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    Determination of Pesticide Residues in Vine Leaves Using the QuEChERS Method and Liquid Chromatography-Tandem Mass Spectrometry
    (Mdpi, 2024) Keklik, Mehmet; Golge, Ozgur; Angel Gonzalez-Curbelo, Miguel; Kabak, Bulent
    Commercial viticulture necessitates regular pesticide applications to manage diseases and pests, raising significant concerns regarding pesticide residues among stakeholders. Due to health risks associated with these residues in Turkish vine leaves, the European Commission has increased the frequency of official control from 20% to 50%. Thus, the aim of this study was to determine multi-class pesticide residues in brined vine leaves from Turkey. A total of 766 samples of vine leaves were collected between May 2022 and June 2023. More than 500 residues were analyzed using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, followed by liquid chromatography-tandem mass spectrometry. In-house validation data demonstrated that the analytical method exhibits fit-for-purpose performance in terms of linearity, accuracy, precision, and measurement uncertainty. Out of 766 samples analyzed, 180 samples (23.5%) contained one (131, 17.1%) or multiple (49, 6.4%) pesticides. Both the frequencies of occurrence and the rate of maximum residue level (MRL) exceedance increased in 2023 compared to 2022, with the MRL exceedance rate rising from 9.5% to 25.2%. Forty-three different residues were found in quantifiable concentrations and eight of them were non-approved. Among the residues, the non-systemic pyrethroid insecticides, lambda-cyhalothrin (8.0%) and cypermethrin (7.2%), were the two most frequently detected, with concentrations ranging from 0.010 to 0.248 mg kg-1 and from 0.011 to 0.533 mg kg-1, respectively. Turkey is a major exporter of vine leaves and these results provide crucial information regarding pesticide occurrence and quality assessment of vine leaves. The significant increase in both pesticide occurrence and MRL exceedance rates between 2022 and 2023 underscores the urgency for regulatory bodies to reassess current pesticide usage and monitoring practices. The findings emphasize the importance of implementing more stringent rules and improving enforcement methods in order to reduce the spread of unapproved pesticides and ensure adherence to global food safety standards.
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    Monitoring and Risk Assessment of Multi-Pesticide Residues in Apples: A Focus on Consumer Safety
    (Mdpi, 2024) Odabas, Eylem; Keklik, Mehmet; Golge, Ozgur; Gonzalez-Curbelo, Miguel angel; Kabak, Bulent
    Pesticide residues in human diets pose significant health hazards, particularly for vulnerable populations such as infants and children. This study aimed to determine pesticide residues in apples and to assess the cumulatively chronic risk posed to adult and child consumers from simultaneous exposure to multiple residues. During the 2022-2023 harvest seasons, 100 apple samples from Turkey were analyzed for the presence of 225 different pesticide residues. Pesticide extraction was performed using the QuEChERS method, followed by detection through liquid chromatography coupled with tandem mass spectrometry. Fifteen distinct pesticides (ten insecticides and five fungicides) were detected in 64 out of the 100 apple samples analyzed. Eleven samples contained pesticide residues that exceeded the maximum residue limit (MRL) set by the Turkish Food Codex and the European Union. Thiophanate-methyl was the most frequently detected pesticide (34%) in apples, with concentrations ranging from 0.012 to 0.108 mg kg-1, all of which were well below the MRL of 0.5 mg kg-1. Other commonly detected residues included chlorantraniliprole (28%), acetamiprid (24%), sulfoxaflor (22%), bifenazate (18%), indoxacarb (13%), diflubenzuron (12%), and carbendazim (10%). Under a worst-case scenario, the hazard index (HI) values for adults and children were 0.85% and 2.60%, respectively, indicating that these values remain significantly below the risk threshold of 100%, suggesting no associated health risks from apple consumption. However, regular monitoring of pesticide residues in fresh fruits and vegetables remains critically important.
