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Analytical and Bioanalytical Chemistry Research - Volume:3 Issue: 1, Winter - Spring 2016

Analytical and Bioanalytical Chemistry Research
Volume:3 Issue: 1, Winter - Spring 2016

  • تاریخ انتشار: 1394/12/03
  • تعداد عناوین: 13
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  • Hasan Bagheri, Abbas Afkhami, Amin Noroozi Pages 1-18
    Over the past few years, residual pharmaceuticals (antibiotics, anticonvulsants, antipyretics drugs, hormones) have begun to be considered as emerging environmental pollutants due to their continuous input and persistence to aquatic ecosystem even at low concentrations. Therefore, the development of efficient, cost-effective, and stable methods and materials for the wastewaters treatment have gained more recognition in recent years. In the path of meeting these developments, nanomaterials have attracted much attention as economical, convenient and ecofriendly tools for removing of pharmaceuticals from the hospital wastewaters because of their unique properties. The present review deals with recent advances in removal and/or destruction of residual pharmaceutical in wastewater samples using nanomaterials including metal nanoparticles, carbon nanotubes and nanofilters. In spite of using a variety of nanomaterials to remove the residual of pharmaceuticals, there is still a dearth of successful applicability of them in industrial processes. Therefore, some defects of nanomaterials to be used for the removal of pharmaceutical contaminate in environmental samples and their impacts on human health and environment is briefly discussed.
    Keywords: Hospital wastewater, Pharmaceutical, Nanomaterials, Wastewater, Nanoparticles, Carbon nanotube, Removal
  • Morteza Bahram, Loghman Shokri, Naimeh Mohseni Pages 19-27
    The aim of this work was to develop a new and simple coacervative extraction method for the preconcentration and spectrophotometric determination of Cu(II) in water samples. Dithizone was used as the chelating agent while an anionic surfactant, namely sodium dodecyl sulfate (SDS), was used as extracting agent at room temperature. Central composite design (CCD) based on response surface methodology (RSM) was employed to optimize main experimental parameters such as pH values of solutions, concentration of the surfactant and volume of the saturated salt. Analytical characteristics of the method such as limit of detection, linear range, relative standard deviation (R.S.D.) and relative standard error (R.S.E.) were calculated under the optimum conditions. The calibration graph was linear in the range of 10-100 ng ml-1 with the detection limit of 3.8 ng ml-1. The interference effects of some anions and cations were also studied. The method was successfully applied for the determination of Cu(II) in water samples.
    Keywords: Coacervative extraction, Cu(II), Dithizone, SDS, Central Composite Design
  • Atkuru Veera Venkata Naga Krishna Sunil Kumar, Tamanampudi Varahala Reddy, Chandra Sekharan Pages 29-39
    Two new spectrophotometric methods (M1 and M2) are developed for the determination of vardenafil in bulk and in tablet dosage forms. The method M1 involves oxidative coupling of vardenafil with 3-methyl-2-benzothiazolinone hydrazone hydrochloride in presence of ferric chloride in acidic medium yielding green colored chromogen with absorption maxima at 625 nm. The method M2 is based on the oxidation of 4-aminoantipyrine by potassium periodate, which subsequently couples with vardenafil in an alkaline medium to form a red colored product having absorption maxima at 530 nm. The absorbance concentration graphs were rectilinear over the range of 4-40 μg ml-1 for the method M1 and 4-60 μg ml-1 for the method M2. The limit of detection values was found to be 0.044 μg ml-1 and 0.035 μg ml-1 for the methods M1 and M2, respectively. The analytical performance of the developed methods was fully validated as per the guidelines prescribed by International Conference on Harmonization. The results were found to be acceptable. The application of the proposed methods in the determination of vardenafil in their commercial tablet dosage forms was successful showing good percentage recoveries.
