This study evaluated the influence of different drying methods (oven, vacuum oven, sun, shade, and greenhouse) and temperatures (60, 70, and 80 °C) on the reduction of acetamiprid and pyridaben residues in capia peppers (Capsicum annuum L.). Drying was conducted until the samples reached the target moisture content, and drying characteristics, energy consumption, color parameters, and pesticide residues were determined. Among the tested methods, oven drying at 80 °C resulted in the shortest drying time and the highest energy efficiency. Greenhouse drying generally preserved product color more effectively than the other methods. Drying kinetics were best described by the Page model (R2 = 0.9997). Both pesticides showed significant reductions during the drying process, with pyridaben exhibiting greater reduction than acetamiprid. Increasing drying temperature enhanced pesticide reduction across all drying methods. The highest residue reductions were obtained under oven and vacuum oven drying at 80 °C. While vacuum drying at 80 °C produced the greatest net residue reduction, oven drying at the same temperature provided a more favorable balance between drying time and energy efficiency. These findings demonstrate that drying, particularly at elevated temperatures, can serve as an effective postharvest strategy for reducing pesticide residues in peppers while maintaining acceptable product quality and process efficiency.
OBJECTIVES:The chemical composition of resin composites and the use of modeling liquids may influence the release of residual monomer, potentially impacting biocompatibility. This in vitro study evaluated the effect of different modeling liquids on the elution of monomers from two resin composites. MATERIALS AND METHODS:Eighty disc-shaped samples were prepared using two nano-hybrid resin composites (Estelite Sigma Quick, Tokuyama; Harmonize, KERR) and three modeling liquids; Composite Wetting Resin (Ultradent, USA), Modeling Resin (Bisco, USA), and Modeling Liquid (GC, Japan) (n = 10). Resin composites were placed in four 0.5-mm increments into Teflon molds, and modeling liquids were applied with a brush between layers; control groups were prepared without modeling liquids. After polishing (Sof-Lex, 3 M ESPE), specimens were stored in 75% ethanol at 37°C. Release of UDMA, Bis-GMA, TEGDMA, and HEMA was quantified using a liquid chromatography-tandem mass spectrometry (LC-MS/MS) system (LCMS-8050, Shimadzu, Japan) at 24 h, 7 days, and 30 days. Data normality was assessed, and effects of resin composites type, modeling liquid, and time were analyzed using three-way ANOVA with Bonferroni post hoc testing (α = 0.05). RESULTS:Application of modeling liquid significantly reduced Bis-GMA release for both resin composites (p < 0.05). While TEGDMA release was significantly decreased in Estelite Sigma Quick groups (p < 0.05), no difference was observed in Harmonize groups. Modeling liquid applications increased total HEMA and UDMA release (p < 0.05). TEGDMA release in the Estelite Sigma Quick-control group was higher than the Harmonize-control group (p < 0.05). CONCLUSION:The organic matrix of composite resins and the modeling liquids used influence the release of the tested monomers (TEGDMA, BisGMA, UDMA, and HEMA). The use of modeling liquid showed differences in monomer release according to the content of the liquid. CLINICAL SIGNIFICANCE:Modeling liquids may increase residual monomer release from resin composites, particularly shortly after polymerization. Clinicians should use these materials sparingly and in accordance with manufacturers' instructions to minimize potential biocompatibility risks.
This study evaluated the effects of foliar paclobutrazol (PBZ) applications at different doses and intervals on plant growth, yield, fruit quality, and under greenhouse conditions. The experiment was conducted using a randomized complete block design with three replications. PBZ was applied to shoot tips at concentrations of 10, 20, and 40 mg L-1, at 7- and 14-day intervals, while distilled water was used for the control group. PBZ treatments significantly reduced plant height and internode length. The most notable reduction in plant height (20.3%) was observed with the 20 mg L-1 dose applied weekly. The highest marketable yield (184.03 t/ha) was achieved with the 40 mg L-1 PBZ treatment applied every 14 days, which was 1.08% higher than the control (182.07 t ha-1). In contrast, the 20 mg L-1 weekly application resulted in an 11.7% decrease in yield. The average marketable fruit weight increased by 13.5% (reaching 98.44 g) under the 40 mg L-1 weekly treatment. However, this increase was accompanied by a 13.6% reduction in fruit number per plant. PBZ applications significantly affected the chlorophyll index (SPAD), with the highest value (55.47) recorded in the 40 mg L-1 treatment applied at 7day intervals. In contrast, fruit and leaf dry matter contents were not significantly influenced by the treatments. The PBZ doses and application methods used in the study did not result in detectable residues in cucumber fruits under the experimental conditions. This finding suggests that, within the scope of this study, the application does not pose a residue-related concern for food safety and represents one of the key outcomes of the research. In conclusion, foliar PBZ applications fruit weight, and total yield, without compromising fruit quality. or leaving harmful residues.
