Analytical methods for the routinely evaluation of pesticide residues in lemon fruits and by products

Abstract

Citrus fruits and their by-products such as concentrated juices and essential oils are important intermediate by-products in the food industry that can selectively accumulate plant protection agrochemicals employed in their production. They are very difficult matrices for pesticide residue analysis due their high number and concentration of phytochemicals that could hamper the determinations. The fruit processing leads to the concentration/dilution or elimination of some of these natural products that change totally the nature of the matrix where the pesticides partition unevenly. Looking at the industrial process of the fruit, a unified vision for the pesticide residues analysis throughout the lemon fruit chain production, useful for the routine analysis of the above mentioned three matrices is presented. The driven concept is the minimization of matrix effects through sample dilution of the concentrated by-products, either after sample treatment or not. This approach will contribute to the maintenance of the whole instrumental system. QuEChERS AOAC 2007.01 was selected as the most suitable protocol for routine determination of, residues of 16 the pesticides most commonly used in the fruits during the citrus production through liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The same protocol was applied for pesticide residue analysis in concentrated juice after diluting 4 times the sample to minimize the matrix effects. For the analysis of lemon essential oils, the dilution and shoot procedure proved to be useful for LC-MS/MS and gas chromatography-mass spectrometry determination. The three methodologies were validated following SANTE guidelines, with quantitation limits below the established European Union and Codex Alimentarius maximum residue limits. The developed methodologies are useful tools for the routine control analysis of pesticide residues in lemon matrices, allowing high sample throughput and enhancing labs productivity.

Challenges in the Application of Circular Economy Models to Agricultural By-Products: Pesticides in Spain as a Case Study

“…Molecules present at very low levels would require the use of high volumes of by-products, which would imply the accumulation of pesticides. Previously published works have determined the presence of pesticides in by-products derived from processing olives, coffee, oranges, lemons, strawberries, soybeans or cow peas using analytical techniques [ 128 , 129 , 130 , 131 , 132 , 133 ]. Each study used a different weight of biomass and volume of solvent, in addition to using very variable kinds of solvents.…”

“…Each study used a different weight of biomass and volume of solvent, in addition to using very variable kinds of solvents. The studies that used lower biomass weights (50 mg or 10 g) did not detect pesticides or they were detected below the MRL [ 128 , 130 ]. The studies that used higher biomass weights (25 g, 500 g or 1 kg) found pesticides above the MRL [ 129 , 131 , 132 ].…”

Limonun evde işlenmesi sırasında bazı insektisitlerin kalıntılarının değerlendirilmesi

“…There are some reported studies in literature dedicated to analysis of pesticide residue level in the lemon fruit and lemon products. Based on those studies, registered insecticides including abamectin and buprofezin and non-registered insecticide residues were reported in lemon fruits (Andrascikova & Hrouzkova, 2013;Bakirci et al, 2014;Cicero et al, 2015;Dincay & Civelek, 2017;Besil et al, 2019;Chen et al, 2021;Aslantas et al, 2023;Karaagaçlı, 2023). Moreover, the number of Rapid Alert System for Food and Feed (RASFF) notifications in 2021 for Turkey which was the most reported origin, increased from 191 to 361.…”

Surveillance and Dietary Risk Assessment of Endocrine Disrupting Pesticides in Brinjal and Cauliflowers

“…Few studies have reported the residues of different pesticides in these vegetables (Chen et al, 2012;Ali et al, 2019).Consumption of these contaminated vegetables can be hazardous to one's health (Chen et al, 2012), and dietary exposure assessments should be included in routine annual monitoring programs. Different vegetables have different phytochemicals which may possess physicochemical properties similar to targeted pesticides which results in falsepositive results in chromatographic instruments (Besil et al, 2019). Moreover, these phytochemicals may contaminate the sensitive instruments and reduce the selectivity of the analytical method.…”

“…Moreover, these phytochemicals may contaminate the sensitive instruments and reduce the selectivity of the analytical method. Thus for robust and precise quantitation of multiple pesticides, the standard analytical method should be validated for each food commodity before analysis (Besil et al, 2019;SANTE, 2019).…”