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Articles

Polar pesticides in food of animal origin: interlaboratory validation to evaluate method fitness-for-purpose of official control

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Pages 1345-1356 | Received 19 May 2023, Accepted 30 Aug 2023, Published online: 20 Sep 2023

Figures & data

Figure 1. Reports an LC–MS/MS chromatograms of a chicken eggs sample spiked at 0.005 mg/kg for AMPA, cyanuric acid, ethephon, fosetyl Al, glyphosate, HEPA, maleic hydrazide, N-Acetyl- glyphosate; at 0.001 mg/kg for glufosinate ammonium, MPP, and NAG for three different chromatographic columns. Raptor polar X (30x2.1 mm, 2.7 µm); Hypercarb (100x2.1 mm, 5 µm); Anionic Polar Pesticides (APP, 100x2.1 mm, 5 µm).

Figure 1. Reports an LC–MS/MS chromatograms of a chicken eggs sample spiked at 0.005 mg/kg for AMPA, cyanuric acid, ethephon, fosetyl Al, glyphosate, HEPA, maleic hydrazide, N-Acetyl- glyphosate; at 0.001 mg/kg for glufosinate ammonium, MPP, and NAG for three different chromatographic columns. Raptor polar X (30x2.1 mm, 2.7 µm); Hypercarb (100x2.1 mm, 5 µm); Anionic Polar Pesticides (APP, 100x2.1 mm, 5 µm).

Table 1. Overview of LC-MS/MS systems used by the trial participants (*column dedicated to analyse maleic hydrazyde).

Figure 2. Graphic overview of the study results: relative recovery rate (%) ± RSDR for polar pesticides in bovine fat (A), chicken egg (B) and cow milk (C). The dotted lines indicate the range of acceptability according to SANTE/11312/2021 criteria.

Figure 2. Graphic overview of the study results: relative recovery rate (%) ± RSDR for polar pesticides in bovine fat (A), chicken egg (B) and cow milk (C). The dotted lines indicate the range of acceptability according to SANTE/11312/2021 criteria.

Table 2. Method performance characteristics for all analyte/matrix. The samples were spiked at two concentration levels: equal to or lower than the MRLs (spiking level A) and at levels corresponding to 5 times the LOQs (spiking level C). For the other pesticides were no MRL in food of animal origins are already sets, the lowest level (LOQ) was set at the same concentration set for LOQ during in-house validation study (Verdini et al. Citation2023). n.i.: not included in the MRL definition. * = LOQ could be equal to MRL. Average RSDr (%) obtained in the house validation study (Verdini et al. Citation2023) were also reported **validation level used in-house validation.

Figure 3. Selected ion chromatogram of (A) bovine fat, (B) chicken egg and (C) cow milk sampled spiked with 0.25 mg kg -1 AMPA, cyanuric acid, ethephon, glyphosate, fosetyl aluminum, HEPA, maleic hydrazide and N-acetyl-glyphosate, 0.01 mg kg -1 of glufosinate ammonium, MPP, N-acetyl glufosinate (NAG) and relevant isotopically labelled internal standard (sum of quantifier and qualifier transition for each analyte - upper line, ISTD quantifier transition—lower lines) analyzed with Anionic Polar Pesticides (APP, 100x2.1 mm, 5 µm) column.

Figure 3. Selected ion chromatogram of (A) bovine fat, (B) chicken egg and (C) cow milk sampled spiked with 0.25 mg kg -1 AMPA, cyanuric acid, ethephon, glyphosate, fosetyl aluminum, HEPA, maleic hydrazide and N-acetyl-glyphosate, 0.01 mg kg -1 of glufosinate ammonium, MPP, N-acetyl glufosinate (NAG) and relevant isotopically labelled internal standard (sum of quantifier and qualifier transition for each analyte - upper line, ISTD quantifier transition—lower lines) analyzed with Anionic Polar Pesticides (APP, 100x2.1 mm, 5 µm) column.
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