Research Group on Fundamental Studies in Chromatography

Description

Based on the prior research experience of María Celia García Álvarez-Coque, the activity of the FUSCHROM group began under her lead in 1992, in the Micellar liquid chromatography field, applied to drug analysis in biological fluids and to the improvement of the characteristics of chromatographic peaks in basic compounds. As a result of these researches, the group specialised in fundamental studies and chemometric developments, aimed at extracting the potential information contained in chromatographic signals and improving separations, extending its application field to other chromatographic modes. In particular, new optimisation strategies, peak models, purity tests, deconvolution methods and quantitative structure-retention relationships have been developed. In addition, numerous analytical methods for the analysis of pharmaceutical, clinical and food samples have been published. The group is currently involved in the use of secondary equilibria in liquid chromatography, development of clean analytical methods, rapid chromatography, chromatographic column characterisation, column coupling and two-dimensional separations.

The members of the group have jointly published more than 400 scientific articles, approximately half of them in journals belonging to the first quartile of the ISI Web of Knowledge, with more than 110 articles in Journal of Chromatography A. In addition, they have published 40 review articles, 25 book chapters, and three books (Micellar liquid chromatography, Chemometrics and Ionic Liquids in Analytical Chemistry: New Insights and Recent Developments, published by Marcel Dekker, Síntesis and Elsevier, respectively). The group director is part of the editorial board of the Journal of Chromatography A, Analytica Chimica Acta and Separation and Purification Reviews.

For its researches, the group has received continuous funding from several Ministries for more than 30 years. Under the direction of group members, 30 students from different countries have received their PhDs. Of these students, 8 have been awarded doctoral prizes, 3 have received Marie Curie grants from the European Community, 3 have been awarded Ramón y Cajal contracts, and 12 have been professors at various universities.

It is noteworthy the collaborations with Alain Berthod (Université de Lyon, France), Desiré Massart (Vrije Universeit Brussel, Belgium), Michael Abraham (University College London, UK), Daniel Armstrong (University of Texas, Arlington, USA), Peter Schoenmakers (van't Hoff Institute of Molecular Sciences, University of Amsterdam, The Netherlands), Elisabeth Bosch and Martí Rosés (University of Barcelona), and Benjamín Monrabal and Alberto Ortín (manufacturing company of scientific instrumentation for polyolefin characterisation, Polymer Char, Valencia).

Goals CT

Effect of secondary equilibria and temperature on selectivity, retention and peak shape in HPLC (High Performance Liquid Chromatography), and research of retention mechanisms.
HPLC column characterisation: microparticulated columns for conventional and rapid chromatography, silica-based monolithic and polymeric columns.
Fundamental studies on peak capacity and its prediction in HPLC, relationship between kinetics of interaction equilibria and efficacy.
Column coupling with different separation mechanisms in one-and two-dimensional HPLC for the analysis of complex samples.
New HPLC separation strategies and their optimisation using software development.
Analysis of complex samples by chromatographic fingerprints.

Research lines

Chromatographic column characterisation
Classical methods to characterise chromatographic columns are based on the measure of retention and the use of a selected group of compounds. The validity of these approaches is investigated and new, more reliable strategies based on retention, selectivity and peak shape are proposed.
Development of clean analytical methods
The addition of additives to the mobile phase allows the volume of organic solvent to be reduced in conventional reversed-phase HPLC. When the additive is biodegradable, a clean method (classified as Green Chemistry) is achieved. In particular, by using microemulsions, water and soap separations are developed.
Studies on interaction kinetics and its prediction in chromatographic columns
Fundamental studies are carried out to explain the shape of chromatographic peaks which continue or question historical studies by other authors on this subject. Peak models and peak prediction strategies are developed to optimise separation conditions.
Method development for the analysis of pharmaceutical, clinical and food samples
Based on the fundamental advances in HPLC made by the research group, analytical methods for several samples in the pharmaceutical, clinical and food fields are designed. Method development is accompanied by an extensive validation.
Development of rapid analytical methods
Due to the increasing number of analyses performed in laboratories, there is an interest in reducing the analysis time. For this purpose, instrumental techniques and rapid columns, as well as direct injection strategies of the analysed samples, are used.
Use of secondary equilibria in reversed-phase liquid chromatography (RPLC)
Commercially available RPLC columns do not allow the analysis of charged or highly polar compounds. A line is developed to improve chromatographic performance using secondary equilibria, with special emphasis on the addition of surfactants and ionic liquids to the mobile phase.
Study of the chromatographic behaviour of ionisable compounds
Many compounds of pharmaceutical interest have an acid-base character, therefore the nature and concentration of the dominant species depend on pH. Models of mobile phase behaviour are developed in the absence and presence of additives, and with conventional or extended pH columns.
Combination of separation mechanisms
The combination of HPLC separation mechanisms allows unreachable selectivities with individual columns to be obtained. Several strategies are proposed, including the use of parallel columns, sequential column coupling and two-dimensional HPLC.
Modelling, signal processing and optimisation in liquid chromatography
Reliable optimisation of chromatographic separation conditions requires tools that use retention and peak shape models. Diverse tools and new strategies for the analysis of complex samples are developed, which consider one to three experimental factors.