Publications by authors named "Mustafa Soylak"

236 Publications

Dual-response electrochemical electrode for sensitive monitoring of topotecan and mitomycin as anticancer drugs in real samples.

Chemosphere 2021 Nov 13:132809. Epub 2021 Nov 13.

Ankara University, Faculty of Pharmacy, Department of Analytical Chemistry, 06560, Ankara, Turkey; Sakarya University, Biomaterials, Energy, Photocatalysis, Enzyme Technology, Nano & Advanced Materials, Additive Manufacturing, Environmental Applications, and Sustainability Research & Development Group (BIOENAMS R&D Group), 54187, Sakarya, Turkey. Electronic address:

This research paper employed an innovative electrochemical electrode to simultaneously determine topotecan (TPT) and mitomycin (MMC) as anticancer agents. For this purpose, a novel nanocomposite was synthesized using a hydrothermal procedure. The nanocomposites were characterized using FTIR, STEM, FESEM, mapping analysis, EDX, and XRD methods. The novelty of this work is the successful synthesis of FeO decorated on the surface of CuCoS ([email protected]) nanocomposites showed two separate anodic peaks at 0.8 V for TPT and 1.0 V for MMC with potential separation of 0.2 V. This was enough for the simultaneous electrochemical determination of topotecan and mitomycin on a glassy carbon electrode (GCE), simultaneously. At optimized conditions, the developed electrode exhibited linear responses with TPT and MMC concentration in the ranges of 0.01-0.89 and 0.89-8.95 μM for topotecan and 0.1-19.53 μM for mitomycin. The detection limits were observed as 6.94 nM and 80.00 nM for topotecan and mitomycin, respectively. The fabricated [email protected]/GCE showed high sensitivity, long-term stability, and repeatability towards the sensing of TPT and MMC simultaneously and can be utilized in real samples. The obtained results confirmed that the fabricated [email protected]/GCE nanocomposites can be utilize in the simultaneous electrochemical determination of topotecan and mitomycin in real samples.
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http://dx.doi.org/10.1016/j.chemosphere.2021.132809DOI Listing
November 2021

Preconcentrations of Zn(II) and Hg(II) in Environmental and Food Samples by SPE on B. licheniformis Loaded Amberlite XAD-4.

Biol Trace Elem Res 2021 Nov 2. Epub 2021 Nov 2.

Department of Chemistry, Faculty of Sciences, Erciyes University, 38030, Kayseri, Turkey.

In this work, the separations and preconcentrations of Zn(II) and Hg(II) ions on Bacillus lichenifoemis loaded onto Amberlite XAD-4 resin by solid-phase extraction has been performed. The biosorbent was characterized by using FT-IR, SEM, and EDX. pH, sample flow rate, eluent type and concentration, amount of B. licheniformis and XAD-4 resin, sample volume, and possible interfering ions effect were investigated in details as experimental variables in the SPE procedure. Limit of detection values for Zn(II) and Hg(II) were detected as 0.03 and 0.06 ng mL, respectively. 0.2-15 ng mL linear range values were achieved for Zn(II) and Hg(II), respectively. Relative standard deviation values were found to be lower than 5%. For validation of the procedure, the certified standard reference materials (CWW-TM-D, EU-L-2, NCS ZC73O14, NCS ZC73350) were analyzed. The concentrations of Zn(II) and Hg(II) in water and food samples were measured by ICP-OES. Consequently, it can be inferred that the immobilized B. licheniformis microcolumn has ideal selectivity for Zn(II) and Hg(II) biosorption.
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http://dx.doi.org/10.1007/s12011-021-03000-wDOI Listing
November 2021

Hydrolytic enzyme modified magnetic nanoparticles: An innovative and green microextraction system for inorganic species in food samples.

Anal Chim Acta 2021 Sep 30;1178:338808. Epub 2021 Jun 30.

Technology Research & Application Center (TAUM), Erciyes University, 38039, Kayseri, Turkey; Erciyes University, Faculty of Sciences, Department of Chemistry, 38039, Kayseri-Turkey; Turkish Academy of Sciences (TUBA), Cankaya, Ankara, Turkey. Electronic address:

In the presented study, the usability of hydrolytic enzyme immobilized magnetic nanoparticles as an extraction agent for the microextraction of metal ions from food samples was investigated. α-amylase modified magnetic carbon nanotubes (α-amylase-FeO/MWCNTs) was used as an extraction agent for direct microextraction of trace arsenic from food sample phase into liquid phase medium prior to its ICP-MS determination. In extraction studies using hydrolytic enzymes, it is impossible to recover the free soluble enzyme after extraction without losing its activity. In our study, this problem was overcome by immobilizing the hydrolytic enzyme on magnetic support. In this way, α-amylase-FeO/MWCNTs as an extraction agent with a reuse property of at least six times was used. α-amylase-FeO/MWCNTs was characterized by FT-IR, XRD, SEM, SEM-EDX, VSM, TGA, and DTG techniques. Optimization of the presented method was performed using 1568 A rice flour certified reference material. Analytical parameters such as type of hydrolytic enzyme, pH and volume of the aqueous phase, extraction temperature and ultrasonic irridation time were optimized. The microextraction step was performed in ultrasonic water bath within only ∼15 min. Limit of detection (LOD), limit of quantification (LOQ) and relative standard deviation (RSD %) values for the developed method were found to be 14.3 μg kg, 47.3 μg kg and 7.5%, respectively. The method was successfully applied to the analysis of arsenic contents of different rice and flour samples.
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http://dx.doi.org/10.1016/j.aca.2021.338808DOI Listing
September 2021

Sensitive determination of Fluoxetine and Citalopram antidepressants in urine and wastewater samples by liquid chromatography coupled with photodiode array detector.

J Chromatogr A 2021 Jul 2;1648:462215. Epub 2021 May 2.

Department of Chemistry and Biochemistry, Florida International University, 11200 SW 8th St, Miami, FL 33199, USA.

