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Öğe Combination of homogeneous liquid-liquid extraction and vortex assisted dispersive liquid-liquid microextraction for the extraction and analysis of ochratoxin A in dried fruit samples: Central composite design optimization(Academic Press Inc Elsevier Science, 2023) Elik, Adil; Ablak, Ozlem; Ul Haq, Hameed; Boczkaj, Grzegorz; Altunay, NailThis paper presents a new analytical procedure based on combination of homogeneous liquid-liquid extraction (HLLE) and vortex-assisted dispersive liquid-liquid microextraction (VA-DLLME) for the accurate and reliable determination of ochratoxin A (OTA) in dried fruit samples. To enable selective extraction of the OTA, six hydrophobic deep eutectic solvents (hDESs) were prepared and tested as extraction solvents. Optimization of DES volume, pH, NaCl amount, and mixing time affecting the efficiency of VA-DES-DLLME step was achieved by central composite design (CCD). Using optimized conditions, the working range was obtained in the range 0.4-350 ng mL-1 with an enrichment factor of 138. The limit of detection was 0.12 ng mL-1. To evaluate the accuracy of the method, the samples were analyzed with both the HLLE-VA-DES-DLLME procedure and reference method. The precision of the method was investigated by intraday/interday studies. The robustness of the method was also evaluated by making minor changes to the optimized conditions. The HLLE-VA-DES-DLLME procedure was successfully applied to dried fruit samples and quantitative recoveries were obtained (92.1-99.2%) confirming its usefulness for implementation in routine analysis of food samples.Öğe Development of a vortex-assisted switchable-hydrophilicity solvent-based liquid phase microextraction for fast and reliable extraction of Zn (II), Fe (II), Pb (II), and Cd (II) from various baby food products(Elsevier Sci Ltd, 2024) Ul Haq, Hameed; Elik, Adil; Isci, Gursel; Ekici, Merve; Gursoy, Nevcihan; Boczkaj, Grzegorz; Altunay, NailThis manuscript describes the development of a novel liquid phase microextraction (LPME) method for the extraction and determination of Zn (II), Fe (II), Pb (II), and Cd (II) in various infant/baby food and supplements products. The method is based on vortex -assisted extraction combined with a switchable-hydrophilicity solvent (SHS) sample preparation. The SHS, which undergoes reversible phase changes triggered by pH change, enables selective extraction and easy phase separation. A flame atomic absorption spectroscopy was used in the final determination step. Optimization studies revealed, that the optimal pH of the sample solution (after digestion) during analytes extraction is 5.5. A L-proline is added to the sample (375 mM) to ensure the complexation of the target metal cations. After the complexation step, 750 mu L of SHS - a N, N-Dimethylcyclohexylamine along with 0.9 mL of 2 M of acetic acid solution is added (hydrophilicity switch -on stage) and mixed manually to obtain a homogeneous solution. In the last stage, 0.45 mL of 10 M NaOH solution (hydrophilicity switch -off stage) is added to the sample solution and a vortex for 100 s is applied to ensure the effective extraction and separation of the complex containing the analytes. At this stage, a cloudy solution is immediately obtained. Finally, the effective phase separation is obtained at the centrifugation step (4000 rpm for 2 mins). The method limit of detection was as 0.03, 0.009, 0.6, and 0.2 ng/L for Zn (II), Fe (II), Cd (II), and Pb (II) respectively with RSD% below 2.0 %. The analysis of certified reference materials and real samples proved the full applicability of the method for routine analysis, contributing to the field of heavy metal analysis and ensuring the safety of baby products. According to the AGREE methodology, this method can be named as green analytical chemistry method with a score of 0.77.