Área de Farmacotecnia, Facultad de Química, Bioquímica y Farmacia, Universidad Nacional de San Luis, Argentina.
J Pharm Biomed Anal. 2012 Nov;70:631-5. doi: 10.1016/j.jpba.2012.06.031. Epub 2012 Jun 30.
Single-walled carbon nanotubes (SWNT) are proposed as chiral selectors for separation of carvedilol stereoisomers beginning since its racemic mixture. The novel developed FIA-methodology employs a microcolumn (mC) packed with a few milligrams of SWNT which showed to be effective in S(-) and R(+) carvedilol separation. Attending to spectral properties of analytes, molecular fluorescence was employed in the detection step. Separation of carvedilol enantiomers was achieved in less than 70s with an acceptable resolution factor of 3.16. Variables that influence the chiral separation such as pH and composition of eluent solution, sample injection volume and flow rate, activation mode of NTs and mass of the same in column have been examined in detail. At optimal operational conditions, well repeatability was achieved using the same column for more than 100 injections, putting in evidence the stability of nanomaterial and the efficacy and versatility of the proposed FIA-configuration. The new methodology was successfully applied to S(-) and R(+) carvedilol quantification in pharmaceutical preparations, resulting an attractive alternative to traditional separative methods being fast, simple, using low cost instrumentation and producing scarce waste.
单壁碳纳米管 (SWNT) 被提议作为手性选择剂,用于分离卡维地洛对映异构体,因为其外消旋混合物。所开发的新颖的流动注射分析 (FIA) 方法采用填充有几毫克 SWNT 的微柱 (mC),该微柱在 S(-) 和 R(+) 卡维地洛分离中显示出有效。考虑到分析物的光谱特性,在检测步骤中采用了分子荧光。在不到 70s 的时间内实现了卡维地洛对映异构体的分离,分辨率因子为 3.16。详细研究了影响手性分离的变量,如洗脱液的 pH 和组成、样品进样体积和流速、NTs 的激活模式以及柱中相同物质的质量。在最佳操作条件下,使用同一根柱子进行了 100 多次以上的进样,均具有良好的重现性,这表明纳米材料的稳定性以及所提出的 FIA 配置的有效性和通用性。该新方法已成功应用于药物制剂中 S(-)和 R(+)卡维地洛的定量分析,是一种快速、简单、使用低成本仪器且产生较少废物的有吸引力的替代传统分离方法。