The LCGC Awards, Part II: Advancing the Frontiers of Separation Science

March 4, 2020

This morning session, which continues the conversations of Tuesday’s LCGC Award Symposium, focuses on new developments in analytical separations, particularly in pharmaceutical, environmental, and food and beverage analysis.

This morning session, which continues the conversations of Tuesday’s LCGC Award Symposium, focuses on new developments in analytical separations, particularly in pharmaceutical, environmental, and food and beverage analysis. The session, presided over by LCGC editorial director Laura Bush, will be held in room 184BC.

Zachary Breitbach of AbbVie Inc. will open up the discussion with a talk on online multidimensional methods for pharmaceutical analysis. In this session, the use of 2D-LC will be described as an online approach to: i) add additional resolving power for analyzing peak purity in related substances methods, ii) exchange mobile phase additives to optimize detection when volatile mobile phases are required, iii) remove non-UV absorbing, interfering drug product related excipients which suppress mass spectral detection, and iv) alleviate specificity requirements in chiral methods. 

Next, Fabrice Gritti of the Waters Corporation discusses the race towards the development of faster and still efficient high-throughput gradient liquid chromatography (HT-GLC) and how this progress is driven by the timelines of the pharmaceutical industry.

Milton Lee of Brigham Young University and Axcend LLC will then discuss portable capillary liquid chromatography, and how this method brings together the high performance of traditional high performance liquid chromatography (HPLC) with compact size and mobility to address applications for which conventional HPLC is not applicable, such as on-site analysis of plant extracts, monitoring of water pollution, rapid detection of hazardous materials, and on-line organic reaction monitoring. 

M. Farooq Wahab of The University of Texas at Arlington follows with a discussion on advances in peak processing in separation science, specifically on how to extract peak areas from overlapping and tailing peaks. Complex examples are shown using chiral chromatography for enantiomers, steroids, and twin-column recycling HPLC of IgG aggregates and deuterated benzene isotopes. Peak detection in case of severe overlap and the presence of shoulders are also demonstrated. The strengths and weaknesses of each approach are evaluated and discussed with these real examples.

After a short recess, the program continues with Kevin Schug of The University of Texas at Arlington addressing the targeting of mixtures of intact proteins using multidimensional separations and triple quadrupole mass spectrometry. Combined with high efficiency separations, this top-down quantitative approach provides good analytical performance, except that sensitivity is less than that of common bottom-up quantitative approaches. There currently exist few commercial products for the simultaneous preparation and preconcentration of multiple intact proteins characterized by variable physicochemical properties. The targeting of growth factors and cytokines will be highlighted in this context.

Leonard Sidisky of MilliporeSigma follows with a talk about the development of ionic liquid capillary columns since they were first introduced as commercial products around 10 years ago, as well as providing an update on current studies evaluating and developing new ionic liquids stationary phases and new applications with them. 

Next, Mohsen Talebi of Azyp, LLC describes and evaluates the compatibility of recently launched molecular rotational resonance (MRR) as a GC detector, and how the capabilities can surpass those of high-resolution mass spectrometry and NMR in regard of selectivity, resolution, and compound identification. 

Erik Regalado of Merck & Company, Inc. closes the session with an examination of expanding the reach of sub/supercritical fluid chromatography to biomolecules at the analytical and preparative scale. In addition to showcasing several potential SFC applications for bioanalytical testing and preparative separation of hydrophilic compounds, the work presented will illustrate analytical procedures introduced by Regaldo’s group to interrogate the global conformational structure of model peptides and proteins following purification by preparative SFC.