Supporting dataset on the optimization and validation of a QuEChERS-based method for the determination of 218 pesticide residues in clay loam soil

Abstract

The dataset presented in this article supports "Optimization and validation of a method for the simultaneous environmental monitoring of 218 pesticide residues in clay loam soil" [1]. A method based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged & Safe) for the extraction of pesticide and some metabolites residues was developed. The quantification of the chemicals was performed by a combination of two complementary LC-MS/MS and GC-MS/MS analyses. Detailed optimization data of the QuEChERS extraction method is provided, including (1) salt combination, (2) acidification of the solvent (3) the amount of the selected acid (Formic Acid, FA) and (4) moisturization of the soil samples prior to extraction. In addition, all the validation data are presented, including the matrix effect, which was evaluated for each analyte using the recommended procedure.

Keywords: GC–MS/MS; LC-MS/MS; Matrix effect; Method optimisation; Pesticides; QuEChERS; Soils.

Fig. 1

Performance of the four extraction methods tested with respect to recovery percentage. The figure shows for each extraction method the percentage of the 218 compounds that were recovered at <60%, between 60% and 70%, between 70% and 120% (optimal according to the SANTE guide), between 120% and 130%, and >130% the theoretical level of fortification.

Fig. 2

Acid addition to solvent extraction. The figure shows the number of compounds that, from left to right, had a recovery below 60%, in the range of 60% to 70%, between 70% and 120%, from 120% to 130%, and superior to 130% when the extraction solvent was acetonitrile (orange-coloured bars), acetonitrile-1% acetic acid (brown-coloured bars) and acetonitrile-1% formic acid (dark blue-coloured bars).(For interpretation of the references to color in this figure legend, the reader is referred to the web version of this article.)

Fig. 3

Optimization of the amount of formic acid. Three concentrations of F.A. (0.5%, 1%, 2.5%) are shown for each compound. The compounds are numbered according to the relation in Table 1. Bold-dotted lines shows the recovery limits recommended by the SANTE guide as acceptable (70% and 120%). Since the same guide also permits an expanded 60–130% when the results are highly reproducible these limits are also marked with dotted lines. For clarity the graph has been divided in 8 panels.

Fig. 3

Optimization of the amount of formic acid. Three concentrations of F.A. (0.5%, 1%, 2.5%) are shown for each compound. The compounds are numbered according to the relation in Table 1. Bold-dotted lines shows the recovery limits recommended by the SANTE guide as acceptable (70% and 120%). Since the same guide also permits an expanded 60–130% when the results are highly reproducible these limits are also marked with dotted lines. For clarity the graph has been divided in 8 panels.

Fig. 3

Optimization of the amount of formic acid. Three concentrations of F.A. (0.5%, 1%, 2.5%) are shown for each compound. The compounds are numbered according to the relation in Table 1. Bold-dotted lines shows the recovery limits recommended by the SANTE guide as acceptable (70% and 120%). Since the same guide also permits an expanded 60–130% when the results are highly reproducible these limits are also marked with dotted lines. For clarity the graph has been divided in 8 panels.

Fig. 3

Optimization of the amount of formic acid. Three concentrations of F.A. (0.5%, 1%, 2.5%) are shown for each compound. The compounds are numbered according to the relation in Table 1. Bold-dotted lines shows the recovery limits recommended by the SANTE guide as acceptable (70% and 120%). Since the same guide also permits an expanded 60–130% when the results are highly reproducible these limits are also marked with dotted lines. For clarity the graph has been divided in 8 panels.

Fig. 4

Soil sample moisture effect on the recovery percentages. In Fig. 4 we show the effect of soil moistening on the recovery percentages of the 218 analytes. Various percentages of soil moisture were tested (0%, 10%, 20%, 30%, 40%, and 50% water). The compounds are numbered according to the relation in Table 1. Bold-dotted lines shows the recovery limits recommended by the SANTE guide as acceptable (70% and 120%). Since the same guide also permits an expanded 60–130% when the results are highly reproducible these limits are also marked with dotted lines. For clarity the graph has been divided in 8 panels.

Fig. 4

Soil sample moisture effect on the recovery percentages. In Fig. 4 we show the effect of soil moistening on the recovery percentages of the 218 analytes. Various percentages of soil moisture were tested (0%, 10%, 20%, 30%, 40%, and 50% water). The compounds are numbered according to the relation in Table 1. Bold-dotted lines shows the recovery limits recommended by the SANTE guide as acceptable (70% and 120%). Since the same guide also permits an expanded 60–130% when the results are highly reproducible these limits are also marked with dotted lines. For clarity the graph has been divided in 8 panels.

Fig. 4

Soil sample moisture effect on the recovery percentages. In Fig. 4 we show the effect of soil moistening on the recovery percentages of the 218 analytes. Various percentages of soil moisture were tested (0%, 10%, 20%, 30%, 40%, and 50% water). The compounds are numbered according to the relation in Table 1. Bold-dotted lines shows the recovery limits recommended by the SANTE guide as acceptable (70% and 120%). Since the same guide also permits an expanded 60–130% when the results are highly reproducible these limits are also marked with dotted lines. For clarity the graph has been divided in 8 panels.

Fig. 4

Soil sample moisture effect on the recovery percentages. In Fig. 4 we show the effect of soil moistening on the recovery percentages of the 218 analytes. Various percentages of soil moisture were tested (0%, 10%, 20%, 30%, 40%, and 50% water). The compounds are numbered according to the relation in Table 1. Bold-dotted lines shows the recovery limits recommended by the SANTE guide as acceptable (70% and 120%). Since the same guide also permits an expanded 60–130% when the results are highly reproducible these limits are also marked with dotted lines. For clarity the graph has been divided in 8 panels.

Fig. 5

Matrix effect. Bars represent the mean and SD of the recoveries of the 218 analytes (spiked soil extract quantified against a calibration curve prepared in solvent). The compounds are numbered according to the relation in Table 1. Dotted lines represent the tolerance range in which it is considered that no significant matrix effect exists. For clarity the graph has been divided in 4 panels.

Fig. 5

Matrix effect. Bars represent the mean and SD of the recoveries of the 218 analytes (spiked soil extract quantified against a calibration curve prepared in solvent). The compounds are numbered according to the relation in Table 1. Dotted lines represent the tolerance range in which it is considered that no significant matrix effect exists. For clarity the graph has been divided in 4 panels.