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Öğe Assessment of external calibration, internal standard calibration and quadruple isotope dilution strategies for the determination of acrylamide in wastewater samples after LC-MS/MS quantification(Elsevier, 2023) Yazici, Elif; Bodur, Suleyman; Erarpat, Sezin; Arslan, Ulas Emre; Bakirdere, SezginAcrylamide is a possible neurotoxicant and carcinogen compound and its common usage in various industrial processes causes acrylamide contamination in environmental bodies. For this purpose, there is an increasing demand to develop an accurate and selective analytical method for the determination of acrylamide. In the scope of this study, external calibration (EC), internal standard calibration (ISC) and quadruple isotope dilution (ID4) strategies were compared to each other in terms of accuracy and precision. After the evaluation of these methods, liquid chromatography - quadruple isotope dilution - tandem mass spectrometry (LC-ID4-MS/MS) as a highly accurate and precise analytical approach was proposed to quantify acrylamide in wastewater samples. Several parameters for LC system such as sample injection volume, mobile phase type/composition and mobile phase flow rate were elaborately optimized to enhance peak shape and signal to noise ratio (S/N) belonging to the analyte. Under the optimum chromatographic and mass determination conditions, system analytical perfor-mance study was performed to determine dynamic range and limit of detection/quantitation (LOD and LOQ). LOD and LOQ values of the proposed LC-MS/MS method for the analyte were calculated as 1.18 and 3.93 mu g/kg; respectively. After the system analytical performance study, the spiking experiments in wastewater samples were carried out for the evaluation of accuracy and applicability of LC-MS/MS method. For wastewater samples, percent recovery results with their percent relative standard deviations (%RSD) obtained from EC, ISC and ID4 strategies were 115.8-177.8% (+/- 1.2-11.4%), 94.5-117.7% (0.3-4.7%) and 99.6-100.9% (0.4-1.7%); respec-tively. These results prove the superiority of ID4 strategy with regards to accuracy and precision of the results.Öğe Cadmium determination at trace levels in lake water samples by cold vapor generation-atomic absorption spectrometry after magnetic dispersive solid phase extraction(Springer Int Publ Ag, 2023) Bodur, Suleyman; Erarpat, Sezin; Kayin, Inci; Bakirdere, SezginThis study established an analytical method based on manganese ferrite based magnetic dispersive solid phase extraction (MDSPE) before cold vapor generation-atomic absorption spectrometry (CVG-AAS) for the determination of cadmium at trace levels in lake water samples collected from Horseshoe Island, Antarctica. Manganese ferrite nanoparticles were synthesized to be used as an adsorbent in the MDSPE method. Different MDSPE and CVG parameters were fixed to their optimum values after univariate optimization approach. Under the optimum conditions, analytical performance of the developed MDSPE-CVG-AAS method was evaluated and its applicability/accuracy was determined by recovery experiments. Twelve different lake water samples collected from Horseshoe Island, Antarctica were analyzed. Matrix matching calibration strategy was used to eliminate possible matrix effects arising from the lake water samples. Good recovery results (93.2-112.5%) were obtained from the spiked samples that indicated the method suitability to real samples.Öğe Deep eutectic solvents for the determination of endocrine disrupting chemicals(Elsevier, 2024) Chormey, Dotse Selali; Zaman, Buse Tugba; Kustanto, Tulay Borahan; Bodur, Sezin Erarpat; Bodur, Suleyman; Er, Elif Ozturk; Bakirdere, SezginThe harmful effects of endocrine disrupting chemicals (EDCs) to humans and other organisms in the environment have been well established over the years, and more studies are ongoing to classify other chemicals that have the potential to alter or disrupt the regular function of the endocrine system. In addition to toxicological studies, analytical detection systems are progressively being improved to facilitate accurate determination of EDCs in biological, environmental and food samples. Recent microextraction methods have focused on the use of green chemicals that are safe for analytical applications, and present very low or no toxicity upon disposal. Deep eutectic solvents (DESs) have emerged as one of the viable alternatives to the conventional hazardous solvents, and their unique properties make them very useful in different applications. Notably, the use of renewable sources to prepare DESs leads to highly biodegradable products that mitigate negative ecological impacts. This review presents an overview of both organic and inorganic EDCs and their ramifications on human health. It also presents the fundamental principles of liquid phase and solid phase microextraction methods, and gives a comprehensive account of the use of DESs for the determination of EDCs in various samples.