用不对称催化还原法以3′-氯-苯丙醇(CPNL)为原料制备了手性3′-氯-1-苯丙酮(CPNL),并用气相色谱法测定反应液中产品及剩留的原料的含量。选用2-甲基-苯丙醇为内标物,并用化学键合β-环糊精为固定相的手性毛细管色谱柱CP-Chirasil-Dex-CB对产品及原料进行分离。在所选条件下,不仅使CPNN与CPNL,还可使CPNL的右、左旋对映体相互有效分离。由于采有内标法,因进样不准而产生的误差得以克服,测得CPNN及(S)CPNL的检出限(3S/N)依次为13.14,18.75 mg·L-1。上述两种化合物的加标回收率依次为99.5%~101.8%及96.5%~100.4%范围内;两者测定值的相对标准偏差(n=6)分别为0.39%,0.74%(左、右旋对映体相同)。

Chiral 3′-chloro-1-phenylpropanol (CPNL) was prepared by asymmetric catalytic reduction of 3′-chloro-phenylpropanone (CPNN), and gas chromatography was applied to the determination of the product and the unreacted raw material in the reaction liquid. 2-Methyl-phenylpropanol was used as internal standard and the chiral capillary chromatographic column, CP-Chirasil-Dex CB with chemical bonded β-cyclodextrin as stantionary phase was used for separation. Both the separation of CPNN and CPNL and the separation of the enantiomorphs of (R) and (S) CPNL were carried out effectively. Errors due to in-accurate sample introductions were overcome by the use of internal standard. Values of detection limit (3S/N) for CPNN and (S) CPNL were found to be 13.14 mg·L-1 and 18.75 mg·L-1 respectively. Results of recovery tests for the 2 above mentioned compounds found by addition of standards were in the ranges of 99.5%-101.8% and 96.5%-100.4% respectively. Values of RSD′s (n=6) found were 0.39% for CPNN and 0.74% for both the (R)-and (S)-CPNL.