A simple and rapid analytical methodology based on liquid chromatography-tandem mass spectrometry for monitoring pesticide residues in soils from Argentina

Abstract

Rapid analytical methodology has been developed for multi-residue determination of pesticides in soils using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) with triple quadrupole analyzer. Soil samples were collected from Argentina in 12 representative agricultural areas, and 18 pesticides were selected on the basis of their use. Special attention was paid to minimize sample preparation, making easier the method application to routine analysis. Several extraction procedures were tested, performing a careful study on matrix effects. The method finally proposed (extraction with acetonitrile and subsequent 2-fold dilution with water without any clean-up step) was fully validated at 0.05 and 0.5 mg/kg on the basis on European SANCO 12571/2013 and 825/00 guidelines. The method applicability and robustness was demonstrated by analysis of quality control (QC) samples, consisting on eleven soils spiked at 0.5 mg/kg. These soil samples were collected from different experimental plots, and were very diverse in their physico-chemical characteristics. The methodology developed is of easy application, there is low consumption of solvents and reagents, and no clean-up is required despite the complexity of the soil matrix. In the near future, the method developed will be used to monitor the presence of pesticides in large agricultural areas of Argentina.

Spatial and temporal trends and flow dynamics of glyphosate and other pesticides within an agricultural watershed in Argentina

“…After 30 min, the samples were sonicated 3 times for 15 min and centrifuged at 3000 rpm for 15 min. An aliquot of 1 mL was taken from the supernatant, mixed with 1 mL of ultrapure water, and later filtered through a 0.22‐µm nylon filter and placed into a 1‐mL vial for UHPLC–MS/MS determination .…”

“…Positive findings were confirmed by calculating the peak area ratios between the Q/q and comparing them with ion ratios obtained from a reference standard. A finding was considered positive when the concentration ratio Q/q was in the range of 0.8 to 1.2 . For UHPLC analysis, Masslynx NT Ver 4.1 (Waters) software was used to process quantitative data obtained from calibration standards and from the samples.…”

Residues of currently used pesticides in soils and earthworms: A silent threat?

“…In each plot, regardless of the size of the sampled habitats (i.e., winter cereal fields, grasslands, hedgerows), three subsamples (0-5 cm depth; Amelung et al, 2007;de Geronimo et al, 2015) were taken using a 5 cm Ø soil auger. They were then combined to obtain one composite sample per site.…”

Development of a multi-residue method for 58 pesticides in soil using QuEChERS and gas chromatography-tandem mass spectrometry

“…The LOQ for each pesticide was determined as the lowest spiked concentration with 5 replicates that can be quantied with satisfactory recovery values (70-120%) and a RSD # 20%. 28,29 3 Results and discussion…”