Analytical Sciences
Online ISSN : 1348-2246
Print ISSN : 0910-6340
ISSN-L : 0910-6340
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Volume 20, Issue 7
Displaying 1-24 of 24 articles from this issue
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Rapid Communications
Original Papers
  • Fluorescent-based Single-strand Conformation Polymorphism/Heteroduplex Capillary Electrophoretic Mutation Analysis of the P53 Gene
    Chunxia ZHAO, Guowang XU, Xianzhe SHI, Jianmei MA, Yan ZHANG, Shen LV, ...
    2004 Volume 20 Issue 7 Pages 1001-1005
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1001
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    Fluorescent-based single-strand conformation polymorphism (F-SSCP) analysis with capillary electrophoresis (CE) is the most common method for the detection of mutation because of its high sensitivity and resolution. In this study, we prepared an inexpensive linear polyacrylamide (LPA), and successfully applied it to CE-SSCP analysis and tandem CE-SSCP/heteroduplex analysis (HA) of the P53 gene on an ABI capillary genetic analyzer. A comparison of the sieving capabilities of a homemade LPA and commercial polydimethylacrylamide (PDMA) demonstrates that the homemade LPA has a higher resolution, a shorter analysis time, and is more suitable for tandem SSCP/HA than commercial PDMA. To show the usefulness, mutations of P53 gene exon 7 - 8 in 37 tumor samples were investigated by using homemade LPA. The results indicate that 10 mutations were found in 9 of 37 cases; the majority of P53 mutations were missense mutations, and 70% were located in exon 7, which plays an important role in neoplastic progression in human tumorigenesis.
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  • ppt Level Detection of Samarium(III) with a Coated Graphite Sensor Based on an Antibiotic
    Mohammad REZA GANJALI, Morteza REZAPOUR, Mohammad REZA POURJAVID, Sohe ...
    2004 Volume 20 Issue 7 Pages 1007-1011
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1007
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    N-[2-[4-[[[(Cyclohexylamino)carbonyl]amino]sulfonyl]phenyl]ethyl]-5-methyl pyrazine carboxamide (glipizid) was explored as an electro-active material for preparing a polymeric membrane-based sensor selective to samarium ions. The membrane incorporated 30% poly(vinyl chloride) (PVC), 53% benzyl acetate (BA), 11% glipizid and 6% sodium tetraphenyl borate. When coated on the surface of a graphite electrode, it exhibits Nernstian responses in the concentration range of 1.0 × 10-5 to 1.0 × 10-10 M, with a detection limit of 8.0 × 10-11 M samarium. The electrode shows high selectivity towards samarium over several cations (alkali, alkaline earth, transition and heavy metal ions), and specially lanthanide ions. The proposed sensor has a very short response time (< 15 s), and can be used in a wide pH range for at least ten weeks. It was used as an indicator electrode in potentiometric titration of Sm(III) ions with an EDTA solution, and for determination of samarium in binary and ternary mixtures.
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  • Direct Fluorescence Quantification of Chromium(VI) in Wastewater with Organic Nanoparticles Sensor
    Leyu WANG, Lun WANG, Tingting XIA, Ling DONG, Guirong BIAN, Hongqi CHE ...
    2004 Volume 20 Issue 7 Pages 1013-1017
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1013
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    Under ultrasonic irradiation, organic fluorescence nanoparticles have been prepared by a reprecipitation method. Compared with single organic fluorophores, these nanoparticles are brighter, more stable against photobleaching and more water-soluble. They also have high room-temperature fluorescence quantum yields (∼20%) and a long fluorescence lifetime (∼0.2 µs). Based on the fluorescