Analytical Sciences
Online ISSN : 1348-2246
Print ISSN : 0910-6340
ISSN-L : 0910-6340
Volume 22 , Issue 9
Showing 1-23 articles out of 23 articles from the selected issue
Original Papers
  • Shigeki EGAMI, Hideaki MONJUSHIRO, Hitoshi WATARAI
    2006 Volume 22 Issue 9 Pages 1157-1162
    Published: 2006
    Released: September 12, 2006
    JOURNALS FREE ACCESS
    A new principle to measure the magnetic susceptibility of a solution was proposed; it utilized the displacement of solution surface caused by the magnetic force applied to the solution. The interfacial displacement was measured with the sensitivity of 5 nm from a change of the interference fringes, so called Newton Ring, generated from the solution surface and an upper surface of a small plano-convex lens on the bottom wall of a cell. The surface displacement measurement was carried out in a homemade cell attached by one or two small Nd-Fe-B magnets. The performance of this method was investigated by the measurements of magnetic susceptibility of manganese(II) chloride solution and some lanthanide(III) solutions. An excellent linear relationship between the magnetic susceptibility and the interfacial displacement was observed for each solution system. Then, it was demonstrated that this relationship could be used for the determination of the magnetic susceptibility of solutions or the concentration of a solute by using the manganese(II) solution as a standard solution.
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  • Takashi SUMIDA, Tetsuya NAKAZATO, Hiroaki TAO, Mitsuko OSHIMA, Shoji M ...
    2006 Volume 22 Issue 9 Pages 1163-1168
    Published: 2006
    Released: September 12, 2006
    JOURNALS FREE ACCESS
    An on-line column preconcentration technique coupled with inductively coupled plasma-mass spectrometry (ICP-MS) and -atomic emission spectrometry (ICP-AES) was developed using a mini-column (ca. 3 mm i.d., 40 mm length), that was packed with chelating resin (0.2 g) of iminodiacetic acid groups, Muromac A-1. After the preconcentration step, the column was washed with ammonium acetate buffer (pH 5.5) and water to remove major elements, such as Ca and Mg, and then eluted with 4 ml of 2 mol l-1 nitric acid. Eleven trace elements (Al, V, Fe, Co, Ni, Cu, Zn, Cd, Pb, Th and U) in seawater were determined by ICP-MS/AES. Recoveries for most of the elements tested were over 90%, although those for Al, V and Th were around 70%. The accuracy of the proposed method was evaluated by analyzing a standard reference material of seawater (NASS-4, NRC Canada). The values of Fe, Co, Ni, Cu, Zn, Cd and Pb obtained with the present method showed good agreement with the certified values as judged from the standard deviation. The method was successfully applied to characterize seasonal variations of trace elements in deep seawater (DSW) and surface seawater (SSW). In addition, no serious decrease in analytical performance of the present column system was observed during the experimental period of about 1 year.
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  • Magda Ali AKL, Yoshihito MORI, Kiyoshi SAWADA
    2006 Volume 22 Issue 9 Pages 1169-1174
    Published: 2006
    Released: September 12, 2006
    JOURNALS FREE ACCESS
    Solvent sublation has been studied for the separation and determination of trace iron(II) in various kinds of water samples. A strongly magenta-colored anionic [Fe(FZ)3]4- complex was formed at pH 5.0 upon adding 3-(2-pyridyl)-5,6-bis(4-phenylsulfonic acid)-1,2,4-triazine (ferrozine, FZ) to the sample solution. Tetrabutylammonium bromide (TBAB) was added in the solution to form the (TBA)4[Fe(FZ)3] ion pair, and an oleic acid (HOL) surfactant was added. Then, the (TBA)4[Fe(FZ)3] ion pairs were floated by vigorous shaking in the flotation cell and extracted into methyl isobutyl ketone (MIBK) on the surface of the aqueous solution. The iron collected in the MIBK layer was measured directly by spectrophotometry and/or flame atomic-absorption spectrophotometry. Different experimental variables that may affect the sublation efficiency were thoroughly investigated. The molar absorptivity of the (TBA)4[Fe(FZ)3] ion pair was 2.8 × 104 l mol-1 cm-1 in the aqueous layer. Beer's law held up to 1.0 mg l-1 Fe(II) in the aqueous as well as in the organic layers. The adopted solvent sublation method was successfully applied for the determination of Fe(II) in natural water samples with a preconcentration factor of 200. The application was extended to determine iron in pharmaceutical samples.
