Department of Pharmaceutical Analysis and Nuclear Pharmacy, Faculty of Pharmacy, Comenius University, Bratislava, Slovak Republic.
J Sep Sci. 2011 Dec;34(23):3392-8. doi: 10.1002/jssc.201100633. Epub 2011 Nov 14.
The present study illustrates the possibilities of capillary isotachophoresis (CITP) online coupled with capillary zone electrophoresis (CZE) and hyphenated with fiber-based spectrophotometric diode array detection (DAD) for the direct, highly reliable, and ultrasensitive determination of quinine (QUI) in real multicomponent ionic matrices (beverages). Here, the CITP provided an effective online sample pretreatment (preseparation and preconcentration) prior to the CZE separation. Due to the CITP sample preconcentration, a simple UV-visible absorbance spectrophotometric detection was sufficient for obtaining very low concentration limits of detection (~2.3 ng/mL). Enhanced separation selectivity due to the combination of different separation mechanisms (CITP vs. CZE) enabled to obtain a pure analyte zone, suitable for its detection and quantitation in the directly injected real samples. The spectrophotometric DAD, unlike single wavelength UV detection, enabled to characterize the purity (i.e. spectral homogeneity) of the analyte zone and preliminary data indicate structurally related compounds via characteristic spectra recorded in the interval of 200-600 nm. The proposed CITP-CZE-DAD method was characterized by favorable performance parameters (sensitivity, linearity, precision, recovery, accuracy, robustness, and selectivity) and successfully applied to the control of QUI and potential QUI impurities in commercial beverages. This method is proposed as a routine automatized method for the highly reliable quality food control.
本研究展示了毛细管等速电泳(CITP)与毛细管区带电泳(CZE)在线联用,并与基于光纤的分光光度二极管阵列检测(DAD)联用,用于直接、高可靠和超灵敏测定实际多组分离子基质(饮料)中的奎宁(QUI)的可能性。在这里,CITP 在线分离前提供了有效的样品预处理(预分离和预浓缩)。由于 CITP 样品浓缩,简单的紫外可见分光光度检测足以获得非常低的检测浓度限值(~2.3ng/mL)。由于不同分离机制(CITP 与 CZE)的结合增强了分离选择性,从而获得了纯分析物区,适合直接注入实际样品中的检测和定量。与单一波长紫外检测不同,分光光度 DAD 能够表征分析物区的纯度(即光谱均一性),并通过在 200-600nm 范围内记录的特征光谱初步表明结构相关的化合物。所提出的 CITP-CZE-DAD 方法具有良好的性能参数(灵敏度、线性、精密度、回收率、准确性、稳健性和选择性),并成功应用于商业饮料中 QUI 和潜在 QUI 杂质的控制。该方法被提议作为一种高度可靠的食品质量常规自动化方法。