    Keywords: Vardenafil, Electrophilic coupling agent, 3, Methyl, 2, benzothiazolinone hydrazone, Aminoantipyrine, Analysis
  • Ali Daneshfar, Reza Tabaraki, Raana Khodakaramin, Tahere Khezeli Pages 41-51
    A very simple, rapid and sensitive dispersive liquid-liquid microextraction (DLLME) followed by gas chromatography and flame ionization detection (GC-FID) was developed for the determination of phenol and carvacrol in honey samples. A mixture of 100 µl dichloromethane (extraction solvent) and 0.5 ml acetonitrile (disperser solvent) was rapidly injected into sample solution. Thereby a cloudy solution was formed. After centrifuging, the fine droplets of extraction solvent were sedimented in the bottom of the conical test tube. Sedimented phase (0.6 µl) was injected into the GC-FID system. Experimental parameters which control the performance of DLLME, such as type and volumes of extraction and disperser solvents, pH, salt effect and extraction time were investigated. Under optimum conditions obtained by the response surface methodology, the method was found to be linear in the range of 10-200 mg l-1. The limits of detection for phenol and carvacrol were 4.15 and 3.9, respectively, and the extraction recovery ranged from 67-97.3%.
    Keywords: Phenol, Carvacrol, Dispersive liquid, liquid microextraction, GC-FID
  • Zahra Kaboli Tanha, Mahdieh Koorepazan Moftakhar, Mohammad Reza Yaftian, Nader Noshiranzadeh Pages 53-63
    Oxime extractants 3-tert-butyl-2-hydroxy-5-methyl benzaldehyde oxime (HL1) and 3-tert-butyl-2-hydroxy-5-methoxy benzaldehyde oxime (HL2) were synthesized and characterized by conventional spectroscopic methods. Suitable lipophilic nature of the prepared extractants allowed examining the ability of these molecules for extraction-separation of copper from its mixture with normally associated metal ions by performing competitive extraction experiments of Cu(II), Co(II), Ni(II), Zn(II), Cd(II) and Pb(II) ions from chloride solutions. Both ligands transfer selectively the copper ions into dichloromethane by a cation exchange mechanism. Conventional log-log analysis and isotherm curves showed that Cu(II) ions are extracted as the complexes with 1:2 metal to ligand ratio by both extractants. Verification of the effect of the organic diluent used in the extraction of copper ions by HL1 and HL2 demonstrated that the extraction efficiency varies as: dichloromethane ~ dichloroethane > toluene > xylene > ethylacetate. Time dependency investigation of the extraction processes revealed that the kinetics of the extraction of copper by HL2 is more rapid than that of HL1. The application of the ligands for extraction-separation of copper ions from leach solutions of cobalt and nickel-cadmium filter-cakes of a zinc production plants was evaluated.
    Keywords: Copper ions, Solvent extraction, Oxime, Selective separation, Recovery
  • Ehsan Zolfonoun, Seyad Mohammad Reza Pakzad, Maryam Salahinejad Pages 65-72
    A simple and rapid method for the determination of 137Ba isotope abundances in water samples by inductively coupled plasma-optical emission spectrometry (ICP-OES) coupled with least-squares support vector machine regression (LS-SVM) is reported. By evaluation of emission lines of barium, it was found that the emission line at 493.408 nm provides the best results for the determination of 137Ba abundances. After recording the emission spectra in the range of 493.362-493.467 nm, quantification of 137Ba abundances was performed with the aid of LS-SVM algorithm. The obtained results revealed that using LS-SVM as a nonlinear modeling approach improves the predictive quality of the developed models compared with partial least squares (PLS) method. The calculated results proved that the combination of ICP-OES and LS-SVM is a suitable and low cost technique for the determination of 137Ba abundances. Performance of the proposed method was examined through measuring 137Ba abundances in synthetic mixtures and water samples.
