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    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, Bulent
    The 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.
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    Determination of more than 500 Pesticide Residues in Hen Eggs by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) and Gas Chromatography-Tandem Mass Spectrometry (GC/MS/MS)
    (Korean Soc Food Science Animal Resources, 2021) Golge, Ozgur; Liman, Turan; Kabak, Bulent
    This study aims to validate a fast method of simultaneous analysis of 365 LC-amenable and 142 GC-amenable pesticides in hen eggs by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS), respectively, operating in multiple reaction monitoring (MRM) acquisition modes. The sample preparation was based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction. Key method performance parameters investigated were specificity, linearity, limit of quantification (LOQ), accuracy, precision and measurement uncertainty. The method was validated at two spiking levels (10 and 50 mu g/kg), and good recoveries (70%-120%) and relative standard deviations (RSDs) (<= 20) were achieved for 92.9% of LC-amenable and 86.6% of GC-amenable pesticide residues. The LOQs were <= 10 mu g/kg for 94.2% of LC-amenable and 92.3% of GC-amenable pesticides. The validated method was further applied to 100 egg samples from caged hens, and none of the pesticides was quantified.
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    Occurrence of deoxynivalenol and zearalenone in cereals and cereal products from Turkey
    (Elsevier Sci Ltd, 2020) Golge, Ozgur; Kabak, Bulent
    This report describes concentrations of deoxynivalenol (DON) and zearalenone (ZEA) in cereals and derived products collected in Turkey from 2015 to 2018. A total of 240 cereals and cereal products were analysed by high performance liquid chromatography coupled with photodiode array (HPLC-PDA) and fluorescence (HPLC-FLD) detectors. The analytical method performance was satisfactory, with limit of quantification (LOQ) values of 46.90-72.30 mu g kg(-1), and 3.50-3.70 mu g kg(-1) for DON and ZEA, respectively. Thirteen wheat (58-1092 mu g kg(-1)), two maize (313-331 mu g kg(-1)), three barley (138-973 mu g kg(-1)), seven paddy rice (136-256 mu g kg(-1)), three wheat flour (92-151 mu g kg(-1)), two biscuits (31.2-71.3 mu g kg(-1)) and only one pasta (49.3 mu g kg(-1)) contained DON, but levels were below the EU maximum level (ML). DON was not detected in bulgur and wheat bread. ZEA was found in two wheat, three maize, eleven paddy rice and two wheat flour with a mean middle bound ZEA level of 1.34, 28.0, 42.9, and 2.66 mu g kg(-1), respectively. Amongst the samples contaminated with ZEA, only one paddy rice exceeded EU ML of 100 mu g kg(-1). However, barley, bulgur, wheat bread, pasta and biscuit products did not contain ZEA.
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    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, Bulent
    Interest 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.
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    Quantification of pesticide residues in gherkins by liquid and gas chromatography coupled to tandem mass spectrometry
    (Academic Press Inc Elsevier Science, 2021) Golge, Ozgur; Cinpolat, Seren; Kabak, Bulent
    The monitoring of pesticide residues in fruits and vegetables is a great concern in public health and international trade. This study aims to assess the incidence and quantification of pesticides in gherkins cultivated in Turkey. The sample preparation was based on QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction. The residues were determined by in-house validated methods based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS). This study included 109 pesticide residues, of which 85 were analysed by LC-MS/MS, and 24 were analysed by GC-MS/MS. Key method performance parameters investigated were linearity, limit of quantification (LOQ), accuracy, precision and measurement uncertainty. The LOQs ranged from 0.002 to 0.005 mg kg(-1). Of the 203 gherkin samples analysed, 57.6 % were free from the detectable level of residues. In 42.4 % of the samples, 15 different residues were found in measurable levels, of which 5 were non-approved in EU. Multiple pesticide residues were recorded in 17.2 % of the samples. In 7.9 % of the gherkin samples, the residue levels exceeded the maximum residue levels (MRLs). Among the residues, chlorothalonil (detected in 32 % of the samples), acetamiprid (16.3 %) and metalaxyl (and its enantiomer metalaxyl-M) (4.9 %) were the most frequently quantified pesticides.