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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 capsaicin at trace levels in different food, biological and environmental samples by quadruple isotope dilution-gas chromatography mass spectrometry after its preconcentration(Elsevier, 2024) Bodur, Sezin Erarpat; Bodur, Süleyman; Ayyıldız, Merve Fırat; Günkara, Ömer Tahir; Dikmen, Yaren; Doru, Esra Sultan; Bakırdere, SezginDespite the therapeutic properties of capsaicin for some diseases, it shows some side effects for human health. The goal of this study was to develop a precise and accurate analytical strategy for the trace determination of capsaicin in different food, biological and environmental samples including pepper, saliva and wastewater by gas chromatography-mass spectrometry (GC-MS) after spraying-based fine droplet formation-liquid phase microextraction (SFDF-LPME) and quadruple isotope dilution (ID4) method. Acetic anhydride was used as derivatizing agent, and the extraction method was used to enrich the analyte derivative to reach low detection limits. Under the optimum conditions, limit of detection (LOD) and limit of quantitation (LOQ) were determined to be 0.33 and 1.10 mu g/kg, respectively. Percent recoveries calculated for SFDF-LPME-GC-MS method ranged between 84.1 and 131.7 %. After the application of ID4-SFDF-LPME-GC-MS method, percent recoveries were obtained in the range of 94.9 and 104.0 % (%RSD <= 2.8) for the selected samples. It is obvious that the isotope dilution-based method provided high accurate and precise results due to the elimination of errors during the derivatization, extraction and measurement steps.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 Development of dispersive solid phase extraction method for the preconcentration of parathion ethyl as a simulant of nerve agent sarin from soil, plant and water samples prior to GC-MS determination(SPRINGER, 27.08.2024) Bodur, Suleyman; Bodur, Sezin Erarpat; Tutar, Bahar Karademir; Bakirdere, Sezgin; Yagmuroglu, OzanIn the presented study, an efficient and fast analytical method was developed for the determination of parathion ethyl as sarin simulant by gas chromatography-mass spectrometry (GC-MS). Dispersive solid phase extraction (DSPE) was performed to concentrate parathion ethyl from soil, plant and water samples. Reduced graphene oxide-iron (II, III) oxide (rGO-Fe3O4) nanocomposite was used as an adsorbent to collect the target analyte from the aqueous sample solutions. After the optimization of extraction/preconcentration parameters, optimum conditions for adsorbent amount, eluent type, mixing type/period, eluent volume and initial sample volume were determined as 15 mg, acetonitrile, vortex/30 s, 100 mu L and 10 mL, respectively. Under the optimum conditions, analytical performance of the developed DSPE-GC-MS method was evaluated in terms of limit of detection (LOD), limit of quantitation (LOQ) and dynamic range. Dynamic range, LOD and LOQ values were figured out to be 0.94-235.15 mu g/kg, 0.41 mu g/kg and 1.36 mu g/kg (mass based), respectively. Satisfactory percent recovery results (90.3-125% for soil, 93.5-108.7% for plant, 88.5-112.9% for tap water) were achieved for soil, plant and tap water samples which proved the accuracy and applicability of the developed method. It is predicted that the DSPE-GC-MS method can be accurately used for the detection of sarin in soil, plant and water samples taken from war territories.Öğe Development of dispersive solid phase extraction method for the preconcentration of parathion ethyl as a simulant of nerve agent sarin from soil, plant and water samples prior to GC–MS determination(Springer Science and Business Media Deutschland GmbH, 2024) Bodur, Süleyman; Bodur, Sezin Erarpat; Tutar, Bahar Karademir; Bakırdere, Sezgin; Yağmuroğlu, OzanIn the presented study, an efficient and fast analytical method was developed for the determination of parathion ethyl as sarin simulant by gas chromatography–mass spectrometry (GC–MS). Dispersive solid phase extraction (DSPE) was performed to concentrate parathion ethyl from soil, plant and water samples. Reduced graphene oxide–iron (II, III) oxide (rGO-Fe3O4) nanocomposite was used as an adsorbent to collect the target analyte from the aqueous sample solutions. After the optimization of extraction/preconcentration parameters, optimum conditions for adsorbent amount, eluent type, mixing type/period, eluent volume and initial sample volume were determined as 15 mg, acetonitrile, vortex/30 s, 100 µL and 10 mL, respectively. Under the optimum conditions, analytical performance of the developed DSPE-GC–MS method was evaluated in terms of limit of detection (LOD), limit of quantitation (LOQ) and dynamic range. Dynamic range, LOD and LOQ values were figured out to be 0.94–235.15 µg/kg, 0.41 µg/kg and 1.36 µg/kg (mass based), respectively. Satisfactory percent recovery results (90.3–125% for soil, 93.5–108.7% for plant, 88.5–112.9% for tap water) were achieved for soil, plant and tap water samples which proved the accuracy and applicability of the developed method. It is predicted that the DSPE-GC–MS method can be accurately used for the detection of sarin in soil, plant and water samples taken from war territories. © The Author(s), under exclusive licence to Springer Nature Switzerland AG 2024.