顶空气相色谱法测定比伐芦定原料药中三乙胺残留量

Determination of Residual Solvent Triethylamine in Bivarudin by Headspace GC

建立了顶空气相色谱法测定比伐芦定中三乙胺的残留量.顶空进样毛细管气相色谱法,采用DB-1毛细管色谱柱,柱温100℃,载气为氮气,检测器为氢火焰检测器.在上述色谱条件下三乙胺峰形最佳,三乙胺在1.9～17.5 μg/mL浓度范围内,呈良好线性关系（r=0.9995）;三乙胺回收率为101.2 ％（RSD=0.5％）;定量限为0.19 μg/mL,检测限为90 ng/mL.本方法准确可靠,简便灵敏,重现性好,可用于比伐芦定中三乙胺残留量的测定.

A headspace gas chromatography method for determination of residual triethylamine in bivarudin was established. It was quantitatively determined by headspace gas chromatography on DB-1 capillary column with FID detector, nitrogen as the carries. The column temperature was 100 ~C. The peak shape of triethylamine is quite well. Triethylamine presented a good linear correlation in range of 1.9-17.5 μg/mL, the correlation coefficient is 0.9995. The recoveries of triethylamine was 101.2 % （RSD=0.5 %）. The limit of quantification is 0.19 μg/mL. The detection limit is 90 ng/mL. This method is definite, reliable, and simple, and can be used for determination of residual triethylamine in bivarudin.