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Öğe A potential threat to black figs intended for export from Turkey: Ethephon(Academic Press Inc Elsevier Science, 2021) Gormez, Emrah; Golge, Ozgur; Dincay, Orhan; Kabak, BulentThe analysis of highly polar pesticide residues in fruits and vegetables has become a controversial issue in the last decade. This report shows the results of highly polar pesticide residues (ethephon, fosetyl aluminium (fosetyl-Al) and phosphonic acid) monitoring on black figs intended for export from Turkey. From 2017-2020, a total of 9237 black fig samples were analysed for ethephon, fosetyl-Al and phosphonic acid residues using the Quick Polar Pesticides (QuPPe) method. The method has shown to have sufficiently low limits of quantification with respect to EU Maximum Residue Levels (MRLs). The obtained recovery and precision parameters fulfil the requirements in SANTE/11813/2017 Guideline. The 16.8 % of black fig samples were detected with ethephon at quantifiable concentrations but below the EU MRL of 3 mg kg- 1. The concentration of ethephon ranged between 0.005 and 2.47 mg kg- 1. However, no quantifiable residues of fosetyl-Al and phosphonic acid were detected in any black fig samples.Öğe A preliminary study on patulin contamination in spirit drinks(Taylor & Francis Ltd, 2022) Golge, Ozgur; Yenisehirlioglu, Emirhan; Kabak, BulentA total of 120 spirit drinks and 40 apple juices were collected between 2018 and 2020 in three regions of Turkey and analysed by high-performance liquid chromatography coupled with a photodiode array detector (HPLC-PDA) for the incidence of patulin. The analytical method was successfully validated for both matrices. In 26.7% of apple juice samples, patulin was quantified at levels between 5.8 and 66.4 mu g L-1. Only one regulatory level exceedance was identified for apple juice. The mean dietary exposure of the adult population to patulin ranged from 0.083 to 0.091 ng kg(-1) bw day(-1). With the HPLC-PDA method, patulin was measured in quantifiable concentrations in 11 out of 25 cognac, 5 out of 40 liqueur, and 1 out of 10 whisky samples, up to a level of 42.6 mu g/l, whereas all vodka samples were free from patulin. In only one liqueur sample, the presence of patulin could be confirmed with LC-MS/MS, at a level of 8.9 mu g L-1.Öğe Assessment of pesticide contamination in pomegranates: A multivariate approach and health risk evaluation(Pergamon-Elsevier Science Ltd, 2025) Gormez, Emrah; Odabas, Eylem; Golge, Ozgur; Gonzalez-Curbelo, Miguel Angel; Kabak, BulentPesticide residues in pomegranates pose a significant food safety concern, particularly given the rising global consumption of this fruit. This study monitored 316 pesticide residues in 342 pomegranate samples from Turkey's three primary pomegranate production regions using liquid chromatography-tandem mass spectrometry. Pesticide residues were detected in 72.8% of the samples, with 40 different pesticides identified, 15 of which were unauthorized. Spirotetramat, acetamiprid, and fludioxonil were among the most frequently detected, with concentrations exceeding the maximum residue levels set by the European Union in 40.6% of the contaminated samples. Multivariate analysis revealed strong correlations between specific pesticide pairs, suggesting common usage patterns. The chronic hazard index was 0.0132 for adults and 0.0403 for children, indicating no significant chronic health risks. The acute health risks for all pesticides remained below acceptable limits, except for acetamiprid, which exceeded the threshold (1.186) for children. However, the presence of non-approved pesticides, such as omethoate, raises concerns about regulatory compliance. Continued surveillance and risk assessment are essential to minimize potential health risks, particularly for vulnerable populations consuming pomegranates.