气相色谱法测定R-3,5-(三氟二甲基)苯乙醇合成反应液中的相关物质

GC Determination of Related Substances in Reaction Liquid of Synthesis of R-3,5-(Trifluoro-Dimethyl)Phenyl Ethanol

采用气相色谱法测定合成R-3，5-（三氟二甲基）苯乙醇的反应液中的相关物质，即3，5-（三氟二甲基）苯乙酮和左及右旋3，5-（三氟二甲基）苯乙醇。采用cp—chirasil—DexCB手性毛细管色谱柱（25m×0．25mm，0．25μm），在100℃～140℃温度区间用程序升温方式进行分离，气相色谱分析中，用火焰离子化检测。以对氟苯乙酮为内标物，3种相关物质的Ai／As比值与其相关质量浓度在一定的范围内呈线性关系，检出限（3S／N）在0．1～0．2mg·L-1之间。用标准加入法测得3种相关物质的回收率在94．2％～104％之间，测定值的相对标准偏差（n=7）在2．1％～3．5％之间。

GC was applied to the determination of related substances, i. e. , 3,5-（trifluoro-dimethyl）-aceto- phenone, R and S-3, 5-（trifluoro-dimethyl）-phenyl-ethanol, in reaction liquid of synthesis of R 3, 5-（trifluoro dimethyl） phenyl ethanol. Chiral capillary chromatographic column of cp-chirasil-Dex CB （25 m × 0. 25 mm, 0. 25 μm） was used for separation with programmed temperature elevation from 100 ℃ to 140 ℃, and FID was used in the GC-analysis. p-Fluoroacetophenone was used as internal standard. Linear relationships between values of Ai/As and mass concentration of the 3 related substances were found in definite ranges, with detection limits （3S/ N） in the range of 0.1-0.2 mg . L -1. Tests for recovery and precision were made, giving values of recovery in the ranges of 94.2%-104% and RSD＇s （n=7） in the range of 2. 1%-3.5%.