A new analyte separation and preconcentration method for the trace determination of antidepressant drugs, Fluoxetine (FLU) and Citalopram (CIT) in urine and wastewaters, was developed based on HPLC-DAD analysis after magnetic solid phase extraction (MSPE). In the proposed method, FLU and CIT were retained on the newly synthetized magnetic sorbent ([email protected]) in the presence of buffer (pH 10.0) and then were desorbed into a lower volume of acetonitrile prior to the chromatographic determinations. Before HPLC analysis, all samples were filtered through a 0.45 µm PTFE filter. Experimental parameters such as interaction time, desorption solvent and volume, and pH were studied and optimized in order to establish the detection limit, linearity, enrichment factor and other analytical figures of merit under optimum operation conditions. In the developed method, FLU and CIT were analyzed by diode array detector at the corresponding maximum wavelengths of 227 and 238 nm, respectively, by using an isocratic elution of 60% pH 3.0 buffer, 30% acetonitrile, and 10% methanol. By using the optimum conditions, limit of detections for FLU and CIT were 1.58 and 1.43 ng mL, respectively, while the limit of quantifications was 4.82 and 4.71 ng mL, respectively. Relative standard deviations (RSD%) for triplicate analyses of model solutions containing 100 ng mL target molecules were found to be less than 5.0 %. Finally, the method was successfully applied to urine (both simulated and real healthy human) and wastewater samples, and quantitative results were obtained in recovery experiments.
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http://dx.doi.org/10.1016/j.chroma.2021.462215DOI Listing
July 2021

Determination of chloramphenicol and tetracycline residues in milk samples by means of nanofiber coated magnetic particles prior to high-performance liquid chromatography-diode array detection.

Talanta 2021 Aug 16;230:122307. Epub 2021 Mar 16.

Technology Research and Application Center (TAUM), Erciyes University, 38039, Kayseri, Turkey; Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri, Turkey; Turkish Academy of Sciences (TUBA), Cankaya, Ankara, Turkey. Electronic address:

A magnetic solid phase extraction (MSPE) coupled with high-performance liquid chromatography-diode array detection (HPLC-DAD) methodology was developed for the determination of chloramphenicol (CP) and tetracycline (TET) antibiotic residues in milk samples. As a solid phase sorbent, C-nanofiber coated magnetic nanoparticles were synthesized and extensively characterized using Field Emission Scanning Electron Microscopy (FE-SEM), Raman Spectroscopy and X-ray Powder Diffraction (XRD) analysis. Experimental variables of MSPE method for both antibiotic analytes were investigated and optimized systematically. After MSPE, the linear range for both the analytes (r > 0.9954) were obtained in a range 10.0-600.0 ng mL. The limit of detections (LODs) for CP and TET were 3.02 and 3.52 ng mL, respectively while RSDs % were below than 4.0%. Finally, the developed method based on MPSE-HPLC-DAD was applied to real milk samples to quantify the antibiotic residues. Recovery values for each antibiotic compound were found in the range of 94.6-105.4% (n = 3) by using spiked model solution.
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http://dx.doi.org/10.1016/j.talanta.2021.122307DOI Listing
August 2021

Application of magnetic nanomaterials in bioanalysis.

Talanta 2021 Jul 12;229:122285. Epub 2021 Mar 12.

Technology Research and Application Center (TAUM), Erciyes University, Kayseri, Turkey; Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri, Turkey. Electronic address:

The importance of magnetic nanomaterials and magnetic hybrid materials, which are classified as new generation materials, in analytical applications is increasingly understood, and research on the adaptation of these materials to analytical methods has gained momentum. Development of sample preparation techniques and sensor systems using magnetic nanomaterials for the analysis of inorganic, organic and biomolecules in biological samples, which are among the samples that analytical chemists work on most, are among the priority issues. Therefore in this review, we focused on the use of magnetic nanomaterials for the bioanalytical applications including inorganic and organic species and biomolecules in different biological samples such as primarily blood, serum, plasma, tissue extracts, urine and milk. We summarized recent progresses, prevailing techniques, applied formats, and future trends in sample preparation-analysis methods and sensors based on magnetic nanomaterials (Mag-NMs). First, we provided a brief introduction of magnetic nanomaterials, especially their magnetic properties that can be utilized for bioanalytical applications. Second, we discussed the synthesis of these Mag-NMs. Third, we reviewed recent advances in bioanalytical applications of the Mag-NMs in different formats. Finally, recently literature studies on the relevance of Mag-NMs for bioanalysis applications were presented.
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http://dx.doi.org/10.1016/j.talanta.2021.122285DOI Listing
July 2021

Advanced Methodologies for Trace Elements in Edible Oil Samples: A Review.

Crit Rev Anal Chem 2021 Mar 15:1-20. Epub 2021 Mar 15.

Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri, Turkey.

Advanced methodologies were applied for the detection of some elements at trace levels in edible oils. Trace elements play a role in oil stability, quality of edible oils and fats. In the present study, problems were addressed related to simple, cheap, less time consuming and suitable pretreatment advanced methods for suitable sample introduction and calibrations as well as the strategies and techniques are discussed. The present review is aimed to discuss the significance of simplifying sample treatments are offered for trace elements in oils. The period covered by this review is last twenty years. However, the various applications of advanced methodologies including extraction and microextraction. The scope of spectrometric techniques used for the analysis of trace elements in edible oils was discussed by new instrumental development trends.
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http://dx.doi.org/10.1080/10408347.2021.1895710DOI Listing
March 2021

Vortex-assisted magnetic solid phase extraction of Pb and Cu in some herb samples on magnetic multiwalled carbon nanotubes.

Turk J Chem 2021 17;45(1):210-218. Epub 2021 Feb 17.

Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri Turkey.

