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Covalent Organic Frameworks, a Renewable and Emergent Source for the Separation and Pre-concentration of the Traces of Targeted Species
(Elsevier, 2023) Jagirani, Muhammad Saqaf; Gumus, Z. Pinar; Soylak, Mustafa
Covalent organic frameworks (COFs) are the emerging class of porous materials that are associated with covalent bonds. Due to the unique characteristics such as total organic backbone, large specific surface three-dimensional structures, highly porous in nature multiple functionalities, excellent adsorptive efficiency high flexibility in structure. Due to their extraordinary characteristics, COFs are employed in different areas, such as catalysts, sensors, separation, and preconcentration processes. Along with the development in COFs-based materials, scientific gaps remain due to the limited literature. COFs-based materials need more attention to improve the analytical efficacy as well as in the availability of literature. The limited literature source may cause a lack of improvement in the field of COFs and their applications in the separation and pre-concentration of traces of targeted species. This review focuses on the assessment and development of COFs-based materials and different applications.
Determination of Atrazine in Food, Water, and Synthetic Urine by Activated Carbon Cloth (ACC) Micro-Solid-Phase Extraction (mu SPE) with High-Performance Liquid Chromatography - Diode Array Detection (HPLC-DAD)
(Taylor & Francis Inc, 2023) Ahmed, Hassan Elzain Hassan; Gumus, Zinar Pinar; Soylak, Mustafa
Activated carbon cloth (ACC) was used as a micro solid phase extraction (mu SPE) sorbent for the separation-preconcentration and determination of atrazine in water, juice, spice, and artificial urine by high-performance liquid chromatography-diode array detector (HPLC-DAD). The adsorbent mass was 10mg, the adsorption-desorption duration was 90-s, and the proposed method can be applied to different matrices. The preconcentration factor of the method is 16.7. The limit of detection (LOD) and limit of quantification (LOQ) were 0.7 and 2.2 ng mL(-1), respectively. The recovery values of the presented procedure were from 93 to 108% for real samples. This mu SPE-HPLC-DAD protocol is practical and sensitive for atrazine and shows that activated carbon cloth is a highly effective adsorbent.
Dispersive-solid phase extraction of diniconazole from water and fruit juice samples using MnCoCu-LDHs@MOF-235 nanocomposite
(Elsevier, 2024) Salamat, Qamar; Ahmed, Hassan Elzain Hassan; Gumus, Zinar Pinar; Soylak, Mustafa
In this study, a new, affordable, and promising adsorbent based on MnCoCu-LDHs@MOF-235(Fe) nanocomposite was successfully synthesized, characterized, and utilized for the solid phase extraction of diniconazole (DNC) pesticide from water and food samples before it was determined by liquid chromatography. The structural characteristics of the synthesized nanocomposite were confirmed by various techniques, including FTIR, XRD, FE-SEM, and FE-SEM-EDX. The central composite design (CCD) technique was used for multi-response optimization of effective parameters including the sample solution's pH (6.0), adsorbent amount (15 mg), adsorption time (5 min), sample volume (30 mL) and eluent volume (2.5 mL), and desorption time (3 min) to achieve optimum extraction efficiency. Under optimal conditions, the method's analytical performance was assessed. The results showed that the calibration graphs showed linearity for DNC in the range of 1.3-500 mu g L- 1, with a detection limit of 0.4 mu g L- 1 and a correlation coefficient of 0.9988. Additionally, 2.9 intra-day RSD, 6.1 interday RSD, 12.0 preconcentration factor, and 2.53-11.53 enrichment factors was attained. The performance of the method to extract DNC from nine different real samples was realized with high relative recoveries (88.0-108 %). In addition, the greenness of the method was assessed with the AGREE metric tool, confirming that the method is environmentally friendly.