Öğe Determination of 355 Pesticides in Lemon and Lemon Juice by LC-MS/MS and GC-MS/MS(Mdpi, 2023) Aslantas, Sule; Golge, Ozgur; Gonzalez-Curbelo, Miguel Angel; Kabak, BulentWhile pesticides have become a primary tool in modern agriculture, these compounds remain a high priority on the list of consumer concerns regarding food safety. The use of pesticides in the production and post-harvesting of lemon fruits is widely used to ensure agricultural yield and fruit quality. Therefore, monitoring studies on citrus fruits to enforce regulatory compliance and ensure food safety is in great demand. The aim of this study was to monitor multi-class pesticide residues in lemon fruits commercialized in Turkey. The transmission of residues that existed on the outer surface of the fruit into its juice was also studied. Whole fruits and lemon juice samples were prepared using the quick, easy, cheap, effective, rugged and safe (QuEChERS) methodology prior to analysis. For the screening and quantification of 355 pesticide residues, liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS) were used. The analytical method has been shown to have a sufficiently low limit of quantification with respect to current maximum residue limits (MRLs) for all target analytes. The obtained recovery and precision parameters fulfilled the requirements in DG SANTE guidelines. The in-house validated analytical method was then applied for the determination of 355 pesticide substances in 100 whole fruit samples and their juices. Sixteen different residues were detected in 43% of lemon fruits, whereas 57 lemon samples were pesticide-free. The MRLs exceedances were recorded in 29 lemon samples. The most frequently detected (17%) pesticide in lemon fruits was chlorpyrifos-methyl, with a range of 0.013-0.098 mg kg(-1). A lower frequency was detected for metamitron (10%, 0.027-0.118 mg kg(-1)), buprofezin (9%, 0.023-0.076 mg kg(-1)), pyriproxyfen (9%, 0.021-0.102 mg kg(-1)) and malathion (7%, 0.100-0.482 mg kg(-1)) in whole fruits. However, none of the pesticide residues were detected in lemon juice samples. These results showed that target analytes are unable to penetrate the lemon exocarp and/or endocarp.Öğe 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, BulentCommercial 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.Öğe Infant and toddler health risks associated with pesticide residue exposure through fruit- and vegetable-based baby food(Academic Press Inc Elsevier Science, 2025) Isci, Gursel; Golge, Ozgur; Kabak, BulentThis research specifically delves into the potential health risks associated with pesticide residues in fruit- and vegetable-based foods for Turkish infants and toddlers. A total of 36 baby food samples were analyzed using a validated method covering 355 pesticide residues, employing liquid chromatography-tandem mass spectrometry (LCMS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS). Notably, 72.2 % of the samples revealed no pesticide residues, while 10 samples exceeded the Maximum Residue Limits (MRLs) stipulated by the EU Directives. Specifically, pyriproxyfen had the greatest average concentration in pear fruits (0.573 mg/kg). Notably, both pyrimethanil and pyriproxyfen were the most frequently detected analytes in all positive samples. The study further simulated a population, considering age-specific energy requirements for infants and toddlers. Pyriproxyfen demonstrated the highest average exposure (1.58 +/- 2.20 mu g/kg bw/day) across all age groups. Notably, for 6-month-old infants, the toxicological contribution as a percentage of the ADI for pesticides remained below 14.73 %. It emphasizes the necessity for regulatory measures to ensure the safety of foods intended for infants and toddlers in the Turkish market. These findings support ongoing efforts to uphold pesticide levels within acceptable safety limits.Öğe Monitoring and Exposure Assessment of Fosetyl Aluminium and Other Highly Polar Pesticide Residues in Sweet Cherry(Mdpi, 2023) Gormez, Emrah; Golge, Ozgur; Angel Gonzalez-Curbelo, Miguel; Kabak, BulentCherries are popular fruits due to their health benefits, organoleptic quality, and attractive appearance. Since highly polar pesticides are of low mass and amphoteric character, and are not amenable to traditional multi-residue extraction methods, they are more commonly not included in the pesticide monitoring program. This study aims to determine twelve highly polar pesticide residues in cherry samples intended for export from Turkey. A total of 16,022 cherry samples from 2018-2020 harvests in four production areas of Turkey were analyzed using a modification of the Quick Polar Pesticides method and liquid chromatography-tandem mass spectrometry. The method was validated at two fortification levels (0.01 and 0.05 mg kg(-1)), and good recoveries (87.4-111.4%) and relative standard deviations (<6%) were achieved for all analytes. The limits of quantification were in the range of 1.08-2.55 mu g kg(-1). Overall, 28.4% of the analyzed cherry samples were detected with phosphonic acid, calculated as fosetyl aluminium (fosetyl-Al) in amounts up to 77.7 mg kg(-1). For 2304 samples (14.4%), the residues exceeded the European Union maximum residue level of 2 mg kg(-1). There is no reason to be concerned about long-term exposure to phosphonic acid/fosetyl-Al, and the other highly polar pesticides through the consumption of sweet cherry.