Pesticides, including insecticides, are widely used to control pests in modern agriculture. However, a small portion of the applied insecticide reaches the intended target, while off-target losses may contaminate agricultural environments. This review focused on the fate of insecticides in the environment and strategies to reduce their ecotoxicological risks. In this context, the environmental behavior of insecticides, their pathways into the ecosystem and the ecotoxicological effects on non-target organisms, ways to reduce ecotoxicological risks are discussed. Risk-reduction options discussed include IPM, modern application technologies, development of lower-risk insecticides, nanotechnology-based formulations, and remediation. The transport, distribution, persistence, and major exposure routes of insecticides are examined collectively, and measures for minimizing contamination of surface water and groundwater are summarized. Ecotoxicological risk is affected by the physicochemical properties of the insecticide, application method, soil characteristics, and environmental conditions. Future research should prioritize current-use insecticides, acaricides, and nematicides, realistic mixture exposures, and sustainable management strategies.
This study investigates the dissipation kinetics, biodegradation, and health risk assessment of formetanate hydrochloride (FMT) in pepper under field conditions. Utilizing LC–MS/MS, the degradation behavior of FMT was analyzed, revealing significant residue reduction when bacterial strains were applied. The bacteria mix treatment exhibited the most effective residue dissipation, reducing health risks by minimizing both chronic and acute exposure. Climatic factors such as humidity and temperature significantly influenced the dissipation rates, emphasizing the need for localized residue management strategies. The study underscores the potential of microbial treatments as eco-friendly solutions for managing pesticide residues, promoting food safety, and ensuring sustainable agricultural practices. Further research should explore FMT dynamics in diverse crops and environmental conditions to optimize pesticide management frameworks.
Pesticides are widely used in grape production to control pests and diseases, protect yield, and maintain commercial quality. This study investigated pesticide residues in fresh table grapes collected from Salihli, Alaşehir, and Sarıgöl (Manisa Province, Türkiye). A multiresidue QuEChERS-LC–MS/MS method was applied, covering 260 active substances across different pesticide classes (insecticides, fungicides, herbicides, acaricides, and nematicides). In total, 54 grape samples were analyzed. At least one pesticide residue was detected in every sample. Two different pesticides were found in 5 samples, while three or more pesticides were identified in 43 samples, indicating frequent co-occurrence of multiple residues. Overall, 32 different active substances were detected. The insecticides identified included acetamiprid, buprofezin, chlorantraniliprole, lambda-cyhalothrin, deltamethrin, flubendiamide, indoxacarb, methoxyfenozide, and tebufenozide. The fungicides identified included ametoctradin, azoxystrobin, boscalid, bupirimate, cymoxanil, cyprodinil, difenoconazole, dimethomorph, famoxadone, fluopicolide, fluopyram, kresoxim-methyl, mandipropamid, metalaxyl-M, metrafenone, myclobutanil, penconazole, pyrimethanil, spiroxamine, tetraconazole, tebuconazole, triadimenol, and trifloxystrobin. Residue concentrations were evaluated against the European Union maximum residue limits (EU-MRLs). Among 301 quantified pesticide-sample combinations, 294 results complied with EU-MRLs, while seven exceeded the corresponding legal limits. Pyrimethanil, boscalid, and cyprodinil were the most frequently detected compounds. Except for bupirimate (a fungicide), all exceedances involved insecticides, specifically acetamiprid, buprofezin, deltamethrin, and methoxyfenozide. The dietary risk assessment revealed that acetamiprid contributed the highest acute exposure, while bupirimate and famoxadone showed relatively higher chronic exposure values. These results emphasize the importance of continuous pesticide residue monitoring in table grapes, ensuring the use of only authorized plant protection products and maintaining residue levels within regulatory limits to safeguard consumer health and environmental sustainability.
