In general, chromatographic analysis of chiral compounds involves a minimum of two methods; a primary achiral method for assay and impurity analysis and a secondary chiral method for assessing chiral purity. Achiral method resolves main enantiomeric pairs of component from potential impurities and degradation products and chiral method resolves enantiomeric pairs of the main component and diastereomer pairs. Reversed-phase chromatographic methods are preferred for assay and impurity analysis (high efficiency and selectivity) whereas chiral separation is performed by reverse phase, normal phase, or polar organic mode. In this work, we have demonstrated the use of heart-cutting (LC-LC) and comprehensive two-dimensional liquid chromatography (LC × LC) in simultaneous, sequential achiral and chiral analysis and quantitation of minor, undesired enantiomer in the presence of major, desired enantiomer using phenylalanine as an example. The results were comparable between LC-LC and LC × LC with former offering better sensitivity and accuracy. The quantitation range was over three orders of magnitude with undesired D-phenylalanine detected at approximately 0.3% in the presence of predominant, desired L-phenylalanine (99.7%). The limit of quantitation was comparable to conventional high-performance liquid chromatography. A reversed-phase C18 achiral column in the primary and reversed-phase Chirobiotic Tag chiral column in the secondary dimension were used with a compatible mobile phase.
A sensitive analytical method using mixed mode HPLC separation coupled with charged aerosol detection (CAD) was developed for quantitative analysis of lithium. The method is capable of separating lithium ion from different drug matrices and other ions in a single run thus eliminating the organic matrix and ionic analyte interferences without extensive sample preparation such as derivatization and extraction. The separation space and chromatographic conditions are defined by systematic studies of the retention behaviors of lithium and potential interfering ions and different type of pharmaceutical APIs (active pharmaceutical ingredients) under reversed-phase, HILIC and cation/anion exchange mechanisms. Compared to other current analytical techniques for lithium analysis, the presented method provides a new approach and demonstrates high sensitivity (0.02ng for LOD and 0.08ng for LOQ in both standard and sample solution). The method has been validated for pharmaceutical samples and can be potentially applied to biological, food and environmental samples.
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