Abstract
Sample preparation is often reported as the main bottleneck of analytical processes. To meet the requirements of both high-throughput and high sensitivity, improved sample-preparation methods capable of fast analyte preconcentration are urgently needed. To this end, a new three-phase electroextraction (EE) method is presented that allows for ultrafast electroextraction hyphenated to flow-injection analysis mass spectrometry (FIA-MS). Four model compounds, i.e., propranolol, amitriptyline, bupivacaine, and oxeladin, were used to optimize and evaluate the method. Within only 30 s extraction time, enrichment factors (EF) of 105–569 and extraction recoveries (ER) of 10.2%–55.7% were achieved for these analytes, with limits of detection (LODs) ranging from 0.36 to 3.21 ng mL−1, good linear response function (R2 > 0.99), low relative standard deviation (0.6%–17.8%) and acceptable accuracy (73–112%). Finally, the optimized three-phase EE method was successfully applied to human urine and plasma samples. Our three-phase electroextraction method is simple to construct and offers ultrafast, online extraction of trace amounts of analytes from biological samples, and therefore has great potential for high-throughput analysis.
Highlights
Matrix-assisted laser desorption/ionization, multi-dimensional liquid chromatography, ultra-performance liquid chromatography, and capillary electrophoresisemass spectrometry
The voltage was disconnected, the acceptor droplet was aspirated into the fused silica capillary, and the Eppendorf tube was replaced manually with a vial with the same solvent as the acceptor phase, and the droplet was further aspirated into the 1 mL sample loop, after which the valve was switched to the inject position (Fig. 1C, position 2)
The extraction time can be as short as 30 s while achieving enrichment factors of 105e569 and LODs of 360 pg/mL
Summary
Matrix-assisted laser desorption/ionization, multi-dimensional liquid chromatography, ultra-performance liquid chromatography, and capillary electrophoresisemass spectrometry. Contemporary sample-preparation methods often still form a bottleneck for the entire analytical workflow [1e6] This is especially the case for high-throughput and low concentration level analysis [7e10] as they are time- and labor-intensive [1,11e13] and offer relatively low enrichment [14]. Liquid-liquid extraction (LLE) is one of the most commonly-used sample preparation techniques [17], and solid-phase extraction (SPE) has been increasingly used in recent decades [4,18] Both techniques are time consuming, and use large volumes of toxic solvent [7]. The solvent type and composition of the organic phase, the composition of the acceptor phase and the aqueous sample, and the extraction voltage and time were optimized for four commonly used model compounds, i.e., propranolol, amitriptyline, bupivacaine, and oxeladin. Human urine samples (pooled from healthy donors) and EDTA-treated plasma samples (Sanquin, Leiden, The Netherlands) were kept frozen at À80 C until analysis and were thawed at room temperature directly before use
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