Abstract
By using an innovative, positive pressure sample loading technique in combination with an in-line filter of finely ground sand the bottleneck of solid phase extraction (SPE) can be reduced. Recently published work by us has shown the proof of concept of the technique. In this work, emphasis is put on the SPE flow rate and method validation for 26 compounds of emerging environmental concern, mainly from the 1st and 2nd EU Watch List, with various physicochemical properties. The mean absolute recoveries in % and relative standard deviations (RSD) in % for the investigated compounds from spiked pure water samples at the three investigated flow rates of 10, 20, and 40 mL/min were 63.2% (3.2%), 66.9% (3.3%), and 69.0% (4.0%), respectively. All three flow rates produced highly repeatable results, and this allowed a flow rate increase of up to 40 mL/min for a 200 mg, 6 mL, reversed phase SPE cartridge without compromising the recoveries. This figure is more than four times the maximum flow rate recommended by manufacturers. It was indicated that some compounds, especially pronounced for the investigated macrolide molecules, might suffer when long contact times with the sample glass bottle occurs. A reduced contact time somewhat decreases this complication. A very good repeatability also held true for experiments on both spiked matrix-rich pond water (high and low concentrations) and recipient waters (river and wastewater) applying 40 mL/min. This work has shown that, for a large number of compounds of widely differing physicochemical properties, there is a generous flow rate window from 10 to 40 mL/min where sample loading can be conducted. A sample volume of 0.5 L, which at the recommended maximum flow rate speed of 10 mL/min, would previously take 50 min, can now be processed in 12 min using a flow rate of 40 mL/min. This saves 38 min per processed sample. This low-cost technology allows the sample to be transferred to the SPE-column, closer to the sample location and by the person taking the sample. This further means that only the sample cartridge would need to be sent to the laboratory, instead of the whole water sample, like today’s procedure.
Highlights
In environmental organic trace analysis, there is most often a need to enrich the compounds of interest from a large sample volume, where the use of solid phase extraction (SPE) is more or less the standard technique
In this SPE-polymer, work, we investigate the possibility of increasing the sample loading flow rate with the purpose of increasing laboratory sample throughput without compromising repeatability and
We investigate the possibility of increasing the sample loading flow rate with the robustness
Summary
In environmental organic trace analysis, there is most often a need to enrich the compounds of interest from a large sample volume, where the use of solid phase extraction (SPE) is more or less the standard technique. Extraction and clean-up protocols related to the SPE methodology commonly constitute the bottleneck of the analytical procedure and are estimated to account for 75% of the analysis time [1]. SPE-column manufacturers recommend maximum flow rates in reverse phase SPE. SPE-column manufacturers recommend maximum flow rates in reverse phase SPE (200 mg HLB, Hydrophilic Lipophilic Balanced) and 6 mL from 1 to 10 mL/min, to avoid component (200 mg HLB, Hydrophilic Lipophilic Balanced) and 6 mL from 1 to 10 mL/min, to avoid component breakthrough [2,3,4]. A sample volume of 0.5 L will take between 50 to 500 min to process such flow rates are applied. The most common commercial technique for loading samples onto possible flow-interfering matrix.
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