Öğe 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, BulentPesticide 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.Öğe Occurrence, regulatory compliance, and health risk evaluation of pesticide residues in Turkish raisins(Elsevier Sci Ltd, 2026) Ogmen, Esra; Buyuksirit-Bedir, Tuba; Golge, Ozgur; Kabak, BulentPesticide residues in processed fruit products such as raisins are of growing concern due to potential dietary exposure risks. In this study, 100 Turkish raisin samples were analyzed for 290 multi-class pesticides using gas chromatography-tandem mass spectrometry for volatile compounds and liquid chromatography-mass spectrometry for non-volatile compounds. A total of 45 different residues were detected, including fourteen pesticides not approved in the EU. Acetamiprid was the predominant residue (29 % of the samples), reaching levels up to 23.4 times higher than its derived maximum residue level, followed by metalaxyl (27 %), pyrimethanil (25 %), and pyriproxyfen (24 %). Chronic dietary exposure was evaluated using both deterministic and probabilistic (Monte Carlo simulation) approaches. The deterministic chronic hazard index (HIc) values were 0.0011 and 0.0014 for adults and children, respectively, whereas probabilistic simulations yielded mean HIc values of 0.0054 and 0.0070, confirming that chronic dietary exposure poses negligible health risks (HIc < 1). However, acute exposure analysis revealed potential short-term risks for both adults and children, primarily driven by acetamiprid and alpha-cypermethrin. These results highlight the persistence of certain systemic insecticides and the continued use of non-approved compounds despite regulatory restrictions, emphasizing the need for enhanced monitoring programs and stricter regulatory enforcement to ensure food safety.Öğe Pesticide residue levels in strawberries and human health risk assessment(Academic Press Inc Elsevier Science, 2025) Keklik, Mehmet; Odabas, Eylem; Golge, Ozgur; Kabak, BulentPesticides 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.Öğe Pesticide Residues in Mandarins: Three-Year Monitoring Results(Mdpi, 2023) Gormez, Emrah; Golge, Ozgur; Gonzalez-Curbelo, Miguel Angel; Kabak, BulentThe demand of plant production product use has increased because of the current system of citrus production, which prioritizes high agricultural yields. Therefore, the monitoring of pesticide residues in citrus fruits and other agricultural products and their impacts on human health and food security are of great concern. This study aims to determine multi-class pesticides including highly polar residues in satsuma mandarins. A total of 226 mandarin samples were collected over three consecutive harvesting years from 2019 to 2021 in the Izmir region of Turkey. Targeted compounds included pesticides and metabolites with European Union (EU) regulatory levels, plus other non-approved residues and highly polar compounds. The residues excluding highly polar substances were analyzed by applying the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction and liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) determination for 434 analytes and gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) determination for 71 analytes. For six highly polar pesticides, sample preparation was based on Quick Polar Pesticides (QuPPe) extraction. The polar residues were determined by LC-MS/MS using internal standards. Forty different residues, including two highly polar substances, were recorded in mandarin samples through three harvesting years. In 8.4% of the samples, no quantifiable residues were detected, whereas 207 samples contained at least one residue. The maximum residue level (MRL) exceedances were recorded for 22.1% of the samples. The two most frequently found pesticides were phosphonic acid and spirotetramat, with an incidence rate of 48.7% and 46.5%, respectively. The concentration of phosphonic acid and spirotetramat in mandarin samples varied from 0.026 to 39.386 mg kg(-1) and from 0.010 to 1.485 mg kg(-1), respectively. The results will enable researchers and regulatory authorities to assess the extent of pesticide presence, identify potential risks, and take necessary measures to ensure the safety of satsuma mandarins for consumers.