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[反相高效液相色谱法拆分拉贝洛尔对映体]

[Separation of enantiomeric labetalol by reversed-phase high performance liquid chromatography].

作者信息

Zhao H, Li H, Qui Z

机构信息

Chongqing University of Medical Sciences, Chongqing, 400046.

出版信息

Se Pu. 1999 Jul;17(4):369-71.

Abstract

A reversed-phase high performance liquid chromatographic method for the separation of labetalol enantiomers was developed. In the method, 2, 3, 4, 6-tetra-O-acetyl-beta-D-glucopyranosyl isothiocyanate (GITC) was chosen as the reagent for pre-column chiral derivatization of labetalol to give four diastereomeric thiourea derivatives. These derivatives were efficiently separated on a Nova-Pak C18 column using V(MeOH):V(0.01 mol.L-1(pH 7.00) H2PO4(-)-HPO(4)2- buffer) = 51:49 as the mobile phase and detected by UV detector at a wavelength of 250 nm or fluorescence detector at lambda ex = 340 nm and lambda em = 440 nm. The effects of the pH of mobile phase on the retention and fluorescence absorbance are also discussed.

摘要

建立了一种反相高效液相色谱法用于分离拉贝洛尔对映体。该方法选用2,3,4,6-四-O-乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯(GITC)作为柱前手性衍生化试剂,使拉贝洛尔生成四种非对映体硫脲衍生物。这些衍生物在Nova-Pak C18柱上以V(甲醇):V(0.01 mol·L⁻¹(pH 7.00)磷酸二氢钠-磷酸氢二钠缓冲液)= 51:49作为流动相进行有效分离,并通过紫外检测器在250 nm波长处检测,或通过荧光检测器在激发波长λex = 340 nm和发射波长λem = 440 nm处检测。还讨论了流动相pH值对保留时间和荧光吸收的影响。

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