Multi-residue enantioselective determination of emerging drug contaminants in seawater by solid phase extraction and liquid chromatography-tandem mass spectrometry?

Analytical MethodsANAL METHODS-UK Pub Date: 2020-05-15 DOI: 10.1039/D0AY00801J

Abstract

This study proposes a new multi-residue enantioselective method for the determination of emerging drug contaminants in sea water by solid phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). To achieve satisfactory enantiomeric separation with a vancomycin stationary phase it was essential to limit sodium chloride in extracted samples to <1 μg per injection. This was achieved through a straightforward SPE method using a 50 mL water wash volume and analyte elution in acetonitrile. A Chiral-V enantioselective column (150 × 2.1 mm; 2.7 μm particle size) operated in polar ionic mode enabled simultaneous drug separations in 30 minutes. Analytes with enantioresolution ≥1 were the stimulants amphetamine and methamphetamine, the beta-agonist salbutamol, the beta-blockers propranolol, sotalol and acebutolol, the anti-depressants fluoxetine, venlafaxine, desmethylvenlafaxine and citalopram, and the antihistamine chlorpheniramine. Method quantitation limits were <10 ng L?1 and method trueness was 80–110% for most analytes. The method was applied to samples from the Forth and Clyde estuaries, Scotland. Chiral drugs were present at concentrations in the range 4–159 ng L?1 and several were in non-racemic form (enantiomeric fraction ≠ 0.50) demonstrating enantiomer enrichment. This emphasises the need for further enantiospecific drug exposure and effect studies in the marine environment.

Graphical abstract: Multi-residue enantioselective determination of emerging drug contaminants in seawater by solid phase extraction and liquid chromatography-tandem mass spectrometry
Recommended Literature