This study is the development of a new solid phase extraction method based on using magnetic multiwalled carbon nanotubes impregnated with 1-(2-pyridylazo)2-naphthol (PAN) for separation, preconcentration, and flame atomic absorption spectrometric determination of Pb(II) and Cu(II). Optimization of the method was done by investigating pH effect, amount of magnetic multiwalled carbon nanotubes impregnated with PAN, eluent type and volume, matrix effects, and volume of the sample. The optimum adsorbent amount was found to be 75 mg and the optimum pH value was found as 5.5. The detection limits were 16.6 μg L for Pb(II) and 18.9 μg L for Cu(II). The relative standard deviations (RSD%) were less than 4%. Two certified reference materials: SPS-WW2 wastewater and NCS-DC73349 (bush branches and leaves) were used to test the validation of the method. The method was successfully applied to the analysis of Pb(II) and Cu(II) ions in daisy, mint, paprika, sage, rosemary, daphne leaves, heather, green tea, andsamples.
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http://dx.doi.org/10.3906/kim-2009-26DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC7925297PMC
February 2021

Electrocatalytic evaluation of graphene oxide warped tetragonal t-lanthanum vanadate ([email protected]) nanocomposites for the voltammetric detection of antifungal and antiprotozoal drug (clioquinol).

Mikrochim Acta 2021 02 27;188(3):102. Epub 2021 Feb 27.

Faculty of Sciences, Department of Chemistry, Erciyes University, 38039, Kayseri, Turkey.

Metastable and rarely reported GO warped tetragonal phase t-lanthanum vanadate nanocomposites ([email protected]) are reported for the sensitive electrochemical determination of antifungal drug Clioquinol (CQ). The hydrothermal method was adopted for synthesis of [email protected] The electrochemical performance of CQ was examined using cyclic voltammetry (CV) and differential plus voltammetry (DPV) at [email protected] modified glassy carbon electrode (GCE). The electrocatalytic oxidation of CQ at the [email protected]/GCE shows the highest anodic peak current at a potential of +0.51 V vs. Ag/AgCl. The proposed sensor provides excellent sensitivity of 4.1894 μA μM cm, a very low detection limit (LOD) of 2.44 nM, and a wide range of 25 nM to 438.52 μM towards CQ detection. Finally, the detection of CQ in biological media was successfully done using the [email protected]/GCE and possesses recoveries of 94.67-98.0%.
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http://dx.doi.org/10.1007/s00604-021-04758-5DOI Listing
February 2021

New Trend in the Extraction of Pesticides from the Environmental and Food Samples Applying Microextraction Based Green Chemistry Scenario: A Review.

Crit Rev Anal Chem 2021 Feb 9:1-27. Epub 2021 Feb 9.

Faculty of Sciences, Department of Chemistry, Erciyes University, Kayseri, Turkey.

This review focused on the green microextraction methods used for the extraction of pesticides from the environmental and food samples. Microextraction techniques have been explored and applied in various fields of analytical chemistry since its beginning, as evinced by the numerous reviews published. The success of any technique in science and technology is measured by the simplicity, environmentally friendly, and its applications; and the microextraction technique is highly successive. Deliberations were attentive to studies where efforts have been made to validate the methods through the inter-laboratory comparison study to assess the analytical performance of microextraction techniques against conventional methods. Succinctly, developed microextraction methods are shown to impart significant benefits over conventional techniques. Provided that the analytical community continues to put forward attention and resources into the growth and validation of the microextraction technique, a promising future for microextraction is forecasted.
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http://dx.doi.org/10.1080/10408347.2021.1874867DOI Listing
February 2021

Development of Armillae mellea immobilized nanodiamond for the preconcentrations of Cr(III), Hg(II) and Zn(II).

Anal Biochem 2021 03 28;617:114122. Epub 2021 Jan 28.

Department of Chemistry, Faculty of Science, Erciyes University, TR-38039 Kayseri, Turkey.

In this study, we present an environmental friend and easy procedure for simultaneous preconcentration of Cr(III), Hg(II) and Zn(II) by solid-phase extraction before their determination by inductively coupled plasma optical emission spectrometry. Armillae mellea immobilized nanodiamond was used as sorbent. During the study, critical parameters influencing the extraction performance were investigated in detail. The best parameters were found as pH 5.0, 2.0 mL min of flow rate, 200 mg of Armillae mellea, 300 mL of sample volume. LOD values were found as 0.025, 0.13 and 0.038 ng mL, respectively for Cr(III), Hg(II) and Zn(II). By applying the developed procedure, sensitivities of ICP-OES were improved for 60 fold for Cr(III), Hg(II) and Zn(II). Their concentrations in different food samples were measured after microwave digestion and solid-phase extraction.
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http://dx.doi.org/10.1016/j.ab.2021.114122DOI Listing
March 2021

Switchable-hydrophilicity solvent liquid-liquid microextraction prior to magnetic nanoparticle-based dispersive solid-phase microextraction for spectrophotometric determination of erythrosine in food and other samples.

Food Chem 2021 Jun 14;348:129053. Epub 2021 Jan 14.

Department of Chemistry, Faculty of Sciences, Erciyes University, 38039 Kayseri, Turkey. Electronic address:

A combination of switchable-hydrophilicity liquid-liquid microextraction prior to magnetic nanoparticle-based dispersive solid-phase microextraction is proposed for the determination of erythrosine using UV/Vis spectrophotometry at 520 nm. Under optimum conditions (i.e., 1.0 mL octylamine as the extraction solvent, 1.5 mL of 10.0 M sodium hydroxide as the phase separation trigger, pH 4.0, 750 µL of acetone as the eluent, 10.0 mg of [email protected] as the adsorbent, and 15.0 mL of the sample solution), the method showed a superior analytical performance with limits of detection less than 25.9 ng mL, limits of quantitation less than 86.3 ng mL and linear dynamic ranges ranging between 86.3 and 1000 ng mL. Percentage relative standard deviations were less than 4.1 and 7.2% for intra-day and inter-day, respectively. The method was successfully applied for the extraction and determination of erythrosine in food samples and other consumer products with recoveries in the range of 94.6-103.9% and within extraction time of 7.8 min per sample.
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http://dx.doi.org/10.1016/j.foodchem.2021.129053DOI Listing
June 2021

A new method for the preconcentrations of U(VI) and Th(IV) by magnetized thermophilic bacteria as a novel biosorbent.