Öğe Determination of copper in rose tea samples using flame atomic absorption spectrometry after emulsification liquid-liquid microextraction(Elsevier Sci Ltd, 2024) Kartoglu, Bedrihan; Bodur, Suleyman; Zeydanli, Damla; Gover, Tugce; Ozaydin, Ecem; Bakirdere, Emine Gulhan; Bakirdere, SezginRose tea infusion has gained popularity worldwide due to its health benefits. However, it is known that tea plants can be contaminated with heavy metals including copper. Hence, an accurate and applicable analytical method namely emulsification liquid-liquid microextraction based deep eutectic solvent - flame atomic absorption spectrometry (ELLME-DES-FAAS) was proposed to determine copper at trace levels in rose tea samples. Under the optimum experimental conditions, analytical figures of merit for the developed method were examined, and dynamic range, limit of detection (LOD) and limit of quantification (LOQ) were found to be 5.07-246.61 mu g/kg (mass-based) with 0.9992 coefficient of determination, 2.50 mu g/kg and 8.32 mu g/kg, respectively. A matrix matching calibration strategy was employed to boost recovery results, and the acceptable recovery results were recorded between 95.9 % and 118.4 %. According to recovery results, the developed analytical method can be safely employed to determine the concentration of copper in rose tea samples accurately.Öğe Determination of phenytoin at trace levels in domestic wastewater and synthetic urine samples by gas chromatography-mass spectrometry after its preconcentration by simple liquid-phase microextraction(Springer, 2024) Bodur, Sezin Erarpat; Ayan, Gizem Nur; Bodur, Suleyman; Gunkara, Omer Tahir; Bakirdere, SezginThis work presents a sensitive and accurate analytical method for the determination of phenytoin at trace levels in domestic wastewater and synthetic urine samples by gas chromatography-mass spectrometry (GC-MS) after the metal sieve-linked double syringe liquid-phase microextraction (MSLDS-LPME) method. A metal sieve was produced in our laboratory in order to disperse water-immiscible extraction solvents into aqueous media. Univariate optimization studies for the selection of proper extraction solvent, extraction solvent volume, mixing cycle, and initial sample volume were carried out. Under the optimum MSLDS-LPME conditions, mass-based dynamic range, limit of quantitation (LOQ), limit of detection (LOD), and percent relative standard deviation (%RSD) for the lowest concentration in calibration plot were figured out to be 100.5-10964.2 mu g kg-1, 150.6 mu g kg-1, 45.2 mu g kg-1, and 9.4%, respectively. Detection power was improved as 187.7-folds by the developed MSLDS-LPME-GC-MS system while enhancement in calibration sensitivity was recorded as 188.0-folds. In the final step of this study, the accuracy and applicability of the proposed system were tested by matrix matching calibration strategy. Percent recovery results for domestic wastewater and synthetic urine samples were calculated as 95.6-110.3% and 91.7-106.6%, respectively. These results proved the accuracy and applicability of the proposed preconcentration method, and the obtained analytical results showed the efficiency of the lab-made metal sieve apparatus.Öğe Synthesis of Isotopic Labelled Paracetamol Benzoate-d3 and Its Application in the Determination of Paracetamol(Wiley-V C H Verlag Gmbh, 2023) Demirel, Rabia; Erarpat, Sezin; Bodur, Suleyman; Gunkara, Omer Tahir; Bakirdere, Sezgin; Turak, FatmaThis study proposed a precise/accurate analytical method for the paracetamol (PCT) determination in human serum/urine matrices. PCT was simultaneously derivatized and preconcentrated by dispersive liquid-liquid microextraction (DLLME). Benzoyl chloride dissolved in dichloromethane was used as derivatization agent in the extraction solvent. Quadruple isotope dilution (QID) method with three calibration mixtures (A*B-x, x=1,2,3) and one sample mixture (AB) was performed to enhance the method accuracy and precision. In our research laboratory, paracetamol benzoate-d3 (PCT benzoate-d3) was synthesized and used as isotopically labelled substance (B) to conduct QID method. After the combination of QID and DLLME-GC-MS systems, percent recovery results for human serum/urine matrices were found to be 99.3-101.0 % and 98.8-99.9 %, respectively.