Abstract
In this study, three parameters (sample volume, cleanup and elution step) in large volume injection online Solid Phase Extraction Liquid Chromatography with diode array detection (SPE-LC) were optimized for the determination of six pharmaceuticals in wastewater samples. Preconcentration and separation were carried out using 2 columns, Dionex Ion Pac AG14A and Acclaim Polar Advantage II. Response Surface Methodology (RSM) was employed for the optimization of cleanup step (mobile phase composition and valve switching time). The optimum conditions obtained were as follows: Sample volume of 10.0 mL and cleanup with acetonitrile and ultrapure water (5:95) for 1.0 min. The method showed good recovery (82.91-107.7%), precision (0.35-8.26%) and linearity (R2 >0.99). The limit of detection was between 3.5 and 11.7 μg L-1. The proposed method is rapid, simple and sensitive for trace analysis of pharmaceuticals in water samples.
Highlights
In recent years, the occurrence of pharmaceuticals in the aquatic environment has raised concerns (Cardoso et al, 2014; Devier et al, 2013; Lindberg et al, 2014; Repice et al, 2013; Schaider et al, 2014; Vulliet and Cren-Olive, 2011)
The effect of sample loading volume on peak area pharmaceuticals was studied by evaluating 1.0, 5.0 and 10.0 mL of spiked ultrapure water.The peak area of analytes increases with increasing sample volume, increasing the sensitivity of the method (Fig. 2)
A sample volume of 10 mL was selected for subsequent optimization study
Summary
The occurrence of pharmaceuticals in the aquatic environment has raised concerns (Cardoso et al, 2014; Devier et al, 2013; Lindberg et al, 2014; Repice et al, 2013; Schaider et al, 2014; Vulliet and Cren-Olive, 2011). Solid phase extraction is the most used method for extraction of pharmaceuticals in water samples. Switching valve time is used to perform the extraction and separation in online SPE-LC. The method used four major steps: Sample loading, cleanup, elution and LC separation.
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