Semi-Preparative Online SFE-SFC for Solid-State Injection and Purification

User Benefits

- High throughput and low co-solvent consumption due to the use of subcritical carbon dioxide as the extraction fluid and mobile phase. - Simplified sample preparation enable by the use of the extraction oven as “solid-state autosampler”. - Fast and efficient injection and purification of target compounds, even at the gram scale.

Introduction

Preparative (prep.) supercritical fluid chromatography (SFC) offers significant advantages over prep. liquid chromatography (LC), particularly in terms of efficiency and sustainability. SFC employs pressurized CO₂ as the main mobile phase component, reducing solvent consumption and enabling faster separations due to its lower viscosity and higher diffusivity. Since the mobile phase is in a sub/supercritical state, samples cannot be dissolved in it as in liquid chromatography, often causing peak distortion or precipitation. Despite these challenges, liquid injection remains predominant, with solvent selection and injection volume playing a crucial roles in maintaining peak integrity. As an alternative, a supercritical fluid extraction (SFE) oven can be used as “solid-state autosampler”. Using the Nexera UC Prep in semi-prep online SFE-SFC configuration, "solid-state injection“ was performed. In this method, the sample dissolves in the extraction fluid before being transferred to the SFC part of the system, reducing polarity mismatches and minimizing precipitation risks. In this study, we evaluated key parameters impacting sample loading, including the methanol (MeOH) ratio during extraction and the duration of both static (SE) and dynamic extraction (DE). The optimized method was then applied to a few grams sample, to confirm upscaling possibility. This work is based on the original article published in Journal of Chromatography Open.

June 3, 2025 GMT