Electrochemical immunosensor for rapid and highly sensitive detection of SARS-CoV-2 antigen in the nasal sample
(Elsevier, 2022) Mehmandoust, Mohammad; Gumus, Z. Pinar; Soylak, Mustafa; Erk, Nevin
A label-free electrochemical biosensing approach as an appropriate analysis technique for SARS-CoV-2 spike protein (SARS-CoV-2 S-protein) was investigated to facilitate the diagnosis of coronavirus in real samples. It is crucial to construct diagnostic features that can rapidly identify infected individuals to limit the spread of the virus and assign treatment choices. Therefore, a novel and selective method using SiO2@UiO-66 and a label-free electrochemical immunoassay for rapidly detecting spike protein. The development of innovative approaches for direct viral detection employing simplified and ideally reagent-free assays is a pressing and difficult topic. The absence of speedy and effective ways to diagnose viral diseases especially SARS-CoV-2 on demand has worsened the issue of combating the COVID-19 pandemic. The developed electrode illustrated a wide dynamic range of 100.0 fg mL(-1) to 10.0 ng mL(-1) with low limit detection. Therefore, the as-fabricated electrochemical SARS-CoV2 S-protein sensor suggests an appropriate perspective in the point-of-care system, within 5.0 min, in nasal samples with satisfactory recovery.
Magnetic solid-phase extraction of atrazine with ACC@NiCo2O4@Fe3O4 nanocomposite in spice and water samples
(Taylor & Francis Inc, 2023) Ozalp, Ozgur; Gumus, Z. Pinar; Soylak, Mustafa
A simple, environmentally friendly, effective and selective magnetic solid-phase extraction method (MSPE) has been developed for the separation and quantitative determination of atrazine from spices and water samples before liquid chromatographic (LC) analysis. Activated carbon cloth@NiCo2O4@Fe3O4 was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction spectrometry (XRD), Brunauer-Emmett-Teller (BET), and scanning electron microscopy with energy distribution X-Ray detector (SEM-EDX) techniques. The developed MSPE-LC procedure was optimized in terms of pH, adsorbent amount, adsorption time, eluent type and volume, interference parameters and the pre-concentration factor and extraction efficiency at optimum conditions were determined. In the determination of atrazine, it was observed that the activated carbon cloth@NiCo2O4@Fe3O4 nanocomposite could be reused at least 25 times by applying the adsorption-desorption cycle. According to best extraction efficiency of parameters for the extraction and determination of atrazine from spices and water samples were determined as pH 7, adsorbent amount of 0 mg, total adsorption-desorption time of 5 minutes, and enrichment factor of 20. The recovery values of the magnetic solid-phase extraction method in spices and water samples under optimum conditions are between 91% and 94%. Analysis of trace levels of atrazine, limit of detection (LOD) and limit of quantification (LOQ) were determined by HPLC-DAD method with 0.5 ng mL(-1) and 1.7 ng mL(-1), respectively. Sample applications with high recovery values performed with the MSPE-LC method were confirmed by liquid chromatography quadrupole time-of-flight mass spectrometry (LC-Q-TOF/MS) for spices and water samples.
Metal organic frameworks as nanomaterials for analysis of toxic metals in food and environmental applications
(Elsevier Sci Ltd, 2021) Gumus, Z. Pinar; Soylak, Mustafa
It is important to develop new materials for analytical sample preparation for the separation, detection and preconcentration of toxic metals from food, and environmental materials. Metal organic frameworks are a class of crystalline materials used in the analysis of toxic metals in recent years, with their porosity, enormous internal surface areas, adsorption capacities, functionalization properties, and stability. MOFs are promising adsorbents for the fast and efficient extraction of heavy metal ions from complex samples in food safety and environmental pollution management. This review describes recent developments in the use of MOFs in the analysis of toxic metals in food and environmental samples. Thus, it will lead to the planning of new studies for the use of MOFs in different matrices. (C) 2021 Elsevier B.V. All rights reserved.
Metal-organic framework functionalized with deep eutectic solvent for solid-phase extraction of Rhodamine 6G in water and cosmetic products
(Wiley-V C H Verlag Gmbh, 2023) Özalp, Özgür; Gümüş, Zinar Pınar; Soylak, Mustafa
An NH2-MIL-53(Al)-DES(ChCl-Urea) nanocomposite was synthesized for extraction and determination of Rhodamine (Rh) 6G from environmental and cosmetic samples. The deep eutectic solvent (DES) was prepared by mixing choline chloride and urea in a mole ratio of 1:2. NH2-MIL-53(Al)-DES(ChCl-Urea) nanocomposite was synthesized using the impregnation method at a ratio of 60:40 (w/w). The optimum conditions were determined after NH2-MIL-53(Al)-DES(ChCl-Urea) characterization was performed. The optimum conditions were determined as pH 8, adsorbent amount of 15 mg, total adsorption-desorption time of 6 min, and enrichment factor of 20. The recovery values of the solid-phase extraction method for water and cosmetic samples under optimum conditions were between 95% and 106%. NH2-MIL-53(Al)-DES(ChCl-Urea) nanocomposite was an economically advantageous adsorbent because of its reusability of 15 times. All analyses were performed using the ultraviolet-visible spectrophotometer. The linear range, limit of detection, and limit of quantification of the method were 100-1000, 9.80, and 32.68 & mu;g/L, respectively. The obtained results showed that the synthesized nanocomposite is a suitable adsorbent for the determination of Rh 6G in water and cosmetic samples. The real sample applications were verified with the high-performance liquid chromatography system.