Öğe Dispersive solid phase extraction and quadruple isotope dilution–mass spectrometry combination for the accurate and sensitive quantification of capsaicin in pepper, domestic wastewater and human saliva samples by GC–MS system(Elsevier Inc., 2025) Bodur, Süleyman; Bodur, Sezin Erarpat; Gürsoy, Selim; Ayyıldız, Merve Fırat; Kartoğlu, Bedrihan; Akbıyık, Hilal; Günkara, Ömer Tahir; Bakırdere, SezginIn the presented study, reduced graphene oxide/Fe3O4 (rGO/Fe3O4) nanocomposites based dispersive solid phase extraction (DSPE) – gas chromatography–mass spectrometry (GC–MS) method was developed for the determination of capsaicin in domestic wastewater (DW), pepper (PP) and human saliva (HS) samples. All important parameters of the DSPE method affected the preconcentration factor were carefully optimized to achieve high signal to noise ratio for the analyte. After the optimization studies, the system analytical performance of DSPE-GC–MS system was evaluated using the aqueous standard solution of capsaicin. Limit of detection (LOD), limit of quantitation (LOQ) and dynamic range were figured out to be 0.54 µg/kg, 1.80 µg/kg and 2.66 – 487.35 µg/kg, respectively. Under the optimum experimental conditions, recovery studies were conducted with the spiked DW, PP and HS samples, and percent recovery results were recorded between 52.6 % and 183.6 % via matrix matching calibration strategy. After the implementation of ID4 strategy, percent recovery results for the spiked DW, PP and HS samples were calculated as 98.2 %–99.3 %, 99.7 %–100.7 % and 99.4 %–99.8 %, respectively. In addition, capsaicin content in Sivri (S)-PP, Kıl (K)-PP and Samandağ (SA)-PP samples were found to be 309.5 ± 11.8 mg/kg, 873.7 ± 26.7 mg/kg and 165.3 ± 5.1 mg/kg via DSPE-GC-ID4-MS method, respectively. As a result, the combination of quadruple isotope dilution (ID4) strategy and the DSPE-GC–MS method were successfully performed to boost the accuracy and precision of developed DSPE-GC–MS method. © 2024 Elsevier B.V.Öğe Trace element determination using mass spectrometry coupled detection methods(Elsevier B.V., 2025) Chormey, Dotse Selali; Er, Elif Öztürk; Bodur, Sezin Erarpat; Zaman, Buse Tuğba; Bodur, Süleyman; Kustanto, Tülay Borahan; Kayın, İnci; Bakırdere, SezginAbout half a century ago, trace elements in the environment were restricted at upper parts per billion levels due to limited information on their toxicological effects on humans and other organisms in the environment. In this present day, stricter restrictions are being enforced by several regulatory authorities to curb the continuous release of trace elements into the environment through anthropogenic activities that have resulted from the demand to meet the global population increase. The severity of health disorders related to trace elemental exposure from different sources and doses seem to overshadow their relevance for several biological functions. Thus, toxicological studies that elucidate the harmful effects of chemicals and help regulators to set limits of restriction require very sensitive analytical instruments that offer selectivity and specificity for accurate and precise determinations. Mass spectrometry is a unique technique that suits the purpose of identifying, confirming and quantifying elements that emanate from various chemical species. Inductively coupled plasma mass spectrometry is a superior analytical technique used for the simultaneous determination of trace elements in various samples. This superior technique is further augmented by solid phase and liquid phase microextraction methods, which help separate trace elements from complex matrices into clean, readable and enriched forms for the instrument. © 2024 Elsevier B.V.Öğe Trace element determination using mass spectrometry coupled detection methods(Elsevier b.v., 2025) Chormey, Dotse Selali; Er, Elif Öztürk; Bodur, Sezin Erarpat; Zaman, Buse Tuğba; Bodur, Süleyman; Kustanto, Tülay Borahan; Kayın, İnci; Bakırdere, SezginAbout half a century ago, trace elements in the environment were restricted at upper parts per billion levels due to limited information on their toxicological effects on humans and other organisms in the environment. In this present day, stricter restrictions are being enforced by several regulatory authorities to curb the continuous release of trace elements into the environment through anthropogenic activities that have resulted from the demand to meet the global population increase. The severity of health disorders related to trace elemental exposure from different sources and doses seem to overshadow their relevance for several biological functions. Thus, toxicological studies that elucidate the harmful effects of chemicals and help regulators to set limits of restriction require very sensitive analytical instruments that offer selectivity and specificity for accurate and precise determinations. Mass spectrometry is a unique technique that suits the purpose of identifying, confirming and quantifying elements that emanate from various chemical species. Inductively coupled plasma mass spectrometry is a superior analytical technique used for the simultaneous determination of trace elements in various samples. This superior technique is further augmented by solid phase and liquid phase microextraction methods, which help separate trace elements from complex matrices into clean, readable and enriched forms for the instrument.
