A multi-residue method for trace analysis of pesticides in soils with special emphasis on rigorous quality control.
Andrea RöschFelix E WettsteinDaniel WächterVanessa ReiningerReto G MeuliThomas D BucheliPublished in: Analytical and bioanalytical chemistry (2023)
A multi-residue trace analytical method is presented to accurately quantify 146 currently used pesticides in (agricultural) soils with varying soil properties. Pesticides were extracted using an optimized quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach and chemical analysis was carried out by liquid chromatography coupled to tandem mass spectrometry (triple quadrupole). Quantification was based on matrix-matched internal standards calibration, using 95 isotopically labeled analyte analogues. In contrast to the common approach of method validation using soils freshly spiked with analytes shortly before the extraction, our method is additionally validated via an in-house prepared partly aged soil, which contains all target pesticides and via agricultural field soils with native pesticide residues. The developed method is highly sensitive (median method limit of quantification: 0.2 ng/g), precise (e.g., median intra-day and inter-day method precision both ~ 4% based on field soils), and true ((i) quantified pesticide concentrations of the partly aged soil remained stable during 6 months, were close to the initially spiked nominal concentration of 10 ng/g, and thus can be used to review trueness in the future; (ii) median freshly spiked relative recovery: 103%; and (iii) participation in a ring trial: median z-scores close to one (good to satisfactory result)). Its application to selected Swiss (agricultural) soils revealed the presence of in total 77 different pesticides with sum concentrations up to 500 ng/g. The method is now in use for routine soil monitoring as part of the Swiss Action Plan for Risk Reduction and Sustainable Use of Plant Protection Products.
Keyphrases
- heavy metals
- risk assessment
- tandem mass spectrometry
- liquid chromatography
- gas chromatography
- human health
- ultra high performance liquid chromatography
- mass spectrometry
- simultaneous determination
- high performance liquid chromatography
- climate change
- high resolution mass spectrometry
- magnetic resonance imaging
- clinical trial
- magnetic resonance
- organic matter
- physical activity
- randomized controlled trial
- ms ms
- current status
- single cell
- quality control
- molecular dynamics simulations
- phase ii
- study protocol
- amino acid
- living cells