Direct enantioseparation of mandelic acid by high‐performance liquid chromatography using a phenyl column precoated with a small amount of cyclodextrin additive in a mobile phase
Direct enantioseparation of mandelic acid by high‐performance liquid chromatography using a phenyl column precoated with a small amount of cyclodextrin additive in a mobile phase
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使用预涂有少量环糊精添加剂的流动相的苯基柱，通过高效液相色谱法直接对映分离扁桃酸
作者：
Watanabe Yuri;Mikami Ikko;Yamamoto Atsushi;Aizawa Sen‐ichi;Taga Atsushi;Mochizuki Naoki;Ishihara Yoshimi;Kodama Shuji
采用反相色谱柱和含有少量羟丙基-β-环糊精（HP-β-CD）的移动的流动相直接分离扁桃酸对映体，是一种节省CD添加剂用量的有效方法。因此，在本发明中，提出了外消旋扁桃酸可以用苯基柱通过使用由10 mM乙酸铵缓冲液组成的移动的相来分析02%（w/v）HP-β-CD，流速为1.0 mL/min，40°C，通过10 mM乙酸铵缓冲液后（pH 4.2），含有0.1%（w/v）HP-β-CD作为预涂移动的相，柱温60 min。注入的扁桃酸可与吸附的HP-β-CD形成三元复合物。对于HPLC，D-扁桃酸的保留时间长于L-异构体，这可以从HP-β-CD与D-扁桃酸的复合物的更高稳定性来解释，这通过使用HP-β-CD作为选择剂的CE实验来证实。并与其它固定相进行了比较。
Direct enantioseparation of mandelic acid by high‐performance liquid chromatography (HPLC) with a reversed phase column and a mobile phase containing a small amount of hydroxylpropyl‐β‐cyclodextrin (HP‐β‐CD) was studied as an efficient method for saving consumption of the CD additive. As a result, it was proposed that racemic mandelic acid can be analyzed with a phenyl column by using a mobile phase composed of 10 mM ammonium acetate buffer (pH 4.2) and 0.02% (w/v) HP‐β‐CD at a flow rate of 1.0 mL/min at 40°C after the passage of 10 mM ammonium acetate buffer (pH 4.2) containing 0.1% (w/v) HP‐β‐CD as a precoating mobile phase for 60 min. It is suggested that HP‐β‐CD is bound with a phenyl group on the surface of the stationary phase to allow a phenyl column to act as a transient chiral column, and injected mandelic acid can form the ternary complex with the adsorbed HP‐β‐CD. The longer retention time of D‐mandelic acid than the L‐isomer for HPLC can be explained from the higher stability of the HP‐β‐CD complex with D‐mandelic acid, which was confirmed by CE experiment with HP‐β‐CD as a selector. The efficiency of a phenyl column compared with other stationary phases was also discussed.