Abstract
A rugged and high throughput capillary column (cLC) LC-MS switching platform using large volume injection and on-line automatic filtration and filter back-flush (AFFL) solid phase extraction (SPE) for analysis of environmental water samples with minimal sample preparation is presented. Although narrow columns and on-line sample preparation are used in the platform, high ruggedness is achieved e.g., injection of 100 non-filtrated water samples did not result in a pressure rise/clogging of the SPE/capillary columns (inner diameter 300 μm). In addition, satisfactory retention time stability and chromatographic resolution were also features of the system. The potential of the platform for environmental water samples was demonstrated with various pharmaceutical products, which had detection limits (LOD) in the 0.05–12.5 ng/L range. Between-day and within-day repeatability of selected analytes were <20% RSD.
Highlights
If the trapped analytes are back-flushed off the solid phase extraction (SPE) column, these particles can be transferred to the analytical column, resulting in a clogged analytical column
Using the AFFL plumbing, these problems are avoided; particles are trapped by an on-line filter, while analytes are enriched on-line on an SPE column (Figure 1A) using a 10 port switching valve controlled by the LC pump, high flow loading pump (150 μL/min) and non-eluting conditions (0.1% formic acid in H2O)
The capillary column (cLC)-based system provides excellent sensitivity and ruggedness, quantification issues can arise depending on the analyte
Summary
An increasing consumption of pharmaceutical products (PPs) raises significant concerns, as their growing presence in the environment can represent a serious threat to our health and the environment (Khetan and Collins, 2007; Pailler et al, 2009; Kumar et al, 2010; Fatta-Kassinos et al, 2011; Hoff et al, 2015; Richardson and Kimura, 2016). One can modify LC-MS systems to increase sensitivity, e.g., by using very narrow LC columns (inner diameter < 0.5 mm). Columns with reduced inner diameter have less chromatographic dilution (radial) (Chervet et al, 1996; Vissers et al, 1997), allowing increased sensitivity when using concentration sensitive detectors such as electrospray ionization (ESI) MS
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