Öğe Development of an orbital shaker-assisted fatty acid-based switchable solvent microextraction procedure for rapid and green extraction of amoxicillin from complex matrices: Central composite design(Elsevier Sci Ltd, 2024) Elik, Adil; Demirkol, Yagmur; Ul Haq, Hameed; Boczkaj, Grzegorz; Sanaullah; Altunay, NailIn this study, a cheap, fast and simple orbital shaker-assisted fatty acid-based switchable solvent microextraction (OS -FASS -ME) procedure was developed for the extraction of amoxicillin (AMOX) in dairy products, pharmaceutical samples and wastewater prior to its spectrophotometric analysis. Fatty acid-based switchable solvents were investigated for extracting AMOX. The key factors of the OS -FASS -ME procedure were optimized using a central composite design. The linearity of OS -FASS -ME procedure was in the range 5 -600 ng mL -1 with a correlation coefficient of 0.991. In five replicate experiments for 20 ng mL -1 of AMOX solution, the recovery and relative standard deviation were 95.8% and 2.2%, respectively. Limits of detection and quantification were found 1.5 ng mL -1 and 5 ng mL -1 , respectively. The accuracy, precision, robustness and selectivity of the OSFASS -ME procedure were investigated in detail under optimum conditions. The OS -FASS -ME procedure was applied to milk, cheese, wastewater, syrups and tablets. A comparison of the results obtained from the reference method and the OS -FASS -ME method showed that the OS -FASS -ME procedure can be successfully applied to complex matrices.Öğe Investigation of vortex assisted magnetic deep eutectic solvent based dispersive liquid-liquid microextraction for separation and determination of vanadium from water and food matrices: Multivariate analysis(Elsevier, 2024) Altunay, Nail; Lanjwani, Muhammad Farooque; Tuzen, Mustafa; Boczkaj, GrzegorzA new and simple vortex assisted magnetic deep eutectic solvent dispersive liquid-liquid microextraction procedure (VA-MDES-DLLME) was developed for the determination of vanadium (V) in food and water samples by flame atomic absorption spectrometry (FAAS). In the extraction medium, a bis(acetylpivalylmethane) ethylenediimine (H2APM2en) was used for the complexation of V(V) in sample solution at pH 6. The VA-MDESDLLME was optimized by different operation parameters, pH level of solution, MDESs volume, vortex time, concentration of complexing agent and samples volume. The accuracy of VA-MDES-DLLME was confirmed by analysis of certified reference materials (CRMs) and standard additional method in respect to real samples. The detection limit, quantification limit and enhancement factor were found 0.3, 1.0 ng mL-1 and 120, respectively. The linearity was confirmed for wide concentration range from 1 to 600 ng mL-1 and relative standard deviation (RSD) is 2.8 %. The multivariate statistical analysis was used for factorial design to explore the effects of extraction parameters on recovery of V(V) and also significant level of variables.Öğe Magnetic deep eutectic solvents for vortex-assisted liquid phase microextraction method for selective and green extraction of patulin from fruits and fruit juices(Elsevier, 2025) Ul Haq, Hameed; Boczkaj, Grzegorz; Altunay, NailIn this study, a vortex assisted magnetic deep eutectic solvent based liquid phase microextraction (VA-MDESLPME) technique was developed for the extraction of patulin prior to its determination by ultraviolet-visible spectrophotometry (UV-Vis). For this purpose, the use of a magnetic deep eutectic solvent (MDES) consisting of trihexyltetradecylphosphonium chloride, MnCl2, and octanoic acid (molar ratio 1:2:2) was tested to perform an efficient extraction. Important experimental parameters (MDES-3 vol, pH, vortex time, and ethanol volume) were optimized using Box-Behnken Design. Under optimum conditions (MDES-3 vol 560 mu L, pH 3.5, vortex time 300 s, and ethanol volume 300 mu L), the limits of detection for the model solution and matrix-matched solution were 0.06 ng mL- 1 and 0.37 ng mL- 1, and the calibration ranges were 0.2-400 ng mL- 1 and 1.2-300 ng mL- 1, respectively. Furthermore, the extraction recovery was calculated to be 96.3-97.4 % with a low relative standard deviation (2.1-2.5 %). The VA-MDES-LPME technique was successfully applied for the determination of patulin from fruit and juice samples with an enrichment factor between169 and 185.