A fully automated on-line preconcentration and liquid chromatography-tandem mass spectrometry method for the analysis of anti-infectives in wastewaters |
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Authors: | Segura Pedro A Gagnon Christian Sauvé Sébastien |
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Affiliation: | a Département de Chimie, Université de Montréal, C.P. 6128, Succursale Centre-Ville, Montréal, QC, Canada H3C 3J7 b Aquatic Ecosystem Protection Research Division, Environment Canada, 105 McGill Street, Montréal, QC, Canada H2Y 2E7 |
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Abstract: | We developed and validated a novel on-line preconcentration liquid chromatography-tandem mass spectrometry method for the determination of anti-infectives in wastewaters. The presented method preconcentrates 1 mL of sample in a load column using a switching-valve technique. The method was optimized with respect to sample load flow rate, volume of the load column wash and organic solvent content of the load column wash. The sample is cleaned using a 30% organic solvent washing step and then gradually eluted to an analytical column for separation. To compensate for matrix effects, quantitation was performed using standard additions. Confirmation of the presence of the detected compounds was done using a second selective reaction monitoring transition. Method intra-day precision was less than 9% and inter-day precision %R.S.D. varied between 2.5 and 23%. Limits of detection for the selected anti-infective compounds ranged from 13 to 61 ng L−1. All the target anti-infectives were found in the city of Montréal WWTP effluent in concentrations ranging from 71 to 289 ng L−1. This automated method eases the rapid quantitation of those trace contaminants using small sample volumes. |
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Keywords: | Antibiotics Antimicrobials Column-switching On-line solid-phase extraction LC/MS/MS Wastewater Automated method Pharmaceuticals in the environment |
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