Blessington B, Crabb N, Karkee S, Northage A
Department of Pharmaceutical Chemistry, School of Pharmacy, University of Bradford, West Yorkshire U.K.
J Chromatogr. 1989 May 19;469:183-90. doi: 10.1016/s0021-9673(01)96453-2.
The chiral analysis of a range of propionate anti-inflammatory drugs and herbicides was accomplished by gas chromatographic separation of their R-alpha-phenylethylamide diastereomeric derivatives. Using a packed column (3% OV-l on Chromosorb G) good separations were obtained but analysis times were rather long. Examination of the same crystalline derivatives using a capillary column (bonded methylsilicone) resulted in good separations together with much reduced total analysis times. The technique was validated through the analysis of several derivatives prepared on a micro scale and examined directly by gas chromatography without any crystallisation step. Racemic materials all gave virtually 50:50 response ratios while the analysis of optically pure samples produced no evidence of significant racemization. Derivatives of phenoxyacetic acid and myristic acid were also prepared and chromatographed as potential internal standards.
通过对一系列丙酸类抗炎药物和除草剂的R-α-苯乙酰胺非对映体衍生物进行气相色谱分离，完成了它们的手性分析。使用填充柱（Chromosorb G上的3% OV-1）可实现良好的分离，但分析时间较长。使用毛细管柱（键合甲基硅氧烷）对相同的结晶衍生物进行检测，分离效果良好，同时总分析时间大幅缩短。该技术通过对几种微量制备的衍生物进行分析得到验证，这些衍生物未经任何结晶步骤，直接通过气相色谱进行检测。外消旋物质的响应比几乎均为50:50，而对光学纯样品的分析未发现明显消旋化的迹象。还制备了苯氧乙酸和肉豆蔻酸的衍生物，并将其作为潜在的内标进行色谱分析。
