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万古霉素硅胶固定相在填充毛细管电色谱中的应用 I. 碱性化合物的对映体分离

Use of vancomycin silica stationary phase in packed capillary electrochromatography I. Enantiomer separation of basic compounds.

作者信息

Desiderio C, Aturki Z, Fanali S

机构信息

Istituto di Cromatografia del CNR, Monterotondo Scalo, Roma, Italy.

出版信息

Electrophoresis. 2001 Feb;22(3):535-43. doi: 10.1002/1522-2683(200102)22:3<535::AID-ELPS535>3.0.CO;2-8.

Abstract

Chiral separation of basic compounds was achieved by using 75 or 100 microm ID fused-silica capillaries packed with a vanoomycin-modified diol silica stationary phase. The capillary was firstly packed for about 12 cm with a slurry mixture composed of diolsilica (3:1) then with the vancomycin modified diol-silica (3:1) (23 cm), and finally with diol-silica (3:1) for about 2 cm. Frits were prepared by a heating wire at the two ends of the capillary; the detector window was prepared at 8.5 cm from the end of the capillary where vancomycin was not present. The influence of the mobile phase composition (pH and concentration, organic modifier type and concentration) on the velocity of the electroosmotic flow, chiral resolution and enantioselectivity was studied. Good enantiomeric resolution was achieved for atenolol, oxprenolol, propranolol, and venlafaxine using a mobile phase composition of 100 mM ammonium acetate solution (pH 6)/water/acetonitrile (5:5:90 v/v/v) while for terbutaline a mixture of 5:15:80 v/v/v provided the best separations. The use of methanol instead of acetonitrile caused a general increase of enantiomer resolution of the studied compounds together with a reduction of efficiency and detector response. However, the combination of acetonitrile and methanol in the mobile phase (as, e.g., 10% methanol and 80% acetonitrile) allowed to improve the enantiomer resolution with satisfactory detector response.

摘要

使用填充有万古霉素修饰二醇硅胶固定相的内径为75或100微米的熔融石英毛细管实现了碱性化合物的手性分离。首先用由二醇硅胶(3:1)组成的淤浆混合物将毛细管填充约12厘米,然后用万古霉素修饰的二醇硅胶(3:1)(23厘米)填充,最后用二醇硅胶(3:1)填充约2厘米。通过在毛细管两端的加热丝制备筛板;在距不存在万古霉素的毛细管末端8.5厘米处制备检测窗口。研究了流动相组成(pH和浓度、有机改性剂类型和浓度)对电渗流速度、手性拆分和对映体选择性的影响。使用100 mM醋酸铵溶液(pH 6)/水/乙腈(5:5:90 v/v/v)的流动相组成,阿替洛尔、氧烯洛尔、普萘洛尔和文拉法辛实现了良好的对映体拆分,而对于特布他林,5:15:80 v/v/v的混合物提供了最佳分离效果。使用甲醇代替乙腈导致所研究化合物的对映体拆分普遍增加,同时效率和检测器响应降低。然而,流动相中乙腈和甲醇的组合(例如10%甲醇和80%乙腈)能够在检测器响应令人满意的情况下提高对映体拆分效果。

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