Zhou Meng, Stewart James T
Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens, GA 30602, USA.
J Pharm Biomed Anal. 2002 Oct 15;30(3):443-9. doi: 10.1016/s0731-7085(02)00219-4.
An enantioseparation of racemic vesamicol in human serum by capillary electrophoresis with solid phase extraction and sulfated B-cyclodextrin (S-B-CD) is presented The separation was achieved on an uncoated 72 cm x 50 microm id fused silica capillary maintained at 30 degrees C and + 15 kV applied voltage using a run buffer of 128 micro-B-CD in 50 mM phosphate buffer at pH 5. The detection wavelength was 260 nm. Bond Elut C18 solid phase extraction cartridges were used in the sample preparation of the vesamicol samples from serum. Among the CDs studied, the migration order of the enantiomers was reversed in CM-B-CD compared to S-B-CD. Increases in migration time and differences in time between enantiomers was observed with increasing concentrations of S-B-CD. Baseline separation was achieved in the 2-20 microg/ml range of enantiomer concentration (r > .996). A sample stacking technique was used to improve peak shape and LOD. LODs were 0.5 microg/ml for each enantiomer. Studies of various factors and CE conditions showed the effect of CD type, CD concentration, buffer type, buffer concentration and pH on stability and resolution.
介绍了采用固相萃取和硫酸化β-环糊精（S-β-CD）通过毛细管电泳对人血清中消旋维生霉素进行对映体分离的方法。分离是在一根未涂层的72 cm×50μm内径熔融石英毛细管上进行的，毛细管保持在30℃，施加电压为+15 kV，使用的运行缓冲液是在pH 5的50 mM磷酸盐缓冲液中含有128μMβ-环糊精。检测波长为260 nm。Bond Elut C18固相萃取柱用于从血清中制备维生霉素样品。在所研究的环糊精中，与S-β-CD相比，对映体在CM-β-CD中的迁移顺序相反。随着S-β-CD浓度的增加，观察到迁移时间增加以及对映体之间的时间差异。在对映体浓度为2 - 20μg/ml范围内实现了基线分离（r＞0.996）。采用样品堆积技术来改善峰形和检测限。每个对映体的检测限为0.5μg/ml。对各种因素和毛细管电泳条件的研究表明了环糊精类型、环糊精浓度、缓冲液类型、缓冲液浓度和pH对稳定性和分离度的影响。
