A multi-residue method for the determination of pesticides in high water content matrices by gas chromatography–single quadrupole mass spectrometry with electron ionisation (EI-GC/MS)

Abstract

An EI-GC/MS method for the determination of pesticide residues in vegetable matrices with high water content was validated using papaya samples. The validation of a multi-residue pesticide method was in agreement with national and international regulations enabling the Ministry of the Agriculture, Livestock and Food Supply of Brazil to cover a large number of matrices and pesticide residues in its monitoring and control programmes. The extraction used 60 mL of ethyl acetate and 30 g of sample previously processed. After extraction, clean-up of all the extracts was carried out by percolation through GBC cartridges. The samples were then injected in an EI-GC/MS system. Calibration curves were prepared in quadruplet by fortifying blank extracts with a standard solution containing all the pesticides studied at 0.000, 0.005, 0.010, 0.020, 0.030, 0.050, 0.080 and 0.100 mg kg(-1). For the recovery study, blank samples were fortified at 0.010, 0.020, 0.030, 0.050 and 0.080 mg kg(-1) and then submitted to the extraction procedure. The complete procedure was repeated over four different days by two analysts. The regression parameters of calibration curves were calculated for each validation day. Linearity, selectivity, specificity, robustness, limits of detection and quantification were also assessed. The uncertainty was estimated for each analyte at each spike level studied. The method had recoveries between 91% and 105% and precision results ≤ 20%. Limits of quantification were below or equal to the maximum residue limits (MRLs) regulated by Brazilian legislation. The MRLs of the selected pesticides are not regulated by CODEX Alimentarius. The results are also in agreement with SANCO/10684/2009.

Detection of pesticides in environmental and food matrix: A review

“…Due to their sensitivity, detectors like electron flame photometric detector (FPD), 47 capturing detector (ECD), 48 mass selective detector (MSD), and nitrogen phosphorus detector (NPD) are used. 48 In addition, mass spectrometry are also used to improve sensitivity of detection which are equipped with analyzers such as Quadrupole, 49 ion trap (IT), 50 time of flight mass analyzer (TOF), 51 triple quadrupole (QqQ). 52 Further, to decrease interference of matrix or effect of matrix on analysis selective ion monitoring (SIM) 53 or multiple reaction monitoring (MRM) 54 are used, and mass to charge ratio (m/e) of analyte are focused to achieve a lower limit of detection and quantification with less interference.…”

Recent Developments in Clean up Techniques of Pesticide Residue Analysis for Toxicology Study: A Critical Review

“…The elution solvent is pumped through the column at a constant flow rate of 2.0 ml min -1 . A 5.0 ml of the clean-up eluate are collected in a 250 ml round bottomed flask [15]. The solvent is evaporated to 5.0 ml and 1.0 μg of the concentrated eluate is injected into the gas chromatograph for determination.…”

Pesticide Residues in Honey from Stingless Bee Melipona Subnitida (Meliponini, Apidae)

“…Pesticides are widely used to protect agricultural plantations from pests, and thus improve crop production. However, inappropriate use may result in residues in human foods such as vegetables (Madureira et al, 2012), fruits (Oliveira et al, 2012), meat (Oliveira et al, 2018), fish (Oliveira et al, 2015), eggs (Hildmann et al, 2015), milk (Oliveira et al, 2014) and honey from the honeybee Apis mellifera (Pacífico da Silva et al, 2015). People consuming these contaminated foods are thus inadvertently exposed to residual pesticides, which increase the occurrence of such toxic effects as carcinogenesis, immunologic disorders and neurological disturbances (Kotsonis & Burdock, 2013).…”