Anal Bioanal Chem 2021 Feb 2;413(4):1107-1116. Epub 2021 Jan 2.

Department of Chemistry, Faculty of Sciences, Erciyes University, 38030, Kayseri, Turkey.

This paper proposes the use of Anoxybacillus flavithermus SO-15 immobilized on iron oxide nanoparticles (NPs) as a novel magnetized biosorbent for the preconcentrations of uranium (U) and thorium (Th). The SPE procedure was based on biosorption of U(VI) and Th(IV) on a column of iron oxide NPs loaded with dead and dried thermophilic bacterial biomass prior to U(VI) and Th(IV) measurements by ICP-OES. The biosorbent characteristicswere explored using FT-IR, SEM, and EDX. Significant operational factors such as solution pH, volume and flow rate of the sample solution, amounts of dead bacteria and iron oxide nanoparticles, matrix interference effect, eluent type, and repeating use of the biosorbent on process yield were studied. The biosorption capacities were found as 62.7 and 56.4 mg g for U(VI) and Th(IV), respectively. The novel extraction process has been successfullyapplied to the tap, river, and lake water samples for preconcentrations of U(VI) and Th(IV).
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http://dx.doi.org/10.1007/s00216-020-03074-wDOI Listing
February 2021

Review: Microextraction Technique Based New Trends in Food Analysis.

Crit Rev Anal Chem 2020 Nov 30:1-32. Epub 2020 Nov 30.

Faculty of Sciences, Department of Chemistry, Erciyes University, Kayseri, Turkey.

Food chemistry is the study and classification of the quality and origin of foods. The identification of definite biomarkers and the determination of residue contaminants such as toxins, pesticides, metals, human and veterinary drugs, which are a very common source of food-borne diseases. The food analysis is continuously demanding the improvement of more robust, sensitive, highly efficient, and economically beneficial analytical approaches to promise the traceability, safety, and quality of foods in the acquiescence with the consumers and legislation demands. The traditional methods have been used at the starting of the 20th century based on wet chemical methods. Now it existing the powerful analytical techniques used in food analysis and safety. This development has led to substantial enhancements in the analytical accuracy, precision, sensitivity, selectivity, thereby mounting the applied range of food applications. In the present decade, microextraction (micro-scale extraction) pays more attention due to its futures such as low consumption of solvent and sample, throughput analysis easy to operate, greener, robotics, and miniaturization, different adsorbents have been used in the microextraction process with unique nature recognized with wide range applications.
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http://dx.doi.org/10.1080/10408347.2020.1846491DOI Listing
November 2020

Deep Eutectic Solvent-Based Microextraction of Lead(II) Traces from Water and Aqueous Extracts before FAAS Measurements.

Molecules 2020 Oct 19;25(20). Epub 2020 Oct 19.

Department of Chemistry, Faculty of Sciences, Erciyes University, 38039 Kayseri, Turkey.

Microextraction procedures for the separation of Pb(II) from water and food samples extracts were developed. A deep eutectic solvent composed of α-benzoin oxime and iron(III) chloride dissolved in phenol was applied as a phase separator support. In addition, this deep eutectic mixture worked as an efficient extractor of Pb(II). The developed microextraction process showed a high ability to tolerate the common coexisting ions in the real samples. The optimum conditions for quantitative recoveries of Pb(II) from aqueous extracts were at pH 2.0, conducted by adding 150 µL from the deep eutectic solvent. The quantitative recoveries were obtained with various initial sample volumes up to 30 mL. Limits of detection and limits of quantification of 0.008 and 0.025 µg L were achieved with a relative standard deviation (RSD%) of 2.9, which indicates the accuracy and sensitivity of the developed procedure. Recoveries from the reference materials, including TMDA 64.2, TMDA 53.3, and NCSDC-73349, were 100%, 97%, and 102%, respectively. Real samples, such as tap, lake, and river water, as well as food samples, including salted peanuts, chickpeas, roasted yellow corn, pistachios, and almonds, were successfully applied for Pb(II) analysis by atomic absorption spectroscopy (AAS) after applying the developed deep eutectic solvent-based microextraction procedures.
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http://dx.doi.org/10.3390/molecules25204794DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC7587555PMC
October 2020

Nano-clay as a solid phase microextractor of copper, cadmium and lead for ultra-trace quantification by ICP-MS.

Anal Methods 2020 11 7;12(41):4949-4955. Epub 2020 Oct 7.

Department of Chemistry, College of Science, Princess Nourah Bint Abdulrahman University, Riyadh 11671, Kingdom of Saudi Arabia.

Heavy metal microextraction and determination in daily used water is accurately achieved by applying nano-clay as an extractor. The conditions for adsorption/elution of Cu(ii), Cd(ii) and Pb(ii) were investigated by adjusting the pH of samples, sample volume and the type of eluent. The nano-clay showed superior efficiency for microextraction of Cu(ii), Cd(ii) and Pb(ii) at pH 2 using 2 mL of nitric acid (1 M) as the eluent. The microextraction procedure showed high recovery% by changing the sample volume from 15 mL to 70 mL. The preconcentration factor was found to be 37.5. The LOD and LOQ were 1.8, 1.3, and 1.9 μg L and 5.3, 3.9, and 5.7 μg L for Cu(ii), Cd(ii) and Pb(ii) respectively. The addition/recovery from different water samples showed recovery% in the range 88-105 which confirms the efficiency and the accuracy of the developed solid phase microextraction using nano-clay for enrichment of Cu(ii), Cd(ii) and Pb(ii).
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http://dx.doi.org/10.1039/d0ay01343aDOI Listing
November 2020

A new strategy for the combination of supramolecular liquid phase microextraction and UV-Vis spectrophotometric determination for traces of maneb in food and water samples.