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  • Masahiro MARUO, Takashi DOI, Hajime OBATA
    2006 Volume 22 Issue 9 Pages 1175-1178
    Published: 2006
    Released: September 12, 2006
    JOURNALS FREE ACCESS
    Ion-exchange chromatography using a high-capacity anion exchanger with UV detection was applied to the determination of nitrate in seawater. Major ions in seawater samples did not affect the peak shape and the retention time of the nitrate when an alkaline metal cation-chloride solution was used as an eluent at high concentrations (0.5 - 2 mol/l). At a wavelength of 220 nm, the peak of bromide was very small because of low absorption, while its separation from the nitrate peak was good at high concentrations. Among the eluents tested, lithium chloride gave the best separation of nitrate from bromide. It was estimated that the lithium ion had the least potential for ion-pair formation with nitrate, and its retention time was prolonged compared with the retention times when using other cations; with bromide and nitrite, such an effect was not observed. The results of shipboard seawater nitrate determination by our method in the South Pacific Ocean and Antarctic Sea showed good agreement with those by the conventional photometric method using continuous flow.
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  • Jirasak THREEPROM, Waraporn SOM-AUM, Jin-Ming LIN
    2006 Volume 22 Issue 9 Pages 1179-1184
    Published: 2006
    Released: September 12, 2006
    JOURNALS FREE ACCESS
    The simultaneous determination of metal ions using ethylenediaminetetraacetic acid (EDTA) as a complexing agent and vancomycin as a complex selector was successfully studied by capillary electrophoresis with the U-shaped cell. The partial filling method (counter current mode) was used in order to gain selectivity of the separation, and also to increase the detection sensitivity. The effect of the vancomycin concentration on the separation behavior of free EDTA and metal products, and the effect of the EDTA concentration on the stability of metal-EDTA products were considered. Under the optimal condition, the reproducibilities (RSD) of the migration time and the peak area were less than 3.39% and 9.61%, respectively. With the high sensitivity of the method, Pb(II), Cu(II) and Fe(III) in tap water were successfully determined, and the recoveries were 99 - 105%. The concentrations of these metal ions found in tap water did not exceed the maximum allowed concentrations regulated by the U.S. Environmental Protection Agency.
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  • Masafumi SHIMIZU, Yukuya YOSHIAKI, Atsushi SATO, Makoto TSURUOKA
    2006 Volume 22 Issue 9 Pages 1185-1188
    Published: 2006
    Released: September 12, 2006
    JOURNALS FREE ACCESS
    Fluorescence polarization analysis (FPA) of a liquid-phase method was carried out with a glycosylphosphatidylinositol (GPI) anchored membrane receptor bone marrow stromal cell antigen 1 (BST-1, CD157) as a model receptor for medical screening. A soluble receptor, BST1-Fc, was prepared by fusing the extracellular domain of BST-1 and the Fc region of human immunoglobulin G (IgG). The binding curves of BST1-Fc with a fluorescently labeled ligand peptide, or its three derivatives, were developed using ordinary FPA in the liquid phase. The obtained dissociation constants (Kd) were comparable with those reported as measured with SPR of a solid-phase method, except for one derivative peptide with Kd larger than 7000 nM. Competitive FPA was carried out, and it was demonstrated that a very weak interaction, which would be difficult to detect with SPR or other solid-phase methods, could be analyzed with both ordinary and competitive FPA.