Öğe 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, BulentPeaches 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.Öğe 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, BulentPesticides 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.Öğe Quantification of 363 Pesticides in Leafy Vegetables (Dill, Rocket and Parsley) in the Turkey Market by Using QuEChERS with LC-MS/MS and GC-MS/MS(Mdpi, 2023) Deveci, Bilge; Golge, Ozgur; Kabak, BulentContamination of agricultural products with pesticide residues is a growing concern due to their adverse health effects and increasing worldwide usage of pesticides. In 2021 a total of 200 samples of green leafy vegetables, including 80 dill, 80 rocket and 40 parsley, purchased from greengrocer shops, markets and bazaars in Corum Province, Turkey, were monitored for pesticide residues. In green leafy vegetables, 363 pesticides were analyzed using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation, followed by liquid chromatography coupled to mass spectrometry (LC-MS/MS) for 311 residues and gas chromatography coupled to mass spectrometry (GC-MS/MS) for 52 residues. The method was in-house validated at two fortification levels, and satisfactory recoveries and precisions were achieved for all residues. No quantifiable residues were found in 35% of the samples, whereas 43 residues belonging to 24 different chemical classes were detected in 130 green leafy vegetables. Among the green leafy vegetables, the highest occurrence frequency was recorded in the rocket, followed by dill and parsley. In 46% of the green leafy vegetables, the residue levels exceeded European Union Maximum Residue Levels (EU MRLs). The most frequently detected pesticides were pendimethalin (22.5%), diuron (38.7%) and pymetrozine (52.5%) in dill, rocket and parsley, respectively.Öğe Quantification of fosetyl-aluminium/phosphonic acid and other highly polar residues in pomegranates using Quick Polar Pesticides method involving liquid chromatography-tandem mass spectrometry measurement(Elsevier, 2021) Gormez, Emrah; Golge, Ozgur; Kabak, BulentInterest in the quantification of highly polar substances in crops has noticeably increased in the last five years. This study was designed to assess quantification of six polar residues, chlorate, ethephon, fosetlyaluminium (fosetyl-Al), glyphosate, phosphonic acid and perchlorate. A total of 2513 pomegranate samples intended for export from Turkey were analysed using the Quick Polar Pesticides (QuPPe) method. The method was in-house validated with very good performance results. The limits of quantification (LOQs) for residues were much lower than the respective EU Maximum Residue Levels (MRLs). Phosphonic acid was detected in 38.5% of pomegranate samples at quantifiable concentrations, calculated as fosetyl-Al. The concentrations ranged between 0.005 and 12.9 mg kg(-1) . The 20% of pomegranate samples showed fosetyl-Al levels above the EU MRL of 2 mg kg(-1) . Other polar residues were not detected in any pomegranate samples. This is the first report about highly polar pesticides in pomegranates cultivated in Turkey. (C) 2021 Elsevier B.V. All rights reserved.Öğe Validation of Quick Polar Pesticides (QuPPe) Method for Determination of Eight Polar Pesticides in Cherries by LC-MS/MS(Springer, 2021) Golge, OzgurA novel and sensitive chromatography method with modified Quick Polar Pesticide (QuPPe) sample preparation was validated for determination of eight high polar pesticides in cherries by liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS). The validation data executed the conditions of the European SANTE/12682/2019 Guidance Document. Good linearity (R-2 > 0.99) was observed, and the residuals were lower than +/- 20%. Average recoveries ranged from 70.2 to 105.1%, and LOQ values ranged from 1.77 to 12.13 mu g kg(-1). The repeatability and reproducibility are in range of 1.57-15.56% and 3.51-16.17% separately. All measurement uncertainty values were lower than 50% for all polar pesticides. This verified analytical method was used to detect pesticide residue levels of cherries, and none of the eight high polar pesticides were found in 225 real samples. This is the first validation report of QuPPe sample preparation and LC-MS/MS method of high polar pesticide residues in cherries from Turkey.
