Dynamic headspace solid-phase extraction at room temperature: a theoretical model, method, and application for propofol analysis

Abstract

Herein, a simple dynamic headspace solid-phase extraction (DHS-SPE) process at room temperature was used for a material that is sensitive to increase in the temperature. A proposed method was implemented to rapidly extract propofol (PF) from a complex matrix before fluorescence spectroscopy analysis, within a short sampling time without involving a hot plate or stirrer. A mini diaphragm pump was used to circulate the headspace gas. As the headspace gas flows over the sample solution surface, bubbles form and release analytes from the liquid into the headspace. During the extraction process, the headspace gas passes through the coated metal foam as a sorbent that is placed in a homemade glass vessel and analytes are trapped from the gas phase. A theoretical model of DHS-SPE based on the consecutive first-order process is proposed in this study. A mathematical solution for the dynamic process of mass transfer was obtained by correlating the variation in analyte concentration in the headspace and adsorber with the pump speed and amount of analyte extracted to the solid phase. Using electrochemically Nafion-doped polypyrrole (PPy-Naf) film on nickel foam as the solid-phase coupled to fluorescence detection, a linear dynamic range over the concentration range of 100–500 nM with a detection limit of 15 nM was obtained. This method was applied successfully for PF determination in human serum sample matrices without the interference of co-administered drugs, such as cisatracurium, which have significant emission spectrum overlap. The developed method can lead to a new idea for sample pretreatment, which is compatible with many analytical techniques and has been successfully combined with fluorescence spectroscopy in this work. This format of sampling simplifies the transfer of analytes from complex matrices to the headspace for the extraction and preconcentration process, eliminating the heating step and the need for expensive equipment.