Development and Optimisation of a Multiresidue Method for the Determination of 40 Anthelmintic Compounds in Environmental Water Samples by Solid Phase Extraction (SPE) with LC-MS/MS Detection

Abstract

A comprehensive multiresidue method was developed and validated for the determination of 40 anthelmintic compounds, including 13 transformation products, in surface and groundwater samples at sub nanogram per litre (ng L−1) levels. Anthelmintic residues were extracted from unfiltered water samples using polymeric divinylbenzene solid phase extraction (SPE) cartridges, and eluted with methanol: acetone (50:50, v/v). Purified extracts were concentrated, filtered and injected for UHPLC-MS/MS determination. The method recovery (at a concentration representative of realistic expected environmental water levels based on literature review) ranged from 83–113%. The method was validated, at three concentration levels, in accordance to Commission Decision 2002/657/EC and SANTE/11813/2017 guidelines. Trueness and precision, under within-laboratory reproducibility conditions, ranged from 88–114% and 1.1–19.4%, respectively. The applicability of the method was assessed in a pilot study whereby 72 different surface and groundwater samples were collected and analysed for the determination of these 40 compounds for the first time in Ireland. This is the most comprehensive method available for the investigation of the occurrence of both anthelmintic parent compounds and their transformation products in raw, unfiltered environmental waters.

Development of a single‐run liquid chromatography‐mass spectrometry analysis for the detection of 11 multiclass contaminants of emerging concern using a direct filtration method

“…In order to evaluate the method recovery, 100 μg/L of CECs was spiked into samples and analyzed with LC‐MS without any filtration procedure (positive control samples). The concentrations detected in the positive control samples were used to account for any losses caused by analyte sorption to the vial walls prior to the filtration process [16].…”

Benchmarking a decade of holistic agro-environmental studies within the Agricultural Catchments Programme

“…McGrath et al (2019) recognised that for better management of surface and groundwater, it is useful to be able to forecast pesticide residues in soils in real time and developed a new stochastic model developed to account for rainfall variability after application. For the first time, a newly developed and comprehensive analytical procedure (Mooney et al, 2019(Mooney et al, , 2020a allowed for an extensive assessment of pharmaceuticals and transformation products in Irish groundwater (Mooney et al, 2020b(Mooney et al, , 2021. The occurrence of anti-coccidial veterinary drugs, mainly from poultry activity, was found to be the contaminant of concern for groundwater (Mooney et al, 2021).…”

Optimization and validation of high‐performance liquid chromatography using modified QuEChERS to determine anthelmintic drugs in mutton

“…Liquid chromatography (LC) combined with other discovery systems, such as UV or diode array, fluorescence or mass spectrometry (MS), is considered the best technique to quantify multiresidues of veterinary drugs (Chicoine et al, 2020). However, many methods used for the quantification of anthelmintic drug residues in animal‐derived foods, such as high‐performance liquid chromatography with ultraviolet (HPLC‐UV) spectroscopy (Cirkovic et al, 2015; Gili et al, 2014), ultra‐high‐pressure liquid chromatography (UHPLC) with different types of detector depending on the nature of the analytes (da Silva et al, 2017; Del Bianchi A. Cruz et al, 2018), micellar LC (Pawar et al, 2021), capillary zone electrophoresis tandem mass spectrometry (MS/MS) (Tejada‐Casado et al, 2018), and recently LC–MS/MS, have been considered as advanced systematic techniques to quantify anthelmintic drugs in various animal‐based foodstuffs (Baralla et al, 2020; Casey et al, 2021; Mooney et al, 2019; Yoo et al, 2021).…”