Pesticides enhance crop productivity but leave residues that threaten the health and the environment, necessitating sensitive analytical methods to detect widely used compounds like pirimicarb. This study focuses on optimizing the analysis of pirimicarb and its metabolites using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Key instrumental parameters including interface temperature, desolvation line temperature, heat block temperature, column oven temperature, collision-induced dissociation (CID) gas pressure, and interface voltage were systematically optimized to enhance method sensitivity and reliability. Among the tested conditions, interface temperatures of 150 °C and 400 °C provided the highest signal intensity for pirimicarb, while pirimicarb-desmethyl responded best at 250 °C, and pirimicarb-desmethyl-formamido showed maximum signals at 150 °C and 300 °C. For desolvation line temperature, 150 °C yielded the highest intensities for pirimicarb and pirimicarb-desmethyl, whereas 200 °C was optimal for pirimicarb-desmethyl-formamido. Pirimicarb exhibited peak response at a heat block temperature of 300 °C, while pirimicarb-desmethyl showed comparable intensities at 100, 200, and 350 °C, and pirimicarb-desmethyl-formamido responded best at 100 and 200 °C. Column oven temperatures of 40 °C and 50 °C enhanced the response for pirimicarb, with pirimicarb-desmethyl and pirimicarb-desmethyl-formamido showing optimal intensities at 50 °C. Additionally, a CID gas pressure of 270 kPa and interface voltage of 4.0 kV produced the highest ionization efficiency across all analytes. The results demonstrated that specific parameter adjustments significantly improved ionization efficiency and signal intensity, leading to a more robust analytical method. This study underscores the importance of systematic parameter optimization in LC-MS/MS for accurate pesticide residue detection and provides a framework for future research on other pesticide groups.
This study aimed to determine pesticide residues in raisin samples from the Besni and Gölbaşı districts of Adıyaman province, located in the Southeastern Anatolia region of Türkiye. Method validation was carried out for parameters including linearity, limit of detection (LOD), limit of quantification (LOQ), recovery, precision (repeatability and in-laboratory reproducibility), and measurement uncertainty. The results met the criteria outlined in SANTE/11312/2021. A total of 260 pesticides were analyzed, with pesticide residues detected in 95 out of 100 samples. Among these, 42 samples contained a single pesticide, while 53 samples had two or more residues. The insecticides cypermethrin, indoxacarb, and malathion, along with the fungicides boscalid, flubendiamide, fluopyram, pyrimethanil, and spiroxamine, were identified. All detected pesticide residues were within the LOQ and maximum residue limit (MRL), with no residues exceeding the MRL. According to the analysis, eight different pesticides were identified in the samples. The study confirms that pesticide residues in dried grape samples comply with the MRLs, suggesting minimal health risks for consumers, as both long-term and short-term dietary risks were found to be negligible. However, the presence of multiple pesticide residues underscores the need for ongoing monitoring and stringent regulatory measures to ensure food safety and maintain compliance. These findings provide valuable insights into improving sustainable agricultural practices in grape production and establishing a more effective monitoring system for pesticide residues in raisins
This study investigates the dissipation behavior of acetamiprid, boscalid, and pyraclostrobin applied individually and in mixtures to cherries under open-field conditions in Tokat and Niksar, T & uuml;rkiye. The research highlights how application methods (recommended vs. double dose, individual vs. mixture) and environmental factors influence residue persistence. Results showed that dissipation was slower under double-dose and mixture treatments, particularly in Niksar, where lower humidity levels may have contributed to extended half-lives. These findings underscore the importance of evaluating pesticide fate under realistic agricultural practices and variable field conditions. In addition to dissipation analysis, a dietary risk assessment was conducted. Hazard quotient values for both chronic (HQc) and acute (HQa) exposures were below the safety threshold of 1 in all scenarios, indicating no immediate health risk. However, children exhibited the highest HQc values, especially under mixture and double-dose applications, highlighting the need for cautious management practices. Overall, this study contributes valuable data for refining preharvest interval recommendations and promoting safer pesticide use in cherry cultivation.
