Shimadzu SFC User Meeting 2024

5:00pm – Welcome

5:30pm – Exploring solubility in supercritical fluids, Caroline West, Full Professor in analytical chemistry in the Institute of Organic and Analytical Chemistry (ICOA) at the University of Orléans (France)

Solubility in supercritical fluids remains poorly understood to date, especially as it was measured for only a small number of organic molecules and in conditions that are often limited to neat CO2. In addition, current methods to measure solubility are rather long and costly, requiring large quantity of the target molecule. However, measuring and understanding solubility is significant to improving SFE and SFC processes, especially when large-scale extraction or purification is desired. Different fluid compositions need to be explored comprising scCO2 and a co-solvent, and different conditions of temperature and pressure.

In this presentation, we will describe different methods we have explored to determine solubility in supercritical fluids. Firstly, we have examined theoretical methods based on (i) quantum chemistry-based equilibrium thermodynamics with COSMO-RS method and (ii) molecular dynamic simulation. The difficulty here mostly resides in the definition of in silico parameters that would best mimic experimental conditions. Secondly, we have investigated an extraction-collection method where the target compound is placed in an extraction cell and extracted with supercritical fluid, then collected with a fraction collector. The fractions retrieved are then analyzed to quantify the amount extracted in different conditions. Finally, chromatographic methods in supercritical fluid chromatography (SFC) were also examined to determine optimal solubility when the fluid composition varies. This will be illustrated with example molecules like phthalates, carotenes and polynuclear aromatic hydrocarbons.

Caroline West is a full professor in analytical chemistry at the University of Orleans, France, where she is teaching separation science and chemometrics. Her main scientific interests lie in fundamentals of chromatographic selectivity, both in the achiral and chiral modes mainly in SFC, but also in HPLC. She is also applying these methods, with or without hyphenation to extraction methods and/or mass spectrometry, to samples of pharmaceutical interest, and natural products. She has authored more than 100 papers in international peer‐reviewed journals and has presented about 100 lectures in national and international conferences and seminars. In 2015, she received the “LC‐GC Emerging Leader in Chromatography” award from LC‐GC North America and was ranked several times among the most influential people in analytical chemistry by “The Analytical Scientist” magazine (“Top 40 under 40” 2014 & 2018, “The Power List” 2019, 2020 & 2021). More recently, she was the recipient of the Jubilee medal from the Chromatographic Society (2021). She is also an advisory board member for several journals in separation science (LC‐GC North America, Journal of Chromatography A, Journal of Pharmaceutical and Biomedical Analysis, Journal of Separation Science, Chromatographia…)

6:00pm – Achiral SFC: Considerations for method screening, Jim Bradow, Lab Head-Expert Singleton Purification at Pfizer (Groton, CT)

In discovery chemistry, the diversity of compounds that are submitted can create unknown challenges for method development and purification of the submitted batches. Building an achiral SFC screening panel that will allow for a wide range of compound types, purity profiles, and the ability to scale-up for purification is critical. Over the last decade, many ligands and co-solvents have been developed to aid in the creation of a screening panel that is amenable to a wide range of compounds, most of which are beyond typical drug like properties. This discussion will focus on our current screening panel, and what steps we take to adapt to new compound challenges.

Jim Bradow is Principal Scientist with Pfizer for the past 25 years, leading the Expert Singleton Purification Group in Groton, CT. While his focus has always been with analytical chemistry, for the past 15 years he has built a strong foundation around purification of crude materials to support early-stage discovery chemistry. Graduating from Wayne State University in Detroit, MI, he did his undergraduate research with Dr. Collin Poole researching the solvation parameter model for RPLC stationary phases.