Food Chem 2021 Feb 13;338:128068. Epub 2020 Sep 13.

Technology Research and Application Center (TAUM), Erciyes University, 38039 Kayseri, Turkey; Erciyes University, Faculty of Pharmacy, Department of Analytical Chemistry, 38039 Kayseri, Turkey; ERNAM Erciyes University, Nanotechnology Application and Research Center, 38039 Kayseri, Turkey.

A novel and green method was developed for enrichment of maneb (manganese ethylene-bisdithiocarbamate) with a supramolecular solvent liquid phase microextraction method. The microextraction method has been used for the first time in the literature for separation-preconcentration of maneb. 1-decanol and tetrahydrofuran were used in the supramolecular solvent formation. The Mn content of maneb was extracted in the supramolecular solvent phase as 1-(2-pyridylazo)-2-naphthol complex at pH 12.0. Manganese concentration was determined by UV-Vis spectrophotometer at 555 nm. Then, the maneb concentration equivalent to manganese concentration was calculated. The analytical parameters which effective in the method, including pH, volume of reagents, and sample volume were optimized. The limit of detection and the limit of quantification values for maneb were calculated as 2.22 μg L and 7.32 μg L, respectively. The method was successfully applied in the analysis of the maneb content of water and food samples.
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http://dx.doi.org/10.1016/j.foodchem.2020.128068DOI Listing
February 2021

The Determination of Toxic Metals in some Traditional Cosmetic Products and Health Risk Assessment.

Biol Trace Elem Res 2021 Jun 5;199(6):2272-2277. Epub 2020 Sep 5.

Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri, Turkey.

In present study, the levels of some toxic elements in 19 different home-made cosmetic products (spray hair dye, henna, tattoo, eyeliner, eye mascara, smear, lip moisturizer, and lipstick) were analyzed by inductively coupled plasma mass spectrometric (ICP-MS) after microwave digestion. The ICP-MS results were verified by the analyzing certificated reference material (EnviroMAT Drinking Water, High).The detection limit (LOD) was set from 0.1 to 0.2 and the quantification limit (LOQ) from 0.2 to 0.8 μg L and the recoveries estimated from 99% to 109%. The relative standard deviation (RSD) (%) for elements was determined in the range of 0.9 and 2.1%. Although various concentrations of arsenic (As),cadmium (Cd), cobalt (Co), chromium (Cr), cupper (Cu), and nickel (Ni) were determined in some samples, lead (Pb) concentration was found in all the samples. Data obtained were compared with the permissible limit of cosmetic products by the WHO. The concentration of Pb in smear samples was higher than the permitted limit created by the WHO, and Ni concentration in the some samples exceeds the limit set by the WHO. The rank order of toxic elements based on THQ index was Cr > Pb > Ni. The potential non-carcinogenic was considerably lower than the safe risk limits (THQ > 1).
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http://dx.doi.org/10.1007/s12011-020-02357-8DOI Listing
June 2021

An environment-friendly and rapid liquid-liquid microextraction based on new synthesized hydrophobic deep eutectic solvent for separation and preconcentration of erythrosine (E127) in biological and pharmaceutical samples.

Spectrochim Acta A Mol Biomol Spectrosc 2021 Jan 17;244:118842. Epub 2020 Aug 17.

Erciyes University, Faculty of Pharmacy, Department of Analytical Chemistry, 38050 Kayseri, Turkey; Technology Research and Application Center (TAUM), Erciyes University, Kayseri, Turkey; ERNAM-Erciyes University Nanotechnology Application and Research Center, Kayseri 38039, Turkey.

In this study, a new deep eutectic solvent (DES) consist of tetrabuthylammonium bromide (TBABr) and 1-octanol at 1:2 M ratio was prepared for the first time and characterized by Fourier transform infrared spectroscopy (FT-IR), proton nuclear magnetic resonance (H NMR) and carbon nuclear magnetic resonance (C NMR) techniques. The new DES was used as an extraction solvent in the ultrasound assisted liquid-liquid microextraction (UA-LLME) of Erythrosine (E127) in blood, urine, pharmaceutical tablet and syrup samples. Accurate and sensitive determination of erythrosine was accomplished with the combination use of DES-UA-LLME and UV-Vis spectrophotometric detection. Before applying UA-LLME, while protein precipitation was applied to blood samples, pharmaceutical tablets were homogenized and dissolved in methanol. The proposed DES-UA-LLME/UV-VIS procedure was applied directly to urine, syrup sample and supernatant of blood and tablet samples with high recoveries in range of 90% and 100%. Erythrosine in the aqueous sample phase was extracted into 200 μL hydrophobic DES phase at pH 7.0. The effect of important analytical variables such as pH of sample solution, mol ratio of DES components, volume of DES, ultrasonic-based extraction time, sample volume and salt effect were optimized. The preconcentration factor (PF), limit of detection (LOD), intra-day and inter-day relative standard deviations (RSD, %) for the developed procedure were found as 40, 3.75 μg·L, 2.6% and 4.6%, respectively.
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http://dx.doi.org/10.1016/j.saa.2020.118842DOI Listing
January 2021

Nanomaterials-based solid phase extraction and solid phase microextraction for heavy metals food toxicity.

Food Chem Toxicol 2020 Nov 25;145:111704. Epub 2020 Aug 25.