This study investigates the dissipation kinetics of deltamethrin and lambda-cyhalothrin residues in apples grown in two distinct regions in T & uuml;rkiye under open-field conditions. Using the QuEChERS method coupled with LCMS/MS analysis, the method was validated with recovery rates within acceptable ranges and high sensitivity, achieving LOQ values of 2.77 mu g/kg for deltamethrin and 3.40 mu g/kg for lambda-cyhalothrin. Both pesticides exhibited first-order kinetic degradation, with half-lives ranging from 1.49 to 1.99 days for deltamethrin and 2.59 to 3.65 days for lambda-cyhalothrin. Residue levels remained below maximum residue limits (MRLs) for recommended application rates shortly after spraying, ensuring compliance with safety standards. However, double-dose applications resulted in higher initial residues, extended half-lives, and increased short-term exposure risks. A health risk assessment revealed hazard quotients (HQa and HQc) well below 1, indicating negligible acute and chronic risks for consumers under recommended practices. These findings underscore the importance of adhering to proper pesticide application guidelines to minimize risks and ensure food safety.
This study investigated the dissipation kinetics of formetanate hydrochloride (FMT) in tomatoes and cucumbers under greenhouse and open-field conditions in T & uuml;rkiye. Four treatments were applied to both crops: a single dose, a double dose, FMT with a spreader, and FMT with sugar. Residue analysis was conducted using a validated QuEChERS-LC-MS/MS method. In greenhouse-grown tomatoes, the initial FMT concentrations ranged from 0.38 to 0.59 mg/kg, and the half-lives ranged from 4.25 to 4.53 days. In field-grown tomatoes, the half-lives ranged from 5.33 to 8.15 days, indicating slower degradation under open-field conditions. For greenhouse-grown cucumbers, the half-lives ranged from 2.91 to 3.47 days. Residue levels in field-grown cucumbers could not be determined due to insufficient residue concentrations. The results indicated that both environmental conditions and the addition of adjuvants influenced the degradation dynamics of FMT. These findings provide important data for improving pesticide application strategies and ensuring food safety.
This study investigates the occurrence, distribution, and health risks of pesticide residues in citrus fruits (lemon, mandarin, and orange) collected from various regions in T & uuml;rkiye. A total of 260 pesticides were analyzed using liquid chromatography-tandem mass spectrometry (LC-MS/MS), and residue levels were evaluated based on EU maximum residue limits (EU-MRLs). Pesticide residues were detected in 109 samples, with 28 exceeding the EUMRLs. The most frequently detected pesticides were malathion, acetamiprid, and buprofezin. Matrix effects varied significantly among citrus varieties, emphasizing the necessity of matrix-matched calibration for accurate residue quantification. The health risk assessment indicated that chronic exposure to pesticide residues in citrus fruits remained within acceptable limits for adults. However, children were found to be more vulnerable due to their lower body weight and higher consumption relative to body mass. Acute exposure evaluations revealed that certain pesticides (particularly imazalil, chlorpyrifos, and pyrimethanil) exceeded safety thresholds in citrus peels. These findings highlight the need for more rigorous monitoring, improved pre- and post-harvest practices, and risk mitigation strategies, particularly for vulnerable groups such as children. The study emphasizes the importance of considering tissue-specific residue distribution in exposure assessments and policymaking.
The study was conducted in 2022 in a fully automated, soilless agriculture greenhouse at the Research Centre Directorate of Tokat Gaziosmanpaşa University. The study investigated the effects of different doses of paclobutrazol (PBZ) on yield, quality, plant growth, and PBZ residue levels in tomato plants. The plant material employed in this study was the Belford Fı (Syngenta-Türkiye) pole tomato variety. The experiment was conducted in three replicates according to a random plots factorial experiment design. The results of this study indicate that foliar applications of 50 ppm, and 100 ppm PBZ produced the most optimal outcomes. The highest marketable yield was observed in the treatment with a foliar application of 50 ppm PBZ, resulting in an average yield of 385.33 kg/ha. Subsequently, a foliar application of PBZ at a rate of 100 ppm (374.24 kg/ha) was conducted, along with a control treatment (268.55 kg/ha). The study revealed no statistically significant differences between treatments in terms of fruit wet weight, dry weight, pH, and titratable acidity. Furthermore, as the PBZ doses increased, the internode length, and plant height showed a corresponding reduction. The findings of this study indicate that, in soilless tomato cultivation, foliar applications of PBZ produce superior results compared to soil applications. Additionally, no PBZ residue was detected in the fruit.
