eng
Iranian Chemical Society
Analytical and Bioanalytical Chemistry Research
2383-093X
2015-12-01
2
2
73
84
10.22036/abcr.2015.10158
10158
Removal of Dibenzothiophene Using Activated Carbon/γ-Fe2O3 Nano-Composite: Kinetic and Thermodynamic Investigation of the Removal Process
Maryam Fayazi
maryam.fayazi@yahoo.com
1
Mohammad Ali Taher
ma_taher@gmail.com
2
Daryoush Afzali
afzali_dar@gmail.com
3
Ali Mostafavi
a_mostafavi41@gmail.com
4
Shahid Bahonar University of Kerman
Research Institute of Environmental Sciences
Environment Department, Research Institute of Environmental Sciences, International Center for Science, High Technology & Environmental Sciences, Kerman, Iran
Department of Chemistry, Faculty of Sciences, Shahid Bahonar University, Kerman, Iran
In the present study, removal of dibenzothiophene (DBT) from model oil (n-hexane) was investigated using magnetic activated carbon (MAC) nano-composite adsorbent. The synthesized nano-composite was characterized by FT-IR, FE-SEM, BET and VSM techniques. The MAC nano-composite exhibited a nearly superparamagnetic property with a saturation magnetization (Ms) of 29.2 emu g-1, which made it desirable for separation under an external magnetic field. The magnetic adsorbent afforded a maximum adsorption capacity of 38.0 mg DBT g-1 at the optimized conditions (adsorbent dose, 8 g l-1; contact time, 1 h; temperature, 25 °C). Langmuir, Freundlich and Temkin isotherm models were used to fit equilibrium data for MAC nano-composite. Adsorption process could be well described by the Langmuir model. Kinetic studies were carried out and showed the sorption kinetics of DBT was best described by a pseudo-second-order kinetic model. In addition, the MAC nano-composite exhibited good capability of recycling to adsorb DBT in gasoline deep desulfurization.
https://www.analchemres.org/article_10158_245cc0572200492c0c8e3ebb1cf6008e.pdf
Magnetic
Desulfurization
Activated carbon
Adsorbent
Dibenzothiophene
eng
Iranian Chemical Society
Analytical and Bioanalytical Chemistry Research
2383-093X
2015-12-01
2
2
85
89
10.22036/abcr.2015.10300
10300
Electro-Organic Synthesis: An Efficient Method for the Preparation of Nanosized Particles of Phthalazine Derivatives via One-Pot Multicomponent Reactions
Somayeh Makarem
s_makarem@sbu.ac.ir
1
Ali Reza Fakhari
a-zavareh@sbu.ac.ir
2
Ali Asghar Mohammadi
a-mohammadi@sbu.ac.ir
3
Department of chemistry, Karaj branch, Islamic Azad University, Karaj, Iran.
Department of Chemistry, Faculty of Sciences, Shahid Beheshti University, G. c., P. o. Box: 19396-4716, Evin, Tehran, I. R. Iran
chemistry and Chemical Engineering Research Center of Iran (CCERCI), PO Box 14335-186, Tehran, I.R. Iran
Aza heterocyclic compounds are major interest for organic chemists because of their mainly pharmacological activities and clinical applications such as antianxiety, antitumor, anticonvulsant, cardiotonic and vasorelaxant. This contribution describes an electrochemical approach for the preparation of nanosized particles of phthalazine in high yields and very short reaction time. The method is based on theone-pot multicomponent reaction (MCRs) of phthalhydrazide, malononitrile and aldehydes in propanol employing undivided cell in the presence of NaBr as an electrolyte. The product was characterized, after purification, using IR, 1H NMR, 13C NMR, MS and SEM. This procedure provides a method by which nanoparticles are synthesized directly from phthalhydrazide, malononitrile and aldehydes insides of a routine protocol for the synthesis of nano particles of organic compounds in which the synthesized organic compound is transformed into nanosized particles using modern high technology, for example ultrahighpressure rapid expansion of supercritical solution, and supercritical antisolvent with enhanced mass transfer. Size reduction is a fundamental unit operation having important applications in pharmacy. It helps to improve solubility and bioavailability, reduce toxicity, enhance release, and provide better formulation opportunities for drugs.
