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Öğe A sensitive determination of lead by hydride generation integrated with micro-sampling gas–liquid separator-FAAS after preconcentration by NiFe2O4 nanoparticles(Nature Research, 2025) Ayyıldız, Merve Fırat; Bodur, Süleyman; Bakırdere, SezginIn the present study, dispersive solid phase extraction – hydride generation integrated with micro–sampling gas–liquid separator – flame atomic absorption spectrometry was proposed to determine lead in lake water samples taken in the Horseshoe Island, Antarctica. In scope of this study, microwave assisted NiFe2O4 nanoparticles were synthesized, and the characterization of nanoparticles were carried out by FT-IR, XRD and SEM. All influential parameters of dispersive solid phase extraction and hydride generation were optimized to enhance signal intensity belonging to the analyte. System analytical performance studies were performed, and limit of detection and limit of quantitation were calculated as 2.16 µg kg–1 and 7.19 µg kg–1, respectively. Recovery studies were conducted to the spiked lake water samples and two different calibration strategies were applied. Percent recovery results were calculated between 102.0 and 169.5% by external calibration strategy while matrix matching calibration strategy provided recovery results in the range of 78.8–142.9%. © The Author(s) 2025.Öğe A simple and efficient supramolecular solvent based liquid phase microextraction method for the preconcentration of nickel from dandelion tea samples before FAAS quantification, and the practicality and greenness assessment of developed method(Elsevier Inc., 2024) Kartoğlu, Bedrihan; Bodur, Süleyman; Gülhan Bakırdere, Emine; Bakırdere, SezginA sensitive, accurate and practical analytical method (supramolecular solvent based liquid phase microextraction – flame atomic absorption spectrometry (SUPRAS-LPME-FAAS) was developed for the determination of nickel in dandelion tea samples. All influential parameters of SUPRAS-LPME were optimized to attain low detection/quantification limits using a univariate optimization approach. Under the optimum SUPRAS-LPME-FAAS conditions, dynamic range, limit of detection (LOD) and limit of quantification (LOQ) were found to be 25.86–497.64 µg/kg, 8.20 µg/kg and 27.35 µg/kg, respectively. The detection power of FAAS system was augmented as 28-fold with the help of SUPRAS-LPME method. Recovery experiments were performed for the evaluation of the accuracy and the applicability of the SUPRAS-LPME-FAAS method and percent recovery results for the spiked dandelion tea samples were calculated between 86.0 and 131.8 % via matrix matching calibration strategy. Additionally, the practicality and greenness evaluations for the SUPRAS-LPME-FAAS method were carried out using BAGI and AGREEprep software, respectively. © 2024 Elsevier B.V.Öğe Combination of high performance liquid chromatography and flame atomic absorption spectrophotometry using a novel nebulizer interface supported T shaped slotted quartz tube for the determination of Vitamin B12(Elsevier Science, 2022) Erarpat, Sezin; Bodur, Süleyman; Günkara, Ömer Tahir; Bakırdere, SezginA novel nebulizer interface (NI) was proposed to combine high performance liquid chromatography (HPLC) and flame atomic absorption spectrophotometer (FAAS). A glass concentric nebulizer was linked to T-shaped slotted quartz tube (T-SQT) using a tubing to transfer the liquid solution eluted from the chromatographic system into the atomization region of FAAS system. T-SQT was also used to intensify the interaction of atoms with the hollow cathode lamp light. Vitamin B12 was selected as an analyte to show the applicability of the new hyphenated system. After optimizing some parameters such as mobile phase flow rate and pH, nebulizer gas flow rate, T-SQT height and injection volume, linear range for the analyte was determined between 4.7 and 92 mg/kg as Co. Limit of detection (LOD) and limit of quantitation (LOQ) for the HPLC-NI-T-SQT-FAAS system were calculated to be 1.6 and 5.3 mg/kg as Co, respectively. Recovery studies were also conducted to verify the accuracy and applicability of the developed method for vitamin tablets and excellent percent recovery results (~ 100%) with low standard deviation values were obtained when matrix-matching calibration strategy was performed for each vitamin tablet. A successful separation and detection of the analyte was achieved within 3.0 min that offers high sample throughput. Two different vitamin tablets were analyzed by the optimized hyphenated system. The developed method also provides low usage of sample solution in contrast to conventional nebulizer in the FAAS systemÖğe 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 copper at trace levels in fennel tea samples by flame atomic absorption spectrometry after the implementation of simultaneous complexation and supramolecular solvent based spraying assisted liquid phase microextraction(Academic press inc., 2025) Tutar, Bahar Karademir; Tutar, Ömer Faruk; Bodur, Süleyman; Derin, Yavuz; Tutar, Ahmet; Bakırdere, SezginA simple and efficient preconcentration method named as supramolecular solvent based spraying assisted liquid phase microextraction (SUPRAS-SA-LPME) was combined with a flame atomic absorption spectrometry (FAAS) for the determination of copper in fennel tea samples at trace levels. An alkanol (1-decanol)/THF based SUPRAS (containing complexation agent) was used as extraction solvent instead of traditional organic solvents for the first time in an SA-LPME process. Under the optimum conditions, system analytical performance of the developed method was evaluated, and limit of detection (LOD)/limit of quantitation (LOQ) values were recorded as 1.91/ 6.37 mu g kg-1. After the evaluation of system analytical performances, the enhancement in detection power/ calibration sensitivity was found to be 21.3/21.8 folds when the comparison of LOD values/calibration plot slopes of the FAAS and SUPRAS-SA-LPME-FAAS systems. The method applicability was tested for the fennel tea samples by spiking experiments, and acceptable recovery results (80.2% - 111.8%) were obtained for low, mid and high spiked concentration levels.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 A simple spray assisted extraction/preconcentration of cadmium from sunflower oil, olive oil and hazelnut oil samples prior to flame atomic absorption spectrometry determination(Academic Press Inc., 2023) Erarpat, Sezin; Bakırdere, Sezgin; Bodur, Süleyman; Tutar, Ömer FarukIn this study, an efficient and simple analytical approach for the preconcentration and extraction of cadmium from sunflower oil, olive oil and hazelnut oil samples using environmentally friendly, easy and efficient vortex assisted reverse phase spray-based fine droplet formation liquid phase microextraction (VA-RP-SFDF-LPME) prior to flame atomic absorption spectrometry (FAAS) measurement was proposed. Limit of detection (LOD)/limit of quantification (LOQ) values were calculated as 2.89/9.62 µg/kg, 2.00/6.68 µg/kg and 4.77/15.92 µg/kg for sunflower oil, olive oil and hazelnut oil, respectively. Recovery experiments were carried out for the evaluation of applicability and accuracy of the developed method. Satisfactory recovery results for hazelnut oil, olive oil and sunflower oil samples were recorded in the range of 92.8 – 111.9%, 96.6 – 108.2% and 90.0 – 105.7%, respectively. These results verified that the proposed method can be accurately applied to the hazelnut oil, olive oil and sunflower oil samples to qualify/quantify their cadmium content. © 2023 Elsevier Inc.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.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.
