摘要
建立了一种用高效液相色谱(HPLC)测定扁桃酸光学纯度的新方法。用苯胺将扁桃酸衍生化,产生相应的对映体衍生物,正己烷为流动相,乙醇和异丙醇作极性调节,用DNB-Leucine色谱柱进行分离。考察了流动相组成和柱温对其分离的影响,确定分析条件为:流动相为V(正己烷)∶V(乙醇)=85∶15,温度20℃,流速1.5 mL/min。在此条件下拆分扁桃酸衍生物对映体,达到基线分离,分析时间在7 min以内,分离因子达到1.62。与旋光仪方法的测定结果一致,两种方法测定的光学纯度偏差不超过1.96%。该方法可以准确、方便地测定扁桃酸的光学纯度。
A novel and accurate HPLC method was developed for the determination of optical purity of mandelic acid （MA） enantiomers. The MA enantiomers were first derivatised with aniline into their corresponding derivatives which were then separated on a DNB - Leucine column using a mixture of hexane and ethanol as the mobile phase（ Vhexane： Vethanol = 85 ： 15） at a flow rate of 1.5 mL/min and detected at A254 nm and at 20℃. The separation of the derivatives was obtained in less than 7 rain with a separation factor of more than 1.62. The optical purity results obtained agreed quite well with those obtained by the traditional polarimetric method. The relative deviation was less than 1.96% indicating that the proposed method could be used for the determination of MA optical purity accurately.
出处
《分析测试学报》
CAS
CSCD
北大核心
2007年第6期895-897,共3页
Journal of Instrumental Analysis
基金
四川省应用基础研究资助项目(04JY029-083-3)
关键词
高效液相色谱
扁桃酸
衍生化
手性拆分
手性固定相
光学纯度
high performance liquid chromatography
mandelic acid
derivatization
chiral separation
chiral stationary phase
optical purity
