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1.
Environ Pollut ; 352: 124143, 2024 Jul 01.
Article in English | MEDLINE | ID: mdl-38735465

ABSTRACT

Fruits consistently hold a prominent position in healthy dietary habits. Pesticides are used to manage plant diseases, achieve sustainable production, and maintain high food standards. This study utilized a comprehensive analytical technique that involved both targeted analysis and suspect screening. Analysis was conducted using Ultra-high-performance liquid chromatography coupled with hybrid Linear Trap Quadrupole (LTQ)/Orbitrap High Resolution Mass Spectrometry (HRMS) to examine pesticide levels in fruits. The matrices chosen comprised fruit commodities that are commonly consumed in Greece, including table grapes, apples, pears, citrus fruits, and strawberries. The QuEChERS approach was effectively validated for 30 specific pesticides. According to the method acceptance criteria established by SANTE, the QuEChERS method have shown exceptional efficiency in extracting the chosen pesticides, with recovery rates ranging from 70% to 120% in three concentration levels (10, 50, 100 µg kg-1). It also exhibited outstanding linearity, with an R2 more than 0.99. The method exhibited exceptional precision, with relative standard deviations (RSDs) below 20%. Additionally, the combined measurement uncertainty (MU%) was found to be acceptable, remaining below 50% The quantification limits were below 10 µg kg-1 for the majority of the analytes, satisfying the Maximum Residue Levels (MRLs) established by the European Commission. Following targeted analysis, a dietary risk assessment was performed, revealing that both acute and chronic hazard quotients (aHQ and cHQ), along with chronic hazard index (cHI) were below 1, which indicated that the studied commodities are safe for human consumption. In addition, a suspect screening workflow was developed based on an in-house database comprising 355 pesticides commonly applied to the relevant commodities and related transformation products (TPs). Overall, through suspect screening, twenty-two additional pesticides and TPs not included in the target list were identified. Hence, this approach is anticipated to function as proactive alert system guaranteeing the long-term viability of agricultural production.


Subject(s)
Dietary Exposure , Food Contamination , Fruit , Pesticide Residues , Pesticide Residues/analysis , Fruit/chemistry , Food Contamination/analysis , Greece , Chromatography, High Pressure Liquid , Mass Spectrometry/methods , Humans
2.
Environ Res ; 251(Pt 2): 118739, 2024 Jun 15.
Article in English | MEDLINE | ID: mdl-38503377

ABSTRACT

Fish feed is essential in aquaculture fish production because, along with beneficial nutrients and components, many suspected compounds can be transferred to fish and ultimately to humans. In this context, a comprehensive analysis was conducted to monitor various pesticides and pharmaceutical compounds in aquaculture fish feed through target analysis and many other groups of chemicals via suspect screening approaches. In this study, the QuEChERS extraction method was optimized, validated, and applied to fifty-four fish feed samples collected from different production batches. This was followed by liquid chromatography-high-resolution linear ion trap/Orbitrap mass spectrometry (LC-HR-IT/Orbitrap-MS) for targeted and suspect screening purposes. In general, pesticides provided satisfactory recoveries (70-105.5 %), with quantification limits lower than 5 ng g-1, whereas pharmaceuticals displayed recoveries ranging from 70.5 to 120.2 %, with quantification limits below 25 ng g-1. In addition, the matrix effects and measurement uncertainty were assessed to provide more accurate and high-confidence results. Pirimiphos-methyl was detected and quantified in 20 of 54 fish feed samples (37 %) at concentrations <77 ng g-1. Finally, suspect screening revealed the occurrence of 10 mycotoxins (e.g., citrinin, aflatoxin G2, zearalenone, and alternariol), two pesticides excluding the target pesticides (tebuconazole and fenazaquin), perfluorooctane sulfonic acid (PFOS) in almost 2 % of the samples, and ethoxyquin (antioxidant), with 12 of its Transformation Products (TPs). Finally, suspect analysis incorporated in routine analyses have proven to have great potential for complete monitoring.


Subject(s)
Animal Feed , Food Contamination , Mass Spectrometry , Animal Feed/analysis , Food Contamination/analysis , Mass Spectrometry/methods , Animals , Pesticides/analysis , Aquaculture , Chromatography, Liquid/methods , Fishes , Water Pollutants, Chemical/analysis , Pharmaceutical Preparations/analysis , Mycotoxins/analysis
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