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    Pesticide residue levels in strawberries and human health risk assessment
    (Academic Press Inc Elsevier Science, 2025) Keklik, Mehmet; Odabas, Eylem; Golge, Ozgur; Kabak, Bulent
    Pesticides have been a primary tool in pest management worldwide. However, pesticide contamination is a major food safety risk in the fresh food supply chain. This study aims to monitor 240 pesticide residues in 245 strawberry samples and assess the health risk for Turkish adult and child consumer groups. Over three consecutive harvest years (2021-2023), strawberries were collected from farmers in the Ayd & imath;n region of Turkey and analysed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Out of the 245 strawberry samples analysed, 61.6% contained 32 different pesticides (17 fungicides and 15 insecticides), five of which were non-approved. Additionally, 6.5 % of the strawberry samples exceeded the European Union Maximum Residue Limits (MRLs). Multiple residues were recorded in 42.9% of strawberry samples. Pyrimethanil was the most commonly identified pesticide (30.2 %), followed by boscalid (27.4 %), fluopyram (17.1 %), and bifenazate (15.1 %). In the worst-case scenario, cumulative exposure to pesticides through strawberry consumption was determined to be 6.5 x 10-5 mg kg-1 b.w. day-1 for adults and 2.0 x 10-4 mg kg-1 b.w. day-1 for children. The hazard index (HI) values, under the worst-case scenario, were calculated to be 0.32 % for adults and 0.97 % for children. These results indicate that there is no cause for concern regarding cumulative exposure to residues through strawberry consumption for the Turkish population.
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    Pesticide residues in peaches and nectarines: Three-year monitoring data and risk assessment
    (Elsevier Sci Ltd, 2025) Keklik, Mehmet; Golge, Ozgur; Gonzalez-Curbelo, Miguel Angel; Kabak, Bulent
    Peaches and nectarines suffer from various diseases annually, prompting widespread pesticide use for pest management. As a result, pesticide residues remain a notable concern for food safety. This study assessed 474 pesticide residues in peaches and nectarines consumed in Turkey, analyzing 459 samples (164 peaches and 295 nectarines) over three harvest seasons (2021-2023). Using a validated method based on QuEChERS (quick, easy, cheap, effective, rugged, and safe) and liquid chromatography-tandem mass spectrometry, in compliance with the European SANTE/11312/2021 Guideline, residues were found in 71.3% of peaches and 71.9% of nectarines. Multiple residues were more prevalent in peaches (49.4%) than nectarines (37.6%), with 12.8% of peaches and 5.8% of nectarines exceeding maximum residue levels. Peaches contained 40 different residues, including 12 unapproved in the European Union, while nectarines had 35 residues, 13 unapproved. Common residues included thiophanate-methyl, acetamiprid, and boscalid. Hazard Index values (0.49% for adults, 0.60% for children) indicated no significant health risk from chronic pesticide exposure through peach and nectarine consumption among Turks.
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    Quantification and risk assessment of pesticide residues in Sultani seedless grapes: Implications for consumer safety
    (Pergamon-Elsevier Science Ltd, 2025) Keklik, Mehmet; Odabas, Eylem; Golge, Ozgur; Kabak, Bulent
    Pesticides are frequently used in viticulture to control various pests and diseases, but their residues can accumulate in grape products, raising concerns regarding consumer safety. This study aimed to evaluate the occurrence of 268 pesticide residues in Sultani seedless grapes produced in Turkey, with a particular focus on their potential implications for both acute and chronic health risks. Of the 473 grape samples analyzed by liquid chromatography-tandem mass spectrometry, only 11 samples (2.3 %) were free from detectable pesticide residues. Pesticide residues at quantifiable levels were identified in 462 samples (97.7 %), and 52 of these samples exceeded the European Union Maximum Residue Levels. The most frequently recorded pesticides in grapes, with occurrence rates exceeding 50 %, were ametoctradin, metalaxyl, cyprodinil, pyrimethanil, spirotetramat, and fluopyram. Chronic dietary exposure assessments revealed that pesticide residues in grapes do not pose substantial health risks to both adults and children in Turkey, as hazard quotients remained well below critical thresholds. However, acute exposure risks for acetamiprid, emamectin benzoate, and lambda-cyhalothrin exceeded acceptable limits in a fraction of the samples, especially for children. These findings underscore the importance of enhanced pesticide monitoring and regulatory compliance to ensure consumer safety and promote the adoption of integrated pest management practices.