https://www.analchemres.org/article_10300_c5693360e1cb8660db7c3ee181f840b3.pdf
Phthalhydrazide
Malononitrile
Aldehydes
Nanosized particles
Multicomponent
eng
Iranian Chemical Society
Analytical and Bioanalytical Chemistry Research
2383-093X
2015-12-01
2
2
91
98
10.22036/abcr.2015.10756
10756
Selective Liquid-Liquid Extraction of Lead Ions Using Newly Synthesized Extractant 2-(Dibutylcarbamoyl)benzoic Acid
Hossein Soltani
h.soltani@znu.ac.ir
1
Mohammad Reza Yaftian
yaftian@znu.ac.ir
2
Abbasali Zamani
zamani@znu.ac.ir
3
Massomeh Ghorbanloo
m_ghorbanloo@yahoo.com
4
University of Zanjan
University of Zanjan
University of Zanjan
University of Zanjan
A new carboxylic acid extractant, named 2-(dibutylcarbamoyl)benzoic acid, is prepared and its potential for selective solvent extraction and recovery of lead ions from industrial samples was investigated. The slope analysis indicated that the lead ions are extracted by formation of 1:2 metal to ligand complexes. The effect of the parameters influencing the extraction efficiency including kind of the organic diluent, extractant concentration, type of the salt used for ionic strength adjustment, contact time and temperature was evaluated and discussed. Under optimized conditions (aqueous phase: 5 ml, initial lead concentration 1 × 10-4 M, pH 4, sodium chloride 0.1 M; organic phase: 5 ml dichloromethane, ligand concentration 0.05 M), a quantitative (75.2 ± 0.8%) and highly selective extraction of lead ions in the presence of zinc, nickel, cobalt and cadmium ions (each 1 × 10-4 M) was achieved, after 20 min. magnetically stirring of the phases, at 25 °C. The extracted lead ions were stripped from the organic phase by diluted nitric acid (0.1 M) solution. The proposed method was successfully applied for separation of lead from industrial samples. The study of the effect of temperature allowed evaluating the thermodynamic parameters of the extraction process of lead ions by the studied extractant into dichloromethane.
https://www.analchemres.org/article_10756_6da486bcb5bff6e7fd694bf406b65ffb.pdf
Lead ions
Solvent extraction
Selective separation
Carboxylic acid extractant
Industrial samples
eng
Iranian Chemical Society
Analytical and Bioanalytical Chemistry Research
2383-093X
2015-12-01
2
2
99
112
10.22036/abcr.2015.10758
10758
Simultaneous RP-HPLC and UV Spectroscopic Method Development and Validation for Estimation of Ibandronate Sodium in Bulk and Pharmaceutical Dosage Form
Priyanka Bose
meow.bose@gmail.com
1
Suddhasattya Dey
kuntal.kuni@gmail.com
2
Souvik Basak
souvik_basak1@yahoo.com
3
Shreya Shah
shah.shreya723@gmail.com
4
Anjan De
de.anjan@yahoo.co.in
5
Dr. B.C. Roy College of Pharmacy & AHS
WBUT
WBUT
Sigma Institute of Pharmacy
WBUT
The present study describes a simple, accurate, precise and cost effective UV-Vis Spectroscopic and RP-HPLC method for the estimation of Ibandronate sodium (IBN). The determination of Ibandronate sodium (IBN) was performed by both UV and RP-HPLC method using 215 nm as the determination wavelength. The drug was dissolved in NaOH solution (0.1N NaOH) for estimation in UV and in distilled water for the estimation in RP-HPLC using mobile phase 0.01 M Sodium dihydrogen phosphate (NaH2PO4): Acetonitrile (80:20), pH being adjusted to 3.3 with 10% ortho-phosphoric acid. A linear response was observed in the range of 10-50 μg ml-1 (R2 = 0.9981) for UV-Spectroscopy, whereas for RP-HPLC the linear response was observed in the range of 20-70 μg ml-1 (R2 = 0.9965). The limits of quantitation (LOQ) were estimated as 0.1 μg ml-1 and 0.05 μg ml-1, respectively for UV and RP-HPLC respectively. The recoveries of IBN from the marketed formulation were found to be within 100 ± 2% by both the methods. These methods were then effectively applied for the estimation of Boniva (tablet) and the results were obtained according to nominal content. The statistical analysis revealed that there is no significant difference (p > 0.05) between UV and HPLC methods regarding validation parameters and assay content.
