw material. METHODS: The headspace gas chromatography was performed on Agilent DB-624 capillary column(programmed temperature) with inlet temperature of 220 ℃, detection temperature of 250 ℃ using nitrogen(99.999%) as carrier gas at the flow rate of 2.0 mL/min. The split ratio was 20 ∶ 1, and sample size was 1 mL. The headspace equilibrium temperature was 80 ℃,headspace equilibrium time was 30 min. RESULTS: The linear range of ethyl acetate, methanol, dichloromethane, ethanol, acetonitrile, tetrahydrofuran and toluene were 2.0-201.0 μg/mL(r=0.999 8), 1.2-122.3 μg/mL(r=0.999 4), 0.24-24.0 μg/mL(r=0.999 2), 2.0-200.3 μg/mL(r=0.999 9), 0.2-16.7 μg/mL(r=0.999 9), 0.3-29.0 μg/mL(r=0.999 3), 0.4-35.8 μg/mL(r=0.999 3), respectively. The limits of quantification were 2.0, 1.2, 0.24, 2.0, 0.2, 0.3, 0.4 μg/mL; the limits of detection were 0.60, 0.30, 0.07, 0.60, 0.06, 0.09, 0.12 μg/mL. RSDs of precision, stability and reproducibility tests were all lower than 4%. The recoveries were 97.02%-99.84%(RSD=0.88%,n=9), 98.05%-99.64%(RSD=0.54%,n=9), 97.37%-100.00%(RSD=0.83%,n=9), 98.67%-99.60%(RSD=0.34%,n=9), 97.56%-99.76%(RSD=0.79%,n=9), 97.22%-99.45%(RSD=0.65%,n=9), 97.75%-99.33%(RSD=0.59%,n=9), respectively. RSDs of durability tests were all lower than 8%. Methanol, ethanol were detected in samples. CONCLUSIONS: The method is simple, accurate, precise, stable, reproducible and durable, and can be used for simultaneous determination of 7 kinds of residual solvents in vorapaxar sulfate raw material.
关键词
顶空气相色谱法硫酸沃拉帕沙残留溶剂
Keywords
Headspace gas chromatographyVorapaxar sulfateResidual solvents