Pharmaceutical analysis and metabolites. Coordinator: Gotti

Development, validation and application of analytical methods and separation techniques (gas chromatography, liquid chromatography and electrokinetic techniques) also hyphenated to mass spectrometry, in analysis of pharmaceuticals and related substances, bioactive compounds including proteins/peptides and metabolites.

Research themes

Electrokinetic systems based on complex pseudostationary phases. 

Improved separation selectivity in electrokinetic systems can be achieved by supplementing the electrophoretic running buffer with additives able to establish reversible interactions with the solutes to be separated. Among the additives, surfactants are very successful; they are used at concentration higher the critical micelle concentration (cmc) where a micellar pseudostationary phase is obtained. In this field the research activity has been addressed to the development of new systems based on mixed micelle (from different surfactants) such as sodium dodecyl sulfate and bile salts. Further, the role of cyclodextrins as chiral additives in electrokinetic systems has been considered. The role of the components of the pseudostationaty phases are assessed by means of the evaluation of chromatographic parameters such as selectivity, resolution, capacity factor, and efficiency; furthermore, also physico-chemical parameters such as zeta potential, ionic radius of the micelle aggregates, inclusion/complexation constants and kinetic constants can be determined to characterize the separation systems. The development of the complex systems can be advantageously supported by chemometric tools and by means of the Quality by Design approach: this part of the research activity is in collaboration with a team of the University of Florence. The proposed CE systems allowed to achieve interesting and useful methods for related substances analysis in pharmaceuticals. 

Separation techniques (HPLC, GC-MS, CE and CE-MS) in analysis of drugs and biomolecules (including metabolites) in complex real samples. 

Separation methods by techniques as GC, HPLC and CE, are developed and applied also in integrated fashion and in combination with sample prep methods as solid phase microextraction (SPME). In addition, an original approach to the CE-MS hyphenation is developing for the direct insertion of the CE effluent to the electron impact (EI) source by means of tailoring designed interfaces fabricated by 3D printing technologies.   

Lab members

Roberto Gotti 

Internship projects

Two internship slots/year 

Main publications

Hancu, G., Orlandini, S., Papp, L.A., Modroiu, A., Gotti, R., Furlanetto, S. (2021). “Application of experimental design methodologies in the enantioseparation of pharmaceuticals by capillary electrophoresis: A review”. Molecules 26: 4681. 

Fiori, J., Turroni, S., Candela, M., Brigidi, P., Gotti, R. (2018). “Simultaneous HS-SPME GC-MS determination of short chain fatty acids, trimethylamine and trimethylamine N-oxide for gut microbiota metabolic profile”. Talanta 189: 573-581.  

Fiori, J., Pasquini, B., Caprini, C., Orlandini, S., Furlanetto, S., Gotti, R. (2018). “Chiral analysis of theanine and catechin in characterization of green tea by cyclodextrin-modified micellar electrokinetic chromatography and high performance liquid chromatography”. J. Chromatogr. A 1562: 115-122.