    Keywords: 137Ba, ICP-OES, LS, SVM, PLS
  • Morteza Akhond, Ghodratollah Absalan, Ameneh Tafakori, Hamid Ershadifar Pages 73-86
    A carbon ionic liquid electrode (CILE) modified with TiO2-Fe nanoparticles was constructed by incorporating TiO2-Fe nanoparticles into the paste matrix. Under the optimized experimental conditions, using differential pulse voltammetry (DPV), the oxidation of thiocyanate and oxalate were occurred at potentials of 0.740 V and 1.010 V, respectively, at the surface of the modified electrode. Observing a high peak current along with a suitable peak separation allowed introducing the first voltammetric sensor for simultaneous determination of these anions with high sensitivity without mutual interference. A wide linear range of 1.0 × 10-5-1.8 × 10-3 M for thiocyanate with a detection limit of 6.4 × 10-6 Mand a wide linear range of 5.0 × 10-5-3.0 × 10-3 M for oxalate with a detection limit of 2.3 × 10-5 M were obtained. The modified CILE showed good reproducibility, repeatability and storage stability as well as good selectivity. The proposed sensor was successfully applied for analysis of thiocyanate and oxalate in urine samples.
    Keywords: Thiocyanate, Oxalate, Simultaneous determination, TiO2, Fe nanoparticles, Carbon ionic liquid electrode
  • Maryam Fayazi, Masoud Ghanei Motlagh, Mohammad Ali Taher, Raziyeh Fayazi Pages 87-99
    A new method for analysis of trace amount of Rh(III) ions by magnetic activated carbon modified with 2,3,5,6-tetra(2-pyridyl)pyrazine (MAC/TPPZ) as the magnetic sorbent has been proposed. The proposed adsorbent was found to be advantageous over conventional solid phase extraction (SPE) in terms of operational simplicity and low time-consuming. The experimental parameters affecting the extraction/preconcentration and determination of the analyte were systematically examined. In order to investigate the selectivity of this magnetic sorbent, the effect of a variety of ions on preconcentration and recovery of Rh(III) ions were also investigated. Under optimum conditions, the calibration graph was linear for the concentration range of 0.8-650 µg l-1. The limit of detection (LOD, 3Sb/m) and the relative standard deviation (RSD, n = 8, c = 50 µg l-1) were 0.1 µg l-1 and 3.6%, respectively. The maximum sorption capacity of the adsorbent for rhodium was found to be 21.6 mg g-1. The presented procedure was applied to monitoring rhodium in water and synthetic samples.
    Keywords: Spectrometry, Magnetic activated carbon, Rhodium, Nanocomposite
  • Mahmoud Roushani, Somayeh Farokhi Pages 101-110
    A simple and reliable electrochemical sensor based on cobalt oxide nanoparticles modified glassy carbon electrode (GCE/CoOxNPs) for determination of butylated hydroxyanisole is presented here. The nanoparticles were fabricated by electrodepositing method. The modified electrode shows excellent catalytic activity toward butylated hydroxyanisole oxidation in pH 12.0 phosphate buffer solution (PBS). The detection limit (S/N = 3), sensitivity and catalytic rate constant (kcat) of the modified electrode toward butylated hydroxyanisole were 2.9 µM, 5.1 nA μM-1 and 1.1 × 104 M-1 s-1, respectively, at linear concentration rang up to 1350 μM. The capability of the modified electrode for direct butylated hydroxyanisole quantification in real samples is also discussed. This modified electrode shows many advantages such as good catalytic activity, good reproducibility, simple preparation procedure and long-term stability of signal response during butylated hydroxyanisole oxidation. In this report, compared with most cases previously reported, the detection potential of the BHA occurs at a lower potential.
    Keywords: Butylated hydroxyanisole, Cobalt oxide nanoparticles, Electrodeposition, Electrocatalytic oxidation
  • Ramin M.A.Tehrani, Hanieh Ghadimi Pages 111-121
    This study demonstrates the use of a selective and sensitive voltammetric sensor for determination of acetaminophen (AC). This was performed by modifying a glassy carbon electrode with composite film of poly(4-vinylpyridine) and graphene sheet (P4VP/GR-GCE). The redox peak currents of AC increased significantly at P4VP/GR-GCE. The result was achieved by the synergistic effect of combined electron mediator property of P4VP along with remarkable physical properties of GR which improved the kinetics of the catalytic oxidation of AC. The P4VP/GR-GCE exhibited excellent sensitivity, good reproducibilityand long-termstability for measuring AC with detection limits of 3.2 nM in the linear range of 0.04-300 µM. The novel developed sensor was not interfered by physiologically common interference, viz. ascorbic acid (AA) and uric acid (UA). The P4VP/GR-GCE was also successfully applied for detection of AC in tablets and urine samples, so it is reasonable to expect its broad use as AC sensor.