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  • A-Lin XIA, Hai-Long WU, Dong-Mei FANG, Yu-Jie DING, Le-Qian HU, Ru-Qin ...
    2006 Volume 22 Issue 9 Pages 1189-1195
    Published: 2006
    Released: September 12, 2006
    JOURNALS FREE ACCESS
    Daunorubicin (DNR) is a significant antineoplastic antibiotic, which is usually applied to a chemotherapy of acute lymphatic and myelogenous leukaemia. Unfortunately, cardiotoxicity research in animals has indicated that DNR is cardiotoxic. Therefore, it is important to quantify DNR in biological fluids. A new algorithm, the alternating fitting residue (AFR) method, and the traditional parallel factor analysis (PARAFAC) have been utilized to directly determine DNR in human plasma and urine. These methodologies fully exploit the second-order advantage of the employed three-way fluorescence data, allowing the analyte concentrations to be quantified even in the presence of unknown fluorescent interferents. Furthermore, in contrast to PARAFAC, more satisfactory results were gained with AFR.
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  • Verónica ARANCIBIA, Claudia PEÑA, Rodrigo SEGURA
    2006 Volume 22 Issue 9 Pages 1197-1200
    Published: 2006
    Released: September 12, 2006
    JOURNALS FREE ACCESS
    The objective of this study was to determine the complexing capacity of four types of powdered commercial milks with copper(II) using square wave adsorptive stripping voltammetry. Two were types of cow milk adapted for babies under one year (A and B), one was soymilk (C) and the other was normal milk (D). Milk solutions were prepared following the instructions shown on the milk container, and they were mixed with a pepsin solution simulating a baby's stomach conditions (pepsin and salts concentration, pH and temperature). Complexing capacity was determined by titrating milk samples with aliquots of a standard copper solution until the peak current due to solvated or free copper ions was increasing. Assuming a 1:1 copper-milk complex, the apparent stability constant was found using the pseudopolarogram method. The log KCu-milk values were 4.9, 5.0, 3.0 and 5.1 for A, B, C and D types of milk, respectively. Voltammograms of the milk solution as a function of copper added show that the binding properties of the four types of powdered milk studied were different and that saturation of the four types, occurs at different copper concentrations. Concentrations obtained were: 4.9, 5.8, 1.1 and 10.1 mM for A, B, C and D types, respectively. The best complexing agent was the solution prepared with powdered milk D and the worst was that of C. This is important for the bioavailability of this element as a micronutrient.
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  • Jamshid L. MANZOORI, Mohammad AMJADI, Maghsood OROOJI
    2006 Volume 22 Issue 9 Pages 1201-1206
    Published: 2006
    Released: September 12, 2006
    JOURNALS FREE ACCESS
    Crude extract of kohlrabi (Brassica oleracea gongylodes) was prepared by a simple procedure and its enzymatic activity and total protein concentration were determined. It was found that this crude extract is a rich source of peroxidase (POx) and has high specific activity. Cross-linked polyvinylpyrrolidone was used as a stabilizer in the preparation of the crude extract. The POx activity of kohlrabi crude extract did not vary for at least 2 months when deoxygenated and stored at 4°C. This extract was applied for the spectrofluorometric determination of hydrogen peroxide using homovanillic acid as a fluorogenic substrate. POx catalyzes the hydrogen peroxide oxidation of homovanillic acid to produce a dimer which shows strong fluorescence at 420 nm with excitation at 312 nm. In the optimum conditions, the calibration graph for hydrogen peroxide was linear up to 190 ng mL-1, with a detection limit of 4.4 ng mL-1. The relative standard deviation (RSD) was 1.48% for 50 ng mL-1 hydrogen peroxide. The proposed method was successfully applied to the determination of hydrogen peroxide in honey. The concentration-time profile of H2O2 produced upon dilution of honey was studied and H2O2 contents of some different honeys from various areas of Iran were determined.