https://www.analchemres.org/article_10758_6e7865b53685ad91f446371261f18ae7.pdf
Ibandronate sodium (IBN)
UV-Vis spectroscopy
RP-HPLC
Calibration curve
LOD
eng
Iranian Chemical Society
Analytical and Bioanalytical Chemistry Research
2383-093X
2015-12-01
2
2
113
118
10.22036/abcr.2015.11302
11302
Application of Statistics to Evaluate Iranian Analytical Laboratories Proficiency: Case of Aflatoxins in Pistachio
Leila Fotouhi
l.fotouhi@ut.ac.ir
1
Azamosadat Meshkani
ameshkani@yahoo.com
2
Melody Houshmand
me.houshmand@yahoo.com
3
IBB, University of Tehran
Marjaan Khatam, Training, Research & Q.C. Lab. Services, Tehran 1415633341, Iran
Marjaan Khatam, Training, Research & Q.C. Lab. Services, Tehran 1415633341, Iran
The aim of this study was to evaluate the utility of a proficiency testing program among limited number of local laboratories as an alternative to the IUPAC/CITAC guide on proficiency testing with a limited number of participants, specially where international schemes are not accessible. As a sample scheme we planned to determine aflatoxins (B1, G1, B2, G2, total) in Iranian pistachio matrix. A part of naturally contaminated pistachio sample was tested for sufficient homogeneity by a competent laboratory and then homogenized sub-samples were distributed among participants all across the country. The median of participants’ results was selected as assigned value. Student t-test was applied to show there is no significant difference between assigned and mean values of homogeneity test results obtained by the competent laboratory. Calculated z-scores showed that 6 out of 8 results in aflatoxin B1, 7 out of 8 results in aflatoxin B2, 5 out of 8 results in aflatoxin G1, 7 out of 8 results in aflatoxin G2 and 6 out of 9 results in aflatoxin total were in satisfactory range. Together our studies indicate that the approach described here is highly cost efficient and applicable for quality assurance of test results when there is no access to international proficiency testing providers.
https://www.analchemres.org/article_11302_8e75a74caa1f6a34c24edc41129ee6b1.pdf
Proficiency testing
Aflatoxins
Z-score
Pistachio
Quality Assurance
Assigned value
eng
Iranian Chemical Society
Analytical and Bioanalytical Chemistry Research
2383-093X
2015-12-01
2
2
119
128
10.22036/abcr.2015.11540
11540
Voltammetric Determination of Sulfadoxine and Its Application in Pharmaceuticals and Urine Samples
Naveen Gokavi
nvngokavi@gmail.com
1
Sharanappa Nandibewoor
stnandibewoor@yahoo.com
2
Karnatak University Dharwad
Karnatak University Dharwad
The voltammetric behaviour of Sulfadoxine (SDN) was studied at a glassy carbon electrode in 0.2 M phosphate buffer solutions using cyclic, differential-pulse (DPV) and square wave voltammetry (SWV). The dependence of the current on pH, concentration, and scan rate was investigated to optimize the experimental conditions for the determination of SDN. The oxidation process was shown to be diffusion controlled, irreversible over the pH range from 3.0-9.2. An analytical method was developed for the determination of SDN in phosphate buffer solution at pH 3.0 as a supporting electrolyte. A DPV method showed a good linear response as compared to SWV. The anodic peak current varied linearly with SDN concentration in the range 0.310-4.34 µg ml-1 of SDN with a limit of detection (LOD) of 0.01 µg ml-1. The recovery was determined in the range from 95.6-100.1%. The proposed method was successfully applied to the quantitative determination of SDN in pharmaceutical formulations and an urine as real samples.
