Automation of µ-SPE (Smart-SPE) and Liquid-Liquid Extraction Applied for the Analysis of Chemical Warfare Agents

Abstract

Existing autosamplers are frequently applied only for subjecting the samples to the instruments for injection. In our study, we have set up a TriPlusRSH autosampler mounted on a GC-FID-MS/MS system using the new Method Composer and Script Editor software to automatize all necessary sample preparation steps and subsequent injection of samples in the field of chemical disarmament. Those include but are not limited to: liquid-liquid extraction, drying steps, solvent exchange, and µ-SPE. Tedious and error prone off-line steps are eliminated. In particular, when investigating highly toxic substances like chemical warfare agents or anticancer drugs, automation can help to minimize health risks for lab personnel. The setup engaged features brand new prototype equipment, e.g., a centrifuge to assist in phase separation for liquid-liquid extraction. Efficiency and accuracy of the automated methods were carefully evaluated and proven to outperform the respective manual steps after optimization, e.g., the processing time is up to 60% faster and recovery rates are doubled. The developed workflows can easily be adapted to other sample preparation protocols, e.g., determination of octanol/water partition coefficients, and be used amongst different instruments and chromatography data handling systems.