In agriculture, pesticides are substances widely used to protect food crops from pests and diseases, forestry, and horticulture. In particular, the use of these contaminants for food products such as fresh fruit, especially bananas, has improved their quality standards. One of the most imported fruits in Italy are bananas, imported both from Europe, such as Spain, and from outside Europe, such as Ecuador, Colombia and Costa Rica. The determination of these contaminants is essential for the safety of this imported products, as pesticides are widely used in banana cultivation, even in those labelled as organic. In the last decades, the pesticide European legislation was continuously revised, leading to a constant update of maximum residue levels (MRLs), related to the toxicity of these residues and the consumption of potentially contaminated food products. In this work, the extraction and clean-up of pesticides from banana samples were carried out by means of a simple and high-throughput targeted method based on the QuEChERS procedure of the EN 15662 [1].
Thus, ultra-high-performance liquid chromatography with quadrupole electrospray ionization Orbitrap high-resolution mass spectrometry (UHPLC/ESI Q-Orbitrap MS) was used as a tool to analyze and identify over 300 pesticides, including carbamates, thiocarbamates, neonicotinoids, organophosphorus, organochlorines, phenylpyrazoles, and pyrethroids. Matrix effect (ME) can condition the analytical response and the method sensitivity, hence ME was evaluated by the slopes of two different types of calibration curve, i.e. solvent-matched calibration (SMC) and matrix-matched calibration (MMC) [2]. For each pesticide, SMC and MMC curves showed correlation coefficients ≥0.999 and over 85% of pesticides had shown ME values outside the ±20% range, therefore the quantification was performed using MMC curves. The method, LC coupled to tandem mass spectrometry, resulted to be specific, sensitive, with a detection limits from 0.503 to 12.0 µg/Kg and a quantification limits from 1.05 to 38.42 µg/Kg. The recovery values ranged between 70 and 120%, with relative standard deviations below 20%. The analytical performance of this method may be suitable for ensuring the safety and quality of fruit products, such as bananas, confirming its usefulness in a regular pesticide residue monitoring program.
European Committee for Standardization (CEN) Standard Method EN 15662:2019
De O. Gomes H, C. Menezes JM, et al., Ecotoxicology and Environmental Safety, 189 (2020), 110016. DOI: 10.1016/j.ecoenv.2019.110016