Preparative two dimensional separations involving liquid–liquid chromatography

Léa Marlot (1) , Karine Faure (1)

1 ISA-Chromatography & Hyphenated Techniques - Chromatographie et techniques couplées

The increasing performances of analytical techniques, especially two-dimensional liquid chromatography hyphenated with highly sensitive detectors, allow discovery of new targeted compounds in highly complex samples, whether biomarkers in environmental effluents, natural metabolomes in natural products or unknown impurities in synthetic chemical process. While structural identification can usually be achieved through mass spectrometry and databases, it can be useful to confirm the potential structure via NMR analysis and/or to obtain standard reference material for quantitative purposes, incentive for the production of μg to mg of new target compounds. Hence, preparative chromatography, which was initially run for large-scale production, is now facing new challenges, with small volumes of highly complex samples to deal with. Unfortunately, one dimensional chromatographic methods exhibit limited performances when targets are minor compounds in a complex matrix. Moreover, for process intensification or limited amount of sample, it is now a priority to be able to isolate multiple components with the largest yield possible using as few purification steps as possible. With these specifications in mind, a comprehensive multidimensional chromatographic method for preparative purposes is becoming appealing. Liquid-liquid chromatography, also known as countercurrent chromatography or centrifugal partition chromatography, is a technique with a proven high loading capacity, working with multiple choice of solvent systems thus a large range of polarity and selectivity. The liquid nature of the stationary phase prevents sample denaturation, irreversible adsorption resulting in high sample recovery. All these qualities make the LLC technique highly receivable as a first dimension in a 2D strategy, whether combined with another LLC method or with a more conventional LC method. In this review, both hyphenations are investigated from an instrumentation point of view, detailing systems selection methodology and two dimensional development strategy. Preliminarily, the specific LLC instrumentation is briefly summarized in this review and the nomenclature of two dimensional separation as well as the associated criteria are clearly explained and defined.

Mots clés: 2D; LLC- HPLC; Liquid–Liquid Chromatography; two dimensional separations; LLC–LLC

Domaines: Chimie analytique

Léa Marlot, Karine Faure. Preparative two dimensional separations involving liquid–liquid chromatography. Journal of Chromatography A, 2017, 1494, pp.1-17. ⟨10.1016/j.chroma.2017.03.031⟩. ⟨hal-01515553⟩