This study investigated the effects of foliar paclobutrazol (PBZ) applications at varying doses and intervals on the vegetative growth, yield, fruit quality, and residue accumulation in greenhouse-grown tomatoes. The experiment was conducted from April to November 2021 in a controlled greenhouse environment at Tokat Gaziosmanpaşa University, Türkiye. Indeterminate beef tomato cultivar Bellfort F₁ (Enza Zaden) was used in the study. PBZ was applied foliarly at concentrations of 10, 20, and 40 mg/L at 7-day and 14-day intervals. Results indicated that PBZ significantly reduced plant height and internode length, with the most compact plants observed under the 40 mg/L 14-day treatment. However, yield-related parameters responded more favorably to lower PBZ doses. The highest marketable yield (175.59 t/ha) and total yield (178.27 t/ha) were obtained under the 10 mg/L 14-day treatment, which also supported greater fruit number and higher dry matter content. Moderate PBZ doses improved fruit weight and chlorophyll index, whereas higher doses tended to suppress yield and quality. While fruit soluble solids and titratable acidity were not significantly affected, slight improvements were noted under moderate PBZ treatments. Importantly, no PBZ residues were detected in fruit samples. These findings demonstrate that foliar PBZ application at low doses is effective for controlling vegetative growth without compromising fruit quality or leaving detectable residues. The results support the use of foliar PBZ as a safe and practical growth regulation strategy for high-density tomato production under greenhouse conditions.
In pesticide residue trials, selecting crop varieties that accurately represent agricultural practices and morphological diversity is essential to obtaining reliable and applicable results. Generally, widely grown varieties are given priority, but differences in pesticide residues may occur due to the morphological and physiological characteristics of plant varieties. This study investigated the degradation behaviors of pirimicarb in five pepper varieties in Tokat, Türkiye, in 2023. Pirimicarb, an insecticide registered against the peach aphid Myzus persicae (Sulzer, 1776) (Hemiptera: Aphididae), is widely used in peppers, tomatoes, sugar beets, and citrus fruits. While effective in pest control, pirimicarb inhibits acetylcholinesterase, posing neurotoxic risks to target and non-target organisms. Prolonged exposure may cause endocrine disruption and oxidative stress, making residue monitoring essential for food safety. Initially, a rapid and sensitive QuEChERS-LC-MS/MS method was verified to analyze pirimicarb in peppers. Analysis results show that pirimicarb in all varieties decreased below EU-MRL (0.5 mg kg-1) 24 hours after application. Significant variations in degradation rates and half-lives were observed among the varieties, attributed to their morphological and physiological differences. This research fills a critical gap by revealing the impact of varietal differences on the fate of pesticides, providing valuable data to optimize application strategies and ensure consumer safety.
Pepper, Capsicum annuum L. (Solanales: Solanaceae) production is widely cultivated worldwide, with Türkiye ranks third in global pepper production. However, pests in pepper cultivation often necessitate pesticide use, leading to concerns about pesticide residue levels and their potential impact on food safety. This study investigated the dissipation behavior of lufenuron in pepper under field conditions in Tokat, Türkiye in 2022. Liquid chromatography-tandem mass spectrometry coupled with the quick, easy, cheap, effective, rugged, and safe technique was used to analyze residues of lufenuron in pepper. The average recoveries varied from 77% to 97%, with relative standard deviations of 13% for lufenuron. Lufenuron residues administered as recommended dose and double dose degraded in pepper following a first-order kinetic model, with an estimated half-life (t1/2) of 4.33 and 6.42 days in Tokat, 6.80 and 7.45 days in Niksar, respectively. Furthermore, a health risk assessment was conducted, which showed that the chronic risk quotient for lufenuron was much lower than 1. The present results indicated that the health risks posed for consumers by the lufenuron residues were negligible at the recommended dosages.