Öğe Magnetic hydrophobic deep eutectic solvents for orbital shaker-assisted dispersive liquid-liquid microextraction (MAGDES-OS-DLLME)- Determination of nickel and copper in food and water samples by FAAS(Academic Press Inc Elsevier Science, 2024) Elik, Adil; Ul Haq, Hameed; Boczkaj, Grzegorz; Fesliyan, Seckin; Ablak, Ozlem; Altunay, NailIn this work, a cheap and widely applicable dispersive liquid-liquid microextraction (DLLME) method was developed for the extraction of Ni(II) and Cu(II) from water and food samples and analysis using flame atomic absorption spectrometry. DLLME was assisted by orbital shaker, while ferrofluid as an extractant was based on deep eutectic solvent (DES). This ferrofluid was made of hydrophobic DES (hDES), composed of lauric acid and menthol (molar ratio 1:2), and toner powder@aliquat 336 magnetic particles. The extraction procedure does not require any heating or centrifugation. The method limits of detection value were 0.15 mu g L-1 and 0.03 mu g L-1 for Ni(II) and Cu(II) respectively along with wide linearity range (0.4-250 mu g L-1). The validation of the method was performed using certified reference materials (CRMs). The studies revealed excellent accuracy between results obtained by the developed method and expected values for all CRMs. The relative recoveries of Ni(II) and Cu(II) ions ranged from 92.8% to 98.6%. The developed method was further used for the determination of Ni(II) and Cu (II) in real water and food samples and provided quantitative recoveries.Öğe Optimization of vortex-assisted supramolecular solvent-based liquid liquid microextraction for the determination of mercury in real water and food samples(Academic Press Inc., 2024) Lanjwani, Muhammad Farooque; Elik, Adil; Altunay, Ayşenur Öztürk; Tuzen, Mustafa; Haq, Hameed Ul; Boczkaj, GrzegorzA novel method was developed for sample preparation for spectrophotometric determination of Hg(II) in water and food samples. The method was based on vortex-assisted supramolecular solvent-assisted liquid-liquid microextraction (VA-SUPRASs-LLME). Analytical parameters such as pH, chelating agent, solvent type and volume, vortex time and salting out effect were optimized. Surface and normal probability plots were drawn for the variables using the optimization data. Microwave-assisted digestion of samples was performed before the extraction procedure. L-cysteine was found to be more effective as a ligand for Hg(II). Five different SUPRASs were prepared and used for the extraction of Hg(II). A 1-decylamine/thymol/water at a 1:2:1 molar ratio assisted by a salting effect was found most effective for optimal extraction. Limits of detection and limit of quantification were found 0.6 ?g L?1 and 2.0 ?g L?1 with a very good linearity range of 2–350 ?g L?1. Intra-day and inter-day precisions were in the range of 1.8–4.0 % with a preconcentration factor 150. The accuracy of the method estimated by analysis of certified reference materials was 96–98.5 %. Finally, the new method was used for the determination of Hg(II) in real water, food samples, and certified reference materials (NIST, IAEQ/W-4(simulated freshwater), and DORM-4; fish protein). © 2024 Elsevier Inc.Öğe Quality control of cheese samples for the presence of natamycin preservative - A natural deep eutectic solvent (NADES) based extraction coupled with HPLC(Academic Press Inc Elsevier Science, 2024) Ul Haq, Hameed; Altunay, Nail; Tuzen, Mustafa; Boczkaj, GrzegorzA new protocol for the determination of natamycin - an antifungal agent used as a food preservative - in cheese samples - is described. This new method is based on a natural deep eutectic solvent (NADES) green extraction procedure. High-performance liquid chromatography (HPLC) was used for detection and quantification. NADESs with different molar ratios were evaluated for efficient and selective extraction. NADES made of thymol and nonanoic acid (1:1) revealed to be the best extracting solvent. All significant analytical parameters - pH, temperature, NADES volume, time for sonication were optimized using Plackett-Burman (PB) and central composite design (CCD) - response surface methodology (RSM). Optimum conditions for extraction were pH 7, temperature 25 degrees C, NADES volume 4.5 mL for 20 mL sample, and sonication time 10 mins. The developed method has a satisfactory linearity of 2-80.4 mg/kg, limits of detections (LOD), and