丙烯酮醇和丙烯酮乙酸酯对映体分析的气相方法研究

 建立了基于手性毛细管柱直接测定丙烯酮醇和丙烯酮乙酸酯对映体含量的气相法。采用HP 5 890气相仪 ,以WCOTCD Chiral DEXCB(30m× 0 2 5mmi d )为柱 ,在 14 8℃柱温、3 7mL/min载气 (N2 )流量下 ,两对对映体均可达到接近基线分离。用内标法对样品进行测定 ,线性 (相关系数 0 996 5～ 0 9985 )和重复性(RSD :1 0 8%～ 1 2 5 % )均很好。采用该方法测定丙烯酮醇转化为R 丙烯酮乙酸酯过程中反应物及其产物的对映体含量 ,并跟踪分析酶的活性和评价酶的拆分反应的选择性 ,结果令人满意。

Development of Gas Chromatographic Method for Chiral Analysis of Acrylic Ketone Alcohol and Acrylic Ketone Acetate

A gas chromatographic method was developed to directly determine the enantiomers of acrylic ketone alcohol and acrylic ketone acetate. Two pairs of enantiomers were nearly baseline-separated by using Model HP-5890 Gas Chromatograph with flame ionization detector and WCOT CD-Chiral-DEX CB (30 m x 0.25 mm i.d.) column. The optimum conditions were the split ratio of 30:1 for the sample injected, the flow rates of 3.7 mL/min for the carrier gas (nitrogen), 60 mL/min for the hydrogen, and 250 mL/min for the oxygen, and temperatures of 148 degrees C for the column, 230 degrees C for the injector, and 230 degrees C for the detector. The linearity and reproducibility were satisfactory. The regression coefficients were over 0.9965. The RSDs obtained were less than 1.25%. The method was further used to trace the reactants and products, and to evaluate the enzyme catalyst activity and selectivity under different conditions. The results show that the method developed is very successful.