The objective of this study was to evaluate the dissipation kinetics of deltamethrin, emamectin benzoate, and hexythiazox in grapes. The QuEChERS method was employed and validated for the precise determination of these three pesticides using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Excellent linearity was observed with regression coefficients exceeding 0.998. Notably, the limits of quantification (LOQ) were significantly lower than the maximum residue limits (MRLs) established for grapes by the European Union. The QuEChERS method l recovered 93.23% of the pesticides with an acceptable RSD of 5.35% (n = 180), demonstrating its suitability for quantifying them in grapes. Half-lives of deltamethrin, emamectin benzoate, and hexythiazox in grapes were 2.62-2.68 days, 8.15-7.30 days, and 3.24-4.01 days, respectively, for both single and double doses. Residues of all pesticides fell below the MRLs by the preharvest interval. This suggests that their application can be considered safe for grapes, ensuring both pest control and consumer safety.
This study aimed to detect insecticide, acaricide, and nematicide residues in 92 fresh and 50 dried fig samples collected from locations with intensive fig, Ficus carica L. (Rosales: Moraceae) production in Ayd & imath;n, T & uuml;rkiye in 2022. The analysis method was validated according to SANTE 11312/2021 guidelines. The recoveries ranged between 70% and 120%, with repeatability (RSDr) and within-laboratory reproducibility (RSDwR) <= 20% and expanded measurement uncertainties below 50% for all insecticides indicating satisfactory analytical performance. In total, 114 different insecticides were screened, revealing residues in 27 samples. Bifenazate was detected in 13 samples, etoxazole in 3 samples, spiromesifen in 5 samples, and both bifenazate and spiromesifen in 6 samples. No detectable residues were found in the dried fig samples. All samples in which bifenazate was detected were above the European Union Maximum Residue Limits (EU-MRL). Etoxazole and spiromesifen, unauthorized in figs, showed etoxazole residues above EUMRLs, while spiromesifen residues were below EU-MRLs. The acute and chronic health risk indices for the insecticides were found to be below 1, indicating low health risks associated with fig consumption. The risk assessment suggests that fig consumption is safe for consumers.
This study was performed to detect pesticide residues in almond. QuEChERS method was validated for determination of 270 pesticides by liquid chromatography-tandem mass spectrometry (LC–MS/MS) and gas chromatography-mass spectrometry (GC–MS). The method had a suitable linearity (R2 ≥ 0.99). Limit of detection (LOD) and limit of quantification (LOQ) were ranged from 0.28 to 3.00 µg kg−1 and 0.92 to 9.98 µg kg−1 respectively. Average recoveries varied from 70.03 % to 119.82 %. Repeatability and intra-laboratory reproducibility of the method, expressed as RSDs were between 1.65–19.15 % and 1.77–19.42 %, respectively. Expanded relative uncertainties ranged from 15.82 % to 46.58 %. Although minimal matrix effects were observed in the LC-MS/MS analysis, a strong matrix effects were detected in the GC–MS analysis. The validated method was used collected for the analysis of collected 90 samples from fifteen different provinces in Turkey. The data showed that all the studied samples did not contain pesticides above the LOD values.
In this study, pesticide residues in sauce manufactured from agricultural products were examined. A simultaneous multiresidue analysis for 260 pesticides in sauce samples was performed using liquid chromatography with tandem mass spectrometry (LC-MS/MS). The QuEChERS AOAC 2007.01 (quick, easy, cheap, effective, rugged, and safe) was selected as the most suitable protocol for routine determination of pesticide residues. In line with the SANTE/11312/2021 guideline two parameters were used as identification criteria: retention time (RT) with a tolerance of ± 0.1 min in relation to the RT of the analyte in matrix-matched calibration standard and ion ratio tolerance below 30%. The RT deviation in positive samples was always < 0.1 min, and the ion ratio tolerance was < 30%. A total 4 different pesticides were detected in 20 sauce samples. No active ingredient was found in 16 samples. The residue levels were between 10 and 94 µg kg. The residues of acetamiprid, ametoctradin, imazalil sulfate, and metalaxyl-M were below the European Union Maximum Residue Limits (EU-MRLs).