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Analytical Methods in Environmental Chemistry Journal - Volume:4 Issue: 2, Jun 2021

Analytical Methods in Environmental Chemistry Journal
Volume:4 Issue: 2, Jun 2021

  • تاریخ انتشار: 1400/05/03
  • تعداد عناوین: 7
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  • Fatemeh Pourbahman, Mohsen Zeeb*, Amirhossein Monzavi, Zahra Khodadadi, Seyed Saied Homami Pages 5-24

    framework-74/Fe3O4/polytyramine (GO/MOF-74/Fe3O4/PTy) was fabricated and applied in magnetic dispersive micro-solid phase extraction (MD-μ-SPE) coupled with high performance liquid chromatography (HPLC) for simultaneous determination of fluoroquinolones compounds including, ofloxacin, ciprofloxacin, lomefloxacin, enrofloxacin and sperfloxacin in egg samples. The GO/MOF-74/Fe3O4/PTy nanocomposite was fabricated through an in situ synthesis of MOF-74 in the presence of magnetic GO and followed with an oxidative polymerization of tyramine using horsedish peroxide (HRP) enzyme. The modifier agents improved the merits of the nanoporous sorbent. Extraction protocols based on GO/MOF nanocomposites have various benefit such as, the high stability, the tunable porosity, the fast mast transfer and reasonable enrichment factor. The fabricated material was characterized via energy dispersive x-ray analysis (EDX), the scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR), and the x-ray diffraction (XRD). The calibration curves revealed linearity (0.9992 ≤ r2 ≤ 0.9997) in the ranges of 1.0-475.0, 0.5-350.0, 0.5-350.0, 0.5-375.0 and 1.5-300.0 ng mL-1 with limit of detections (LODs, S/N=3) of 0.3, 0.1, 0.2, 0.1 and 0.4 ng mL-1 for ofloxacin, ciprofloxacin, lomefloxacin, enrofloxacin and sperfloxacin, respectively. The intra-assay (≤7.7%, n = 9) and inter-assay (≤7.0%, n = 9) precisions along with accuracy less than 9.0% showed the reliability of the method.

    Keywords: Magnetic dispersive micro-solid phase extraction, Metal–organic framework, Graphene oxide, Polytyramine, Fluoroquinolones
  • Mahdiyeh Ghazizadeh *, Hamideh Asadollahzadeh Pages 25-33

    An ion selective potentiometric electrode (IPE) was prepared based on salen material (bis(salicylaldehydo)ethylenediimine) as a suitable carrier for determination of cadmium ions. An acceptable response for cadmium ions obtained over a linear range 8 × 10−7 to 1.0 × 10−2M with a slope of 29.8 ± 0.8 mv per decade of activity and a detection limit of 3.2 × 10−7 M for Cd (II) ions in water and liquid samples. It has a response time less than 10 s and can be used for at least 2.5 months without any measurable divergence in potential. The ion selective electrode can be used based on potential and potential changes in the pH range 3.5 to 6.5, so, the cadmium determination was obtained at independent pH. Moreover, the selectivity of proposed method in presence of interference ions was studied. The results showed that the other cations do not interfere significantly in response electrode at optimized pH. This electrode was successfully used for the determination of cadmium ions in aqueous samples. The validation was obtained based on ICP analyzer and certified reference material in water samples (CRM, NIST).

    Keywords: Cadmium, Ion selective electrode, Membrane sensor, Potentiometry, Salen, Water samples
  • Mohammad Saraji, Bahman Farajmand*, Esmaeil Heydari Bafrouei Pages 34-46

    In this research nanostructural poly (o-aminophenol) was synthesized by electropolymerization and used for solid phase microextraction fiber procedure (SPME). Thin film of Poly (o-aminophenol) (4 μm thickness) was shaped by sweep potential for 45 min on the surface of stainless steel wire. Polymer was synthesized by potentiostat procedure too. Prepared polymer by sweep potential procedure showed nanostructures on the surface. Acetic anhydride was employed for derivatization of bisphenol A (BPh-A) and analysis of acetylated BPh-A was utilized by gas chromatography-flame ionization detector (GC-FID). Affecting parameters on derivatization and extraction such as amount of acetic anhydride, stirring rate, temperature, ionic strength and extraction time were optimized. The limit of detection (LOD) and relative standard divisions (RSDs%) were achieved 0.6 μgL-1 and less than 6.8%, respectively under optimized conditions. Finally proposed method was used for extraction of bisphenol A from leaching of baby and drinking water bottles. Relative recovery was achieved 98% for leaching from drinking bottle. In leaching from plastic baby bottle, bisphenol A (BPh-A) was detected in the range 5–15 μg L-1

    Keywords: Poly (o-aminophenol), Nanostructure, Bisphenol A, Solid phase microextraction, Gas chromatography-flame ionization detector
  • Somayeh Mirza*, Azadeh Yahya Meymandi Pages 47-59

    The exposure of lead in workplace air and human workers of battery manufacturing factory was evaluated determined by nanotechnology since 2019-2020. Human whole blood (HWB) for subject and healthy peoples (25-55, Men, 40 N) and workplace air (40N) was prepared based on NIOSH sampling. 10 mL of HWB samples added to 20 mg of mixture ionic liquid/ ligand ([HMIM][PF6]/APDC) modified on graphene oxide nanostructures(GONs) at pH=6. After sonication, the lead ions separated/extracted by dispersive ionic liquid solid phase micro extraction (DIL-SPME) and determined by flame atomic absorption spectrometry (F-AAS). All air samples in workplace were analyzed based on NIOSH process. The results showed us the negative correlation between Pb concentration in human blood subject and healthy peoples (r=0.24). The range concentrations of lead in human subject, healthy peoples and workplace air were obtained 193.4-543.7 μg L-1, 85.6-175.9 μgL-1 and 44.7-81.5 μgm-3, respectively. The LOD, linear rang, enrichment factor(EF) and RSD% were achieved 1.25 μg L-1, 5.0- 310 μg L-1,19.6 and less than 5% by procedure. The method was validated by standard reference material (SRM), the electrothermal atomic absorption spectrometry (ET-AAS) and ICP-MS analyzer for human samples.