Department of Chemistry, Faculty of Sciences, Erciyes University, 38039, Kayseri, Turkey; Technology Research and Application Center (TAUM), Erciyes University, 38039, Kayseri, Turkey. Electronic address:

In the last few years, nanomaterials are widely used sorbents for the extraction of heavy metals in food samples. The nanomaterials have a larger surface area and show high selectivity, fast adsorption capability, and high efficiency for food contaminants (heavy metals). Carbon nanomaterials (CNMs), magnetic nanoparticles (MNPs), nano-imprinted polymers (NIPs), nano-based metal-organic frameworks (N-MOFs), and silica nanoparticles (SiNPs) are most prominent nanomaterials used in the preconcentration and determination of heavy metals. The most popular sorbent-based techniques for the extraction of heavy metals are solid phase extraction (SPE) and solid phase microextraction (SPME). The use of these nanomaterial sorbents increases the extraction efficiency of both techniques. This review summarizes the nanomaterial sorbents (published 2015 to May-2020) used in solid phase extraction (SPE) and solid phase microextraction (SPME) for heavy metals extraction in food.
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http://dx.doi.org/10.1016/j.fct.2020.111704DOI Listing
November 2020

An environmentally friendly and novel amine-based liquid phase microextraction of quercetin in food samples prior to its determination by UV-vis spectrophotometry.

Spectrochim Acta A Mol Biomol Spectrosc 2020 Dec 7;243:118806. Epub 2020 Aug 7.

Technology Research and Application Center (TAUM), Erciyes University, 38039 Kayseri, Turkey; Erciyes University, Faculty of Pharmacy, Department of Analytical Chemistry, 38039 Kayseri, Turkey; ERNAM Erciyes University, Nanotechnology Application and Research Center, 38039 Kayseri, Turkey.

A novel and environmentally-friendly method, which includes determination of trace amounts of quercetin in samples by using UV-vis spectrophotometry after enrichment with amine-based liquid phase microextraction (LPME), has been developed. As extraction solvent, N,N-dimethyl-n-octylamine has been used and the quercetin concentration in extraction phase was determined by UV-vis spectrophotometry at 382.5 nm. Important analytical parameters such as pH, extraction solvent type and volume, sample volume, extraction time were optimized by the method. Quercetin in the sample solution was extracted to 200 μL of N,N-dimethyl-n-octylamine phase at pH 4.0. The detection limit (LOD) and the quantitation limit (LOQ) values for quercetin were calculated as 0.07 μg·mL and 0.24 μg·mL, respectively. Accuracy studies for the food samples was carried out by addition and recovery experiments. The developed method has been successfully applied to different food samples including spinach, green pepper, red onion and dill weed.
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http://dx.doi.org/10.1016/j.saa.2020.118806DOI Listing
December 2020

Metal organic frameworks enhanced dispersive solid phase microextraction of malathion before detection by UHPLC-MS/MS.

J Sep Sci 2020 Aug 6;43(15):3103-3109. Epub 2020 Jul 6.

Science Faculty, Department of Chemistry, Erciyes University, Kayseri, Turkey.

Metal organic frameworks are considered as an efficient and promised adsorbent for separation of several ions and compounds from solutions due to its unique geometric structure. Herein, copper-benzyl tricarboxylic acid based metal organic frameworks have showed a high efficiency in enrichment and microextraction of malathion from food and water samples. The microextraction procedures were followed by determination of malathion by ultra high performance liquid chromatography with tandem mass spectrometry. The optimum recoveries for malathion were obtained at pH 6, and with using 2 mL of ethyl acetate as the eluent. The microextraction procedures showed a detection limits and the quantification limits of 4.0 and 10.0 µg/L, respectively. The intra- and interday precision showed a relative standard deviation% less than 10. The feasibility of the proposed procedure was determined by evaluating the addition/recovery studies of malathion from the real samples. The absolute recovery% was ≥92%. Furthermore, some ions were tested as cointerfering ions, and the recovery% was 93-100%. These results confirm that the developed microextraction procedure based on copper-benzyl tricarboxylic acid based metal organic frameworks as extractor for dispersive solid phase microextraction is matrix-independent, and can be applied for various real samples including different matrix or various malathion content.
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http://dx.doi.org/10.1002/jssc.202000033DOI Listing
August 2020

A new magnetized thermophilic bacteria to preconcentrate uranium and thorium from environmental samples through magnetic solid-phase extraction.

J Pharm Biomed Anal 2020 Jul 18;186:113315. Epub 2020 Apr 18.

Sen Research Group, Department of Biochemistry, Kutahya Dumlupinar University, Kutahya, Turkey. Electronic address:

A magnetic solid-phase extraction (MSPE) method was developed for simultaneous preconcentrations of U(VI) and Th(IV) before their measurements by inductively coupled plasma optical emission spectrometry (ICP-OES). The main idea of this biotechnological application depends on the use of bacteria, thermophilic Bacillus cereus SO-14, as a solid-phase biosorbent. It was immobilized to γ-FeO magnetic nanoparticles and used for MSPE. Characterization of the biosorbent was performed using the scanning electron microscope (SEM), the energy dispersive X-ray (EDX) and Fourier transform infrared (FT-IR) spectroscopy. Also, the the best conditions of experimental parameters were examined, and the reliability of the method developed was verified by applying the certified reference materials. Limit of detections (LODs) of the U(VI) and Th(IV) was calculated as 0.008 and 0.013 ng mL respectively. Relative standard deviations (RSDs) were found to be 1.6 and 2.4 %, respectively, for U(VI) and Th(IV). R was also calculated as 0.9991. Preconcentration factors were achieved as 100 for both elements. It should be highlighted that LODs were critically improved and the sensitivity of ICP-OES was enhanced.
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http://dx.doi.org/10.1016/j.jpba.2020.113315DOI Listing
July 2020

Pyrocatechol violet impregnated magnetic graphene oxide for magnetic solid phase microextraction of copper in water, black tea and diet supplements.

Food Chem 2020 Aug 2;321:126737. Epub 2020 Apr 2.

