Bunton B M, Walker T A
Pharmaceutical and Analytical Sciences, Marion Merrell Dow Inc., Kansas City, MO 64134, USA.
J Chromatogr A. 1995 May 5;699(1-2):389-94. doi: 10.1016/0021-9673(95)00088-5.
The enantiomeric separation of MDL 73,005EF (racemic mixture of two enantiomers) has been accomplished using a Chiral AGP (alpha 1-acid glycoprotein) column. The enantiomers are baseline resolved with a runtime of less than 10 min. This separation is used to quantitate the enantiomers present in bulk drug samples, tabletted formulations, and drug used in pharmacological and toxicological studies. Variables found to have an effect on the enantiomeric separation were studied and include: mobile phase ionic strength, type and concentration of organic modifier added to the mobile phase, mobile phase, mobile phase pH, column temperature and the amount of analyte injected. The enantiomeric separation was optimized on the Chiral AGP column based on the effects that each variable had on the separation. Calibration curves for a standard were linear over a range of 0.24 to 61.2 micrograms/g with a correlation coefficient of better than 0.999. A detection limit of 0.012 micrograms/g and a quantitation limit of 0.24 micrograms/g were also found.
已使用手性AGP（α1-酸性糖蛋白）柱完成了MDL 73,005EF（两种对映体的外消旋混合物）的对映体分离。对映体在不到10分钟的运行时间内实现基线分离。这种分离方法用于定量原料药样品、片剂制剂以及药理和毒理学研究中使用的药物中的对映体。研究了发现对对映体分离有影响的变量，包括：流动相离子强度、添加到流动相中的有机改性剂的类型和浓度、流动相、流动相pH值、柱温以及进样分析物的量。根据每个变量对分离的影响，在手性AGP柱上对映体分离进行了优化。标准品的校准曲线在0.24至61.2微克/克范围内呈线性，相关系数优于0.999。还发现检测限为0.012微克/克，定量限为0.24微克/克。