    Keywords: Lead, Human whole blood, Workplace air, Nanotechnology, Dispersive ionic liquid solid phase micro extraction, Battery manufacturing factories
  • Seyedeh-Azam Hosseini, Ali Faghihi zarandi, Somayyeh Karami-Mohajeri* Pages 60-71

    Malathion is one of the widely used broad-spectrum organophosphate insecticides (OPI) in Iran. Malathion affects carbohydrate metabolism, causes hyperglycemia and increases the risk of diabetes. The present study was undertaken to investigate the potential of malathion to exacerbate diabetes-induced oxidative stress and impairment in blood glucose level and glucose tolerance in a sub-acute study. Malathion concentration in blood was analyzed with gas chromatography mass spectrometry (GC-MS) after sample preparation of blood samples based on magnetic Fe3O4-supported graphene oxide (Fe3O4@ GO) nanoparticles. Type 1 diabetes was experimentally induced by intraperitoneal administration of streptozocin (65 mg kg-1). Diabetic and non-diabetic rats were treated with malathion at the dose of 150 mg kg-1day-1 or 0.5-4.0 mg L-1 in blood for 4 weeks. Fasting blood glucose was measured every week. At the end of the study, blood samples were investigated for markers of oxidative stress. Exposure to multiple doses of malathion decreased the total antioxidant capacity of plasma and the activity of catalase and superoxide dismutase enzymes in diabetic rats. Blood glucose and glucose tolerance test (GTT) and oxidative damages did not change significantly in diabetic rats exposed to malathion. However, malathion concentration in blood caused to increase GTT in malathion-treated non-diabetic rats. Taking together, our findings provide evidence that daily exposure to malathion for 4 weeks tends to exacerbate the decrease in blood antioxidant status and protein carbonylation in diabetic rats.

    Keywords: Malathion, Blood samples, Diabetes, Oxidative stress, Erythrocyte, Magnetic graphene oxide, Gas chromatography mass spectrometry
  • Arezou Lari, Nafiseh Esmaeili*, Homanaz Ghafari Pages 72-85

    In this study, a novel synthesis adsorbent, 1-(3-aminopropyl)-3-methylimidazolium hexafluorophosphate functionlized on multiwall carbon nanotubes ([Apmim][PF6]-MWCNTs, IL@MWCNTS) was used for nickel/lead (Ni/Pb) extraction and determination by dispersive ionic liquid micro solid-phase extraction (DIL-μ-SPE) coupled to electrothermal atomic absorption spectrometry (ET-AAS). After dilution of 20 mg of IL@MWCNTS in 200 μL of acetone, the mixture was injected to 10 mL of human serum/urine samples at pH of 8.0. After sonication for 5 min, the Ni(II) / Pb(II) were extracted by ionic liquid phase and then centrifuged for 2.5 min. The upper liquid phase set aside and Ni(II) / Pb(II) loaded in adsorbent were back-extracted by acidic solution at pH=2-3. Finally, the concentration of total nickel and lead was determined by ET-AAS. By optimizing, the limit of detection, linear range, and enrichment factor for nickel and lead were obtained (0.05 μg L−1; 0.1 μg L−1), (0.2-5.8 μg L−1; 0.4-30 μg L−1)and 24.7; 5.1, respectively (RSD less than 5%). Also, the capacity absorption of IL@MWCNTS for nickeland lead ionswere achieved 149.3 mg g-1 and 162.5 mg g-1, respectively. The DIL-μ-SPE procedure was validated for nickel and lead extraction by spiking of real samples and ICP-MS analyzer.

    Keywords: Nickel, lead, Human samples, Ionic liquid, Multiwall carbon nanotubes, Micro solid-phase extraction
  • Tahereh Eskandari, Ali Niazi, Mohammad Hossein Fatemi, Mohammad Javad Chaichi* Pages 86-98

    In the present study, a simple, rapid and efficient dispersive liquid–liquid microextraction (DLLME) coupled with spectrofluorimetry (SFM) and chemometrics methods have been proposed for the preconcentration and determination of fenthion in water samples. Box–Behnken design was applied for multivariate optimization of the extraction conditions (sample pH, the volume of dispersive solvent and volume of extraction solvent). Analysis of variance was performed to study the statistical significance of the variables, their interactions and the model. Under the optimum conditions, the calibration graph was linear in the range of 5.0–110 ng mL-1 with the detection limit of 1.23 ng mL-1 (3Sb/m). Parallel factor analysis (PARAFAC) and partial least square (PLS) modelling were applied for the multivariate calibration of the spectrofluorimetric data. The orthogonal signal correction (OSC) was applied for preprocessing of data matrices and the prediction results of model, and the analysis results were statistically compared. The accuracy of the methods, evaluated by the root mean square error of prediction (RMSEP) for fenthion by OSC-PARAFAC and OSC-PLS models were 0.37 and 0.78, respectively. The proposed procedure could be successfully applied for the determination of fenthion in water samples.

    Keywords: Fenthion, Pesticides, Organophosphoruse pesticides, Dispersive liquid–liquid icroextraction, Box–Behnken design, Spectrofluorimetry