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  • Vepa K. RAO, Mukesh K. SHARMA, Ajay K. GOEL, Lokendra SINGH, Krishnamu ...
    2006 Volume 22 Issue 9 Pages 1207-1211
    Published: 2006
    Released: September 12, 2006
    JOURNALS FREE ACCESS
    A disposable amperometric immunosensor was studied for the rapid detection of Vibrio cholerae (V. cholerae), the causative agent of cholera, employing an indirect sandwich enzyme linked immunosorbent assay (ELISA) principle. Screen-printed electrodes (SPEs) were fabricated (by using commercial and homemade carbon inks), electrochemically characterized and the assay conditions were optimized for capturing antibodies and antigen. Whole cell lysate (WCL) of V. cholerae was used to raise antibodies in rabbits and mice. The antibodies raised against WCL of V. cholerae were found to be specific, and no cross reactivity was observed with other enteric bacteria. 1-Naphthyl phosphate was used as a substrate with the amperometric detection of its enzymatic hydrolysis product 1-naphthol at a potential of +400 mV vs. Ag/AgCl reference electrode. A comparison between the amperometric detection technique and the standard ELISA was made in terms of the total assay time, the amount of biological materials used and the sensitivity of detection. The minimum detection limit of the amperometric immunosensor for V. cholerae was found to be 105 cells/ml in 55 min, while ELISA detected 106 cells/ml in 4 h.
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  • Jahan-Bakhsh RAOOF, Reza OJANI, Hadi BEITOLLAHI, Rahman HOSSEINZADEH
    2006 Volume 22 Issue 9 Pages 1213-1220
    Published: 2006
    Released: September 12, 2006
    JOURNALS FREE ACCESS
    A carbon paste electrode (CPE) chemically modified with 1-[4-(ferrocenyl ethynyl)phenyl]-1-ethanone (4-FEPEMCPE) was employed to study the electrocatalytic oxidation of L-cysteine using cyclic voltammetry, differential pulse voltammetry and double potential step chronoamperometry as diagnostic techniques. The diffusion coefficient (D = 7.863 × 10-6 cm2 s-1) of L-cysteine was also estimated using chronoamperometry. The electron-transfer coefficient, α (= 0.40), for L-cysteine at the surface of 4-FEPEMCPE was determined using cyclic voltammetry technique. It was found that under an optimum pH (= 7.00), the oxidation of L-cysteine at the surface of such an electrode occurred at a potential of about 350 mV less positive than that of an unmodified CPE. The catalytic oxidation peak currents represented a linear dependence on the L-cysteine concentration. Linear analytical curves were obtained in the ranges of 9.0 × 10-5 - 4.9 × 10-3 M and 2.0 × 10-5 - 2.8 × 10-3 M of L-cysteine with correlation coefficients of 0.9981 and 0.9982 in cyclic voltammetry and differential pulse voltammetry, respectively. The detection limits (2 σ) were determined to be 9.9 × 10-6 M and 5 × 10-6 M with cyclic voltammetry and differential pulse voltammetry, respectively. The influences of twenty other amino acids, such as glutamine, L-glutamic acid, L-glysine, L-histidine, L-isoleucine, L-leucine, L-arginine hydrochloride, L-aspargine, L-aspartic acid, S-carboxy methyl-L-cysteine, L-methionine, L-phenyl alanine, L-proline, L-serine, L-threonine, L-cystine, cysteamine and gluthathione, on the current response of the sensor were examined. The obtained results did not show any influence on the analytical signal of L-cysteine by these amino acids (except for cysteamine). The method was also used for the selective determination of L-cysteine in patient-blood plasma and some pharmaceutical preparations by using standard addition method.