https://www.analchemres.org/article_11540_ba9bb9ae8f8b5d88f69a01e30b0572de.pdf
glassy carbon electrode
Sulfadoxine
Voltammetry
Phosphate buffer
eng
Iranian Chemical Society
Analytical and Bioanalytical Chemistry Research
2383-093X
2015-12-01
2
2
129
137
10.22036/abcr.2015.11927
11927
Coupling Second-Order Excitation-Emission Spectrofluorimetric Data with Standard Addition method to Quantify Carvedilol in Real Samples
Masoud Shariati-Rad
mshariati_rad@yahoo.com
1
Mohsen Irandoust
irandoust1341@yahoo.com
2
Sara Sheikhi
sheikhi.sa67@gmail.com
3
Razi University
Razi University
Razi University
Prediction using pure standards is expected to be biased whenever the slope of the calibration is affected by the presence of sample matrix. Moreover, in the presence of unknown spectral interferents, first-order algorithms like partial least squares cannot be used. In this study, a method for determination of carvedilol (CAR) in tablet and urine samples is proposed by excitation-emission fluorescence spectroscopy (EEM). The multivariate curve resolution-alternating least-squares (MCR-ALS) coupled with trilinearity constraint exploiting the second order advantage is applied for the analysis of EEMs. Moreover, the combination of standard addition with MCR-ALS was used to correct the matrix effect. Indeed, by the proposed strategy, both matrix effect and the problem of the presence of unknown interferents in determination of CAR are overcome. The MCR-ALS method was applied on EEMs under non-negativity and trilinearity constraints. For both samples, CAR was quantified at low mg l-1 level with an overall prediction error of -3.1% and -4.0% in urine and tablet samples, respectively.
https://www.analchemres.org/article_11927_29f7be4eebb3c6fd375737bad7b95f41.pdf
Carvedilol
Excitation-emission fluorescence
Multivariate curve resolution
Urine samples
eng
Iranian Chemical Society
Analytical and Bioanalytical Chemistry Research
2383-093X
2015-12-01
2
2
139
150
10.22036/abcr.2015.11928
11928
Electrochemical Sensor for Determination of Fenitrothion at Multi-wall Carbon Nanotubes Modified Glassy Carbon Electrode
Molla Tefera
mtnegash@gmail.com
1
Shimelis Admassie
shimadm09@gamil.com
2
Merid Tessema
tessemamerid@yahoo.com
3
Solomon Mehretie
solomon.mehretie@aau.edu.et
4
Department of Chemistry, Addis Ababa University, P. O. Box: 1176, Addis Ababa, Ethiopia. Department of Chemistry, University of Gondar, P. O. Box: 196, Gondar, Ethiopia
Department of Chemistry, Addis Ababa University, P. O. Box: 1176, Addis Ababa, Ethiopia
Department of Chemistry, Addis Ababa University, P. O. Box: 1176, Addis Ababa, Ethiopia
Department of Chemistry, Addis Ababa University, P. O. Box: 1176, Addis Ababa, Ethiopia
A sensor, based on multi-wall carbon nanotubes modified glassy carbon electrode (MWCNT/GCE), was developed for determination of fenitrothion. Determining the surface area of MWCNT/GCE showed that this surface is three times more active than that of a glassy carbon electrode. The experimental parameters, such as the amount of MWCNTs, pH of the fenitrothion solution, preconcentration potential and preconcentration time were optimized. Under these conditions, reduction current showed a linear relationship with the concentration of fenitrothion in a range of 0.01-5.0 mM, with a detection limit of 6.4 nM. The modified electrode also exhibited good stability and reproducibility. The effects of possible interferents were studied and found to be negligible, indicative of high selectivity of the electrode. This sensor was also successfully employed for determination of fenitrothion in soil and Teff samples with recovery values in the range of 88.0-93.3% and 86.7-91.4%, respectively.
https://www.analchemres.org/article_11928_3d037bc3c9874a76aa49288d55c3e8f0.pdf
Fenitrothion
Multi-wall carbon nanotube
Square wave voltammetry
Soil
Teff