采用气相色谱法测定以4-氟苯基乙酮为原料经不对称加氢还原合成(S)-1-(4-氟苯基)-乙醇反应液中各组分的含量。采用Varian capillary column cp-chirasil-Dex CB毛细管手性色谱柱和氢火焰离子化检测器,以苯丙酮为内标物进行分析。反应液中的4-氟苯基乙酮,(S)-1-(4-氟苯基)-乙醇和(R)-1-(4-氟苯基)-乙醇能很好地分离,3种组分的峰面积与其质量浓度在一定范围内呈线性关系,检出限(3S/N)在6.5~18.8 mg·L-1之间。加标回收率在95.2%~106%之间,测定值的相对标准偏差(n=5)在1.0%~7.2%之间。

GC was applied to the determination of the components in the reaction solution for asymmetric synthesis of (S)-1-(4-fluorophenyl)-ethanol with 1-(4-fluorophenyl)-ethanone as the raw material. Varian capillary column cp-chirasil-Dex CB and FID were adopted, and 1-phenyl-1-propanone was used as internal standard for analysis. 1-(4-fluorophenyl)-ethanone, (S)-1-(4-fluorophenyl)-ethanol and (R)-1-(4-fluorophenyl)-ethanol in the reaction solution were separated, and linear relationships were found between the peak areas and the mass concentrations of the 3 components in definite ranges, with detection limits (3S/N) in the range of 6.5-18.8 mg·L-1. Recovery obtained by standard addition method were in the range of 95.2%-106%, and RSDs (n=5) were in the range of 1.0%-7.2%.