    Keywords: Acetaminophen, Paracetamol, Graphene sheet, Poly(4, vinyl pyridine), Voltammetric determination
  • Masoumeh Mohammadnejad Pages 123-130
    Second order advantage of excitation-emission fluorescence matrix was applied for the simultaneous determination of ibuprofen and caffeine. The proposed method is based on the measurement of the native fluorescence and recording emission spectra of ibuprofen and caffeine in different excitation wavelengths. The mixture of these compounds was resolved by multivariate curve resolution coupled with alternative least squares (MCR-ALS) on constructed matrix. The EEM spectra were recorded at excitation wavelengths from 250-275 nm; the emission wavelengths ranged from 275-400 nm. For each particular quantitative determination, an augmented matrix was defined. The resolution of each augmented-data matrix gave an estimation of the excitation and emission spectra of the species included in the model. Ibuprofen and caffeine were determined in concentration range from 0.10-8.00 and 0.50-15.00 mg ml-1, respectively. The minimal sample pretreatment and relatively low running cost, make this method a good alternative to existing methods for determination of the analytes in urine samples.
    Keywords: ibuprofen, Caffeine, Second order data matrix, Multivariate curve resolution, Alternative least squares
  • Ali Daneshfar, Shirin Babaee Pages 131-138
    A simple and rapid microextraction procedure based on dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-flame ionization detection (GC-FID) was developed for the extraction and analysis of 2-phenylethanol in rose water sample. In the proposed approach, carbon tetrachloride and ethanol were used as extraction and dispersive solvents, respectively. Some important parameters, such as extraction and disperser solvent and volume of them, extraction time, pH and salt effect were investigated. Under optimized conditions, a linear relationship was obtained in the range of 1.0-300.0 mg l-1. The method detection limit was 0.1 mg l-1. The relative standard deviations for the analysis of 2-phenylethanol were in the range of 1.5-2.4%. The relative recoveries of 2-phenylethanol at spiking levels of 10, 75 and 150 mg l-1 were 93.7, 96.9 and 97.2%, respectively. The enrichment factor of the proposed method was 123. The proposed method is a simple, fast, accurate, highly stable and selective and was applied for determination of 2-phenylethanol in rose water sample with satisfactory results.
    Keywords: 2, Phenylethanol, Dispersive liquid, liquid microextraction, Gas chromatography, flame ionization detection, Rose water
  • Kassim Badmus, Jimoh Tijani, Chuks Paul Eze, Ojo Fatoba, Leslie F. Petrik Pages 139-147
    The hydroxyl radical (OH•) is a powerful oxidant produced as a consequence of cavitation in water. It can react nonspecifically in breaking down persistent organic pollutants in water into their mineral form. It can also recombine to form hydrogen peroxide which is very useful in water treatment. In this study, terephthalic acid (TA) and potassium iodide dosimetry were used to quantify and investigate the behaviour of the generated OH radical in a laboratory scale sonicator. The 2-hydroxyl terephthalic acid (HTA) formed during terephthalic acid dosimetry was determined by optical fibre spectrometer. The production rate of HTA served as a means of evaluating and characterizing the OH• generated over given time in a sonicator. The influence of sonicator power intensity, solution pH and irradiation time upon OH• generation were investigated. Approximately 2.2 ´ 10-9 M s-1 of OH radical was generated during the sonication process. The rate of generation of the OH radicals was established to be independent of the concentration of the initial reactant. Thus, the rate of generation of OH• can be predicted by zero order kinetics in a sonicator.
    Keywords: Hydroxyl radical, Hydrogen peroxide, Cavitation, Terephthalic acid, Sonicator, Dosimetry