limit of quantification (LOQ) of 0.45 and 1.45 mg/kg respectively. Under optimized conditions, the sample preparation procedure takes 12 mins. The method was found selective due to the unique and representative features of DESs. Furthermore, the extracts are analyzed by HPLC which provides a second very effective separation step, assuring the selectivity of the method. Validation of the method confirms the robustness and reproducibility of the NADES-based extraction coupled with the HPLC method demonstrating the effectiveness of NADES. The findings of this work contribute to the field of food safety and quality control, offering a novel and efficient approach to the detection of natamycin in cheese samples.Öğe Spectrophotometric determination of chlorpyrifos in foodstuffs after vortex-assisted surfactant-enhanced emulsification microextraction using magnetic deep eutectic solvents: Analytical greenness profile(Academic Press Inc Elsevier Science, 2025) Altunay, Nail; Elik, Adil; Ul Haq, Hameed; Boczkaj, GrzegorzIn this work a novel and green vortex-assisted surfactant-enhanced emulsification microextraction (VA-SEEME) based on magnetic deep eutectic solvents (MDESs) was developed for the determination of chlorpyrifos in foodstuffs by UV-Vis spectrophotometric analysis. MDES (trihexyltetradecylphosphonium chloride: MnCl2: octanoic acid) was used as the extractant, non-ionic surfactant Tween-80 was used as an extraction medium, and ethanol as the eluent solvent. In the VA-MDES-SEEME procedure, a vortex was applied for agitation, and a neodymium magnet was used to separate the MDES from the aqueous solution. Under optimized conditions, a linear dynamic range was obtained in the range of 0.3-260 mu g L- 1 with a detection limit of 0.09 mu g L- 1. The intraday and interday precisions of the method, defined as relative standard deviation, ranged from 1.3 % to 2.5 %. The recovery of the spiked sample after the VA-MDES-SEEME procedure ranged from 88+6 % to 98+1 %, and the enrichment factor was obtained as 91-fold. The VA-MDES-SEEME procedure was validated by analysis of the certified reference materials including 7507a-Green Onion and 7508a-Cabbage. The VA-MDES-SEEME procedure is based on inexpensive equipment and green chemicals and is compatible with UV-Vis spectrophotometer analysis. The green profile of the VA-MDES-SEEME procedure within the scope of the current study was calculated as 0.71 using AGREE.Öğe Synthesis, characterization and application of cross-linked functional terpolymer through epoxy group as sorbent for extraction of cadmium from waters and foods: Multivariate optimization(Elsevier Sci Ltd, 2024) Yilmaz, Ersen; Boztug, Ali; Ul Haq, Hameed; Boczkaj, Grzegorz; Altunay, NailThe purpose of this study was to develop a selective sorbent for cadmium ions (Cd(II)) enrichment in orbital shaker assisted solid phase microextraction (OS-SPME) from different aqueous and food samples. A maleic anhydride-styrene-glycidyl methacrylate (MA-St-GMA) terpolymer was synthesized and characterized in detail. Experimental variables of sample preparation step were optimized using a central composite design (CCD). The final determination step was performed using flame atomic absorption spectroscopy (FAAS). The MA-St-GMA sorbent exhibited a high adsorption capacity (195.9 mg g-1) for the Cd(II) ion. The developed method under optimal conditions provides satisfactory performance and a significant improvement compared to other protocols available in the literature. The linear range and detection limit of the method is 0.1-130 ng mL-1 and 0.03 ng mL-1, respectively. The robustness, intraday/interday precision, selectivity, and accuracy of the method were investigated. To further validate the method, a dedicated series of analysis was performed using certified reference materials (CRMs). This part of the study confirmed the applicability of the method for routine analysis. The OS-SPME-FAAS method was validated using water and food samples. Relative standard deviations and recovery for real-world samples were in ranges 1.7-2.2 % and 95.5-98.5 %, respectively. As a result, the MA-StGMA sorbent showed that it could quantitatively extract Cd(II) ions from aqueous solution.