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  • M. MAZLOUM ARDAKANI, M. JAMSHIDPOUR, H. NAEIMI, L. MORADI
    2006 Volume 22 Issue 9 Pages 1221-1226
    Published: 2006
    Released: September 12, 2006
    JOURNALS FREE ACCESS
    A highly selective poly(vinyl chloride) (PVC) membrane electrode based on an N,N′-ethylene-bis(4-methyl-salicylidineiminato) nickel(II) [Ni(EBMSI)] complex as a carrier for a thiocyanate-selective electrode is reported. The influences of the membrane composition, pH and possible interfering anions were investigated based on the response properties of the electrode. The electrode exhibited a good Nernstian slope of -58.9 ± 0.7 mV decade-1, over a wide pH range of 3.5 - 8.5 and a linear range of 1.0 × 10-6 - 1.0 × 10-1 M for thiocyanate. The detection limit of electrode was 3.1 × 10-7 M SCN-. The selectivity coefficients determined by a fixed interference method (FIM) indicate that a good discriminating ability towards the SCN- ion compared to other anions. The proposed sensor had a fast response time of about 5 - 15 s and could be used for at least 3 months without any considerable divergence in the potential. It was applied as an indicator electrode in the titration of thiocyanate with Ag+ and in the potentiometric determination of thiocyanate in saliva and urine samples.
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  • Magda Ali AKL
    2006 Volume 22 Issue 9 Pages 1227-1231
    Published: 2006
    Released: September 12, 2006
    JOURNALS FREE ACCESS
    Phenanthraquinone monophenyl thiosemicarbazone (PPT), an excellent color-forming chelating agent, combines to Pb(II) to form a slightly soluble complex in aqueous solution. To determine this metal ion, a tedious and time-consuming separation technique, such as liquid-liquid extraction, has to be performed. However, the Pb(II)-PPT complex could be determined conveniently by ultraviolet-visible (UV-Vis) spectrophotometry at 520 nm in a Tween 80 micellar medium that has polyoxyethylene groups. After conditions, such as the pH, the concentration of PPT and the stability, were adjusted to their optimum values, the sensitivities of the Pb(II) ions in the Tween 80 micellar medium and in chloroform were compared. It was shown that the sensitivity of Pb(II) in the Tween 80 micellar medium was higher than in chloroform. The interference from different cations and anions was studied. Beer's law was obeyed over a concentration range of 0 - 40 µg ml-1. The detection limit of Pb(II) was 0.036 µg ml-1. The recovery yields of the lead(II) in the synthetic mixtures and water samples ranged from 98 to 99.8%, and their relative standard deviations (RSD) were below 4%. The proposed method was successfully applied to the determination of lead in certified reference samples, biological samples and in environmental water samples.
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  • Jianya WANG, Bin XUE
    2006 Volume 22 Issue 9 Pages 1233-1236
    Published: 2006
    Released: September 12, 2006
    JOURNALS FREE ACCESS
    On the basis of the chromogenic reaction of chromium(VI) with 1,5-diphenylcarbohydrazide (DPC) on the surface of Polysorb C-18 beads and the sequential injection renewable surface technique (SI-RST), a highly sensitive reflect spectrophotometric method for the determination of chromium(III) and chromium(VI) was proposed. Considerations of system and flow cell design, and factors that influence the determination performance were discussed. With 300 µl of sample loaded and 0.6 mg of beads trapped, the linear response range was 0.02 - 0.5 mg l-1 Cr(VI) with a detection limit (3 σ) of 2.4 µg l-1 Cr(VI). The method achieves a precision of 1.3% RSD (n = 11) and a throughput of 53 samples per hour. The determination of Cr(III) was based on the same reaction for the determination of Cr(VI) after being oxidized by (NH4)2S2O8. The precision of the oxidation method was evaluated using a 0.2 mg l-1 Cr(III) standard, yielding an RSD of 2.5% (n = 11). The average recovery of Cr(III) oxidized was tested to be 99.1%. The proposed method was used in the simultaneous determination of Cr(VI) and Cr(III) in water samples, and the error was less than 3%.
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