MIL-101(Cr) metal-organic frameworks based on deep eutectic solvent (ChCl: Urea) for solid phase extraction of imidacloprid in tea infusions and water samples
(Elsevier, 2023) Ozalp, Ozgur; Gumus, Z. Pinar; Soylak, Mustafa
MIL-101(Cr)@DES (ChCl: Urea) nanocomposite was synthesized by impregnation method to be used in solid phase extraction (SPE) of imidacloprid from herbal tea infusions and water samples before HPLC analysis. The characterization of the MIL-101(Cr)@DES (ChCl: Urea) was described using XPS, SEM-EDX, FT-IR, XRD, TGA, and BET analyses. Recovery of imidacloprid from herbal tea infusions and water samples was obtained in the range of 90%-98% under optimum conditions of SPE parameters (adsorbent amount: 10.0 mg, pH 7.0, adsorption time: 3 min, eluent volume:2.0 mL). The enrichment factor was 20 -fold when the sample volume was 40 mL. 15 adsorption/desorption cycles of the nanocomposite have demonstrated an economically and environmentally advantageous reusability. The recovery results of the SPE-HPLC procedure showed that MIL-101(Cr)@DES (ChCl: Urea) nanocomposite was a good and effective adsorbent in the extraction and determination of imidacloprid from herbal tea infusions and water samples.(c) 2023 Elsevier B.V. All rights reserved.
Sample Preparation Methods for Metal Containing Pesticides in Food and Environmental Samples
(Taylor & Francis Inc, 2022) Ozalp, Ozgur; Uzcan, Furkan; Gumus, Z. Pinar; Soylak, Mustafa
Metal-containing pesticides are used in many areas for purposes such as harvest efficiency and keeping pests away from the vegetable environment. Metal-containing pesticides are in the form of dithiocarbamate complexes and are named differently according to the type of metal they contain and are used for different purposes. Since the presence of these pesticides even at residue level threatens human and environmental health, their determination at trace level is important. In this review, studies on the determination of metal-containing dithiocarbamate pesticides in different matrices are discussed. This review on the analysis of dithiocarbamate pesticides with different techniques will shed light on the studies to be carried out for the determination of these pesticides one by one in different matrices.
Separation and Preconcentration of Atrazine on Magnetic Multiwalled Carbon Nanotubes before Determination in Food and Water Samples by High-Performance LIQUID CHROMATOGRAPHY with Diode Array Detection (HPLC-DAD)
(Taylor & Francis Inc, 2023) Uzcan, Furkan; Gumus, Zinar Pinar; Soylak, Mustafa
This work focuses upon the easy and efficient synthesis of multi-walled carbon nanotubes (MWCNT) decorated with magnetite used in the vortex-assisted magnetic solid-phase microextraction (VA-m-mu-SPE) of atrazine in water and food samples. The nanocomposite was characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and infrared spectroscopy. Parameters that influenced VA-m-mu-SPE (pH, mMWCNT mass, extraction time, eluent type and volume, and sample volume) were optimized. The presented technique provided a preconcentration factor of 10-fold with limits of detection and quantification of 2.1 mu g L-1 and 6.4 mu g L-1, respectively, and a linear range from 12.5 to 250 mu g L-1. VA-m-mu-SPE has been applied in the preconcentration and determination of atrazine in the natural waters. In addition, atrazine was determined in ginger and fennel.
Some trace elements in front and rear dorsal ordinary muscles of wild and farmed bluefin tuna (Thunnus thynnus L. 1758) in the Turkish part of the eastern Mediterranean Sea
(Pergamon-Elsevier Science Ltd, 2011) Percin, Fatih; Sogut, Ozlem; Altinelataman, Can; Soylak, Mustafa
The levels of trace metals of front (F) and rear (R) dorsal ordinary muscles (dom) of wild and farmed bluefin tuna (BFT) were determined by atomic absorption spectrometry. Wilds were obtained from Antalya Bay and farmed were taken from a fish farm in Ildir Bay (Izmir), during spring to early summer. The accuracy of the method was checked standard reference material (NRCC-DORM-2 Dogfish Muscle). Mean trace element content of the wild samples (Fdom and Rdom, respectively) was found as: Cu, 0.790 and 0.591; Mn, 0.084 and 0.096; Ni, 0.101 and 0.124; Zn, 4.788 and 5.577; Fe, 7.670 and 9.222 (mu g g(-1) wet wt.). Values for farmed were detected as Cu, 0.581 and 0.453; Mn, 0.111 and 0.139; Ni, 0.072 and 0.092; Zn, 4.631 and 3.380; Fe, 4.957 and 7.156 (mu g g(-1) wet wt.). The results were compared with literature values. Crown Copyright (C) 2011 Published by Elsevier Ltd. All rights reserved.
Supramolecular solvent-based liquid-liquid microextraction (SUPRAS-LLME) of Sudan dyes from food and water samples with HPLC
(Elsevier, 2024) Ahmed, Hassan Elzain Hassan; Kori, Abdul Hameed; Gumus, Zinar Pinar; Soylak, Mustafa
Utilizing the environmentally friendly technique of supramolecular solvent -based microextraction (SUPRASLLME), Sudan I -IV dyes were successfully isolated and enriched from food and natural water samples. The optimization of the microextraction process was carried out by studying the effects of various parameters such as pH (6.0), supramolecular volume (100 mu L), tetrahydrofuran (THF) volume (200 mu L), ultrasonication temperature (40 degrees C), and vortex time (1.0 min). Extraction efficiency ranged between 82 % and 109 %, while other analytical parameters such as the limits of detection (LOD) were determined to be 0.23, 0.51, 0.42, and 0.39 mu g L -1 for Sudan I, II, III, and IV, respectively. The total figure of merits for the presented SUPRAS-LLME method includes a limits of quantification (LOQ) of 0.78, 1.70, 1.41, and 1.30 mu g L -1 , a relative standard deviation (RSD%) of 3.4, 6.1, 2.9, and 4.4 (n = 10), a linear range of 5-1000 mu g L -1 for all Sudan dyes, a pre -concentration factor (PF) of 15, 10, 10, and 17, and a determination coefficient (R 2 ) of 0.9994, 0.9965, 0.9955, and 0.9946, for Sudan I, II, III, and IV, respectively. The environmental friendliness of the method was confirmed by evaluating the greenness of the method with the AGREE metric tool. A sustainable and environmentally friendly option for the extraction of Sudan dyes from food and water samples is offered by this SUPRAS-LLME method.
Vortex-assisted solid phase extraction on MIL-101(Cr) of parabens in waters and cosmetics by HPLC-DAD
(Springer, 2023) Yengin, Cigdem; Gumus, Zinar Pinar; Ilktac, Raif; Elci, Aydan; Soylak, Mustafa
In this study, metal organic framework MIL-101 (Cr) was used as an adsorbent in the solid phase extraction of parabens before chromatographic analysis. Analytical parameters including pH, adsorption-desorption time, amount of adsorbent, elution solvents, desorption volume and salt effect were optimized. Optimum adsorbent amount and total adsorption and desorption time for determination of parabens were found to be 15 mg and only 10 min. The recovery values obtained with this method are in the range of 90.78-104.89% for water matrix and 85.19-108.35% for cosmetics. The detection limits of the HPLC method for methyl, ethyl, propyl, and butyl parabens are 0.0387, 0.0322, 0.0299, and 0.0339 ug/mL, respectively. Prior to HPLC analysis, a new, fast, inexpensive, and environmentally friendly solid phase extraction method based on vortex-assisted MIL-101 (Cr) adsorption was developed. This proposed VA-SPE-HPLC procedure was used for the extraction and determination of four different parabens from water and cosmetic samples.

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