Tokat Gaziosmanpaşa University, Department of Chemistry, 60250 Tokat, Turkey; King Fahd University of Petroleum and Minerals, Research Institute, Center for Environment and Water, Dhahran, 31261 Saudi Arabia. Electronic address:

Pyrocatechol violet impregnated magnetic graphene oxide hybrid material (PV-MGO) was prepared as magnetic solid phase microextraction for separation and preconcentration of copper before its determination by flame atomic absorption spectrometry. PV-MGO hybrid material was characterized using field emission scanning electron microscope (FE-SEM, SEM-Mapping), scanning transmission electron microscopy (STEM), energy dispersive X-ray (EDX), Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and Raman spectroscopy. Effects of various parameters such as pH, eluent type, vortex time, amount of magnetic adsorbent were investigated. Under the optimized conditions the MSPE-FAAS procedure presents limit of detection (LOD) of 4.0 μg L, limit of quantification (LOQ) of 13.3 μg L, preconcentration factor of 20 and relative standard deviation (RSD) 4.93%. The accuracy of the method was confirmed by the analysis of the certified reference materials (NCS ZC73032 Celery, CRM025-050 metals on soil, TMDA-64.2 fortified water) and addition-recovery tests. The present method was successfully applied to water, black tea and diet supplements.
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http://dx.doi.org/10.1016/j.foodchem.2020.126737DOI Listing
August 2020

Green synthesis of magnetic carbon nanodot/graphene oxide hybrid material ([email protected]@GO) for magnetic solid phase extraction of ibuprofen in human blood samples prior to HPLC-DAD determination.

J Pharm Biomed Anal 2020 Feb 18;179:113001. Epub 2019 Nov 18.

Erciyes University, Faculty of Pharmacy, Department of Analytical Chemistry, Kayseri, Turkey; ERNAM-Erciyes University Nanotechnology Application and Research Center, 38039, Kayseri, Turkey; Erciyes University, Technology Research & Application Center (TAUM), 38039, Kayseri, Turkey. Electronic address:

In this study, a green production method was used to obtain magnetic carbon nanodot/graphene oxide hybrid material ([email protected]@GO) for the magnetic solid phase extraction (MSPE) of ibuprofen (IBU) in human plasma prior to HPLC-DAD determination. For the first time in the literature, [email protected]@GO hybrid material was synthesized and used as an adsorbent. C-nanodots were produced from pasteurized cow milk by using a simple and cheap hydrothermal method. After production of the C-nanodots and GO, [email protected]@GO hybrid material was fabricated in green solvent medium by using an one-step hydrothermal method. The method was based on the simple separation, preconcentration and analysis of ibuprofen by using MSPE-HPLC-DAD combination. The concentration changes of ibuprofen in human bloods against time were successfully monitored by using this combined method. For this purpose, blood samples were taken from volunteers at certain intervals after the administration of a certain dose of ibuprofen, and the MSPE method was used to monitor the concentration changes of ibuprofen in the blood samples. Experimental variables affecting the extraction efficiency of IBU such as sample solution pH, amount of adsorbent, extraction time, eluent type and volume were studied and optimized in the details. The characterization studies for the [email protected]@GO were carried out by X-ray diffraction spectrometry (XRD), Fourier transform infrared spectrometry (FT-IR), Raman spectrometry (Raman), energy dispersive x-ray (EDX), vibrating sample magnetometry (VSM) and scanning electron microscopy (SEM) techniques. Under the optimum experimental conditions, the limit of detection (LOD) was 8.0 ng mL and the recoveries at three spiked levels in human plasma were ranged from 91.0% to 95.0% with the relative standard deviation (RSD %) less than 4.0 % (n = 6). The results show that together use of MSPE with HPLC-DAD provides a simple and rapid analysis of ibuprofen in human plasma samples.
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http://dx.doi.org/10.1016/j.jpba.2019.113001DOI Listing
February 2020

CuO-CuO ball like/multiwalled carbon nanotube hybrid for fast and effective ultrasound-assisted solid phase extraction of uranium at ultra-trace level prior to ICP-MS detection.

Talanta 2020 Jan 23;207:120295. Epub 2019 Aug 23.

Technology Research & Application Center (TAUM), Erciyes University, 38039, Kayseri, Turkey; Erciyes University, Faculty of Sciences, Department of Chemistry, 38039, Kayseri, Turkey.

Multiwalled carbon nanotube/CuO-CuO ball like hybrid material (MWCNTs/CuO-CuO) synthesized using of a green hydrothermal process was evaluated as a new sorbent for solid phase extraction of uranium with inductively coupled plasma mass spectrometry (ICP-MS). According to our best knowledge, this new material was synthesized and used as solid phase extraction adsorbent for the first time in the literature. The characterization of new hybrid material was carried out using Raman spectroscopy, X-ray diffraction (XRD) and scanning electronic microscopy techniques (SEM, SEM-EDX and SEM-Mapping). The characterization results demonstrated that the new hybrid nanostructure was successfully obtained. The ultrasound-assisted solid phase extraction (UA-SPE) procedure was performed using 100 mg of new hybrid sorbent, 1000 μL of a 0.1% (w/v) solution of α-benzoin oxime and 2000 μL of phosphate buffer at pH 7.0 for separation and preconcentration of uranium. Uranium was eluted with 2 M HCl and the levels of uranium was measured by using ICP-MS. The linearity was observed between 2.5 and 100 ng mL concentration range with a good correlation coefficient (r = 0.999, n = 7). The obtained limit of detection and quantitation values were 0.52 and 1.70 ng mL, respectively. Under optimum conditions, the preconcentration factor (PF) was calculated as 13.3. The accuracy of the developed method was assessed by analyzing of TMDA-62.2, TMDA-70.2 (Environment Canada) and GBW-07423 certified reference water and soil materials. The proposed UA-SPE-ICP-MS procedure developed with MWCNTs/CuO-CuO hybrid material was successfully applied to the analysis of uranium at ultra-traces levels in environmental water and geological rock samples.
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http://dx.doi.org/10.1016/j.talanta.2019.120295DOI Listing
January 2020

Multi-element determination in some foods and beverages using silica gel modified with 1-phenylthiosemicarbazide.

Food Addit Contam Part A Chem Anal Control Expo Risk Assess 2019 Nov 6;36(11):1667-1676. Epub 2019 Sep 6.

Chemistry Department, Erciyes University, Kayseri, Turkey.

1-Phenylthiosemicarbazide bonded modified silica gel (PTC-SG) was synthesised and characterised by FTIR, SEM and elemental analysis for a novel separation/preconcentration of multiple elements based on solid phase extraction. The analytical parameters including pH of solutions, amounts of PTC-SG, flow rates of sample, eluent type and sample volume were optimised. The adsorption capacities of PTC-SG were found to be 7.9, 6.4, 6.3, 8.3, 7.2, 8.9 and 6.6 mg/g for Cu(II), Cd(II), Pb(II), Co(II), Cr(III), Ni(II) and Mn(II), respectively. The limit of detection (LOD) was calculated as 3x the standard deviation(s) of the reagent blank (k = 3, N = 21) and the LOD values were obtained to be 0.98 µg L (Cu), 0.65 µg L (Cd), 0.57 µg L (Pb), 1.12 µg L (Co), 1.82 µL (Cr), 1.67 µg L (Ni) and 0.55 µg L (Mn). Certified reference materials were used to test the validation of the present method. The new solid phase extraction method was successfully applied to determination of the amount of multiple elements in food and beverage samples.
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http://dx.doi.org/10.1080/19440049.2019.1662954DOI Listing
November 2019

A hybrid material composed of multiwalled carbon nanotubes and MoSe nanorods as a sorbent for ultrasound-assisted solid-phase extraction of lead(II) and copper(II).

Mikrochim Acta 2019 09 3;186(10):666. Epub 2019 Sep 3.

Faculty of Sciences, Department of Chemistry, Erciyes University, 38039, Kayseri, Turkey.

A [email protected] nanorod hybrid material was synthesized by a hydrothermal method and used as an adsorbent for trace levels of Pb(II) and Cu(II). The material was characterized by Raman spectroscopy, XRD, SEM, SEM-EDX, SEM-mapping and BET methods. The hybrid material is demonstrated to be a viable sorbent for ultrasound-assisted solid phase extraction of Pb(II) and Cu(II) at pH 5.5. Following desorption with 3 M HNO, the two elements were quantified by FAAS. Key parameters affecting the extraction efficiency, including eluent conditions, amount of adsorbent, sample volume were optimized. No significant interference by other ions is observed. The accuracy of the method was evaluated by the analysis of the certified reference materials TMDA-53.3 (lake water) and SPS-WW2 (waste water level 2). The recoveries were in good agreement with certified values. The method was successfully applied to the extraction/preconcentration of Pb(II) and Cu(II) in different real samples. Graphical abstract A hybrid material of type [email protected] was synthesized, characterized, and used as adsorbent for Pb(II) and Cu(II). Key parameters affecting the extraction efficiency, including eluent conditions, amount of adsorbent, sample volume were optimized. The method was applied to the extraction of analytes in water samples.
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http://dx.doi.org/10.1007/s00604-019-3766-1DOI Listing
September 2019

A magnetized fungal solid-phase extractor for the preconcentrations of uranium(VI) and thorium(IV) before their quantitation by ICP-OES.

Mikrochim Acta 2019 05 16;186(6):355. Epub 2019 May 16.

Department of Chemistry, Faculty of Sciences, Erciyes University, 38039, Kayseri, Turkey.

The fungus Bovista plumbea immobilized on γ-FeO nanoparticles is shown to be a novel sorbent for magnetic solid-phase extractions of U(VI) and Th(IV). The biosorbent was characterized by FT-IR, SEM, and EDX. The effects of pH value, flow rate and volume of sample, amounts of biomass and support material, eluent type, foreign ions and repeated use of the sorbent on extraction efficiency were investigated. The sorption capacities are 41 and 44 mg g, respectively, for U(VI) and Th(IV). The results indicated that B. plumbea immobilized onto γ-FeO nanoparticles can be utilized as a novel material for the preconcentrations of U(VI) and Th(IV) in certified materials and in spiked tap, river and lake waters. Graphical abstract Schematic presentation of a method for preconcentrations of Th(IV) and U(VI) ions using γ-FeO nanoparticles loaded with the fungus Bovista plumbea.
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http://dx.doi.org/10.1007/s00604-019-3474-xDOI Listing
May 2019

Magnetic solid phase extractions of Co(II) and Hg(II) by using magnetized C. micaceus from water and food samples.

Food Chem 2019 Jan 12;271:232-238. Epub 2018 Jul 12.

Department of Chemistry, Faculty of Sciences, Erciyes University, 38039 Kayseri, Turkey.

A new bio-MSPE sorbent based on the use of C. micaceus and γ-FeO magnetic nanoparticle was prepared for the preconcentrations of Co(II) and Hg(II). Critical parameters including pH, flow rate, quantity of C. micaceus, quantity of γ-FeO magnetic nanoparticle, eluent (type, concentration and volume), sample volume, and foreign ions were examined. Surface structure and variations after interaction with Co(II) and Hg(II) of bio-MSPE sorbent were investigated by FT-IR, SEM, and EDX. The impact of bio-MSPE column reusage was also tested. The biosorption capacities were determined as 24.7 mg g and 26.2 mg g, respectively for Co(II) and Hg(II). Certified reference materials were utilized to find out the accuracy of the prepared bio-MSPE method. This novel bio-MSPE method was accomplished by being applied to real food and water samples. In particular, it will be possible to make use of C. micaceus as new alternatives, in environmental biotechnology applications.
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http://dx.doi.org/10.1016/j.foodchem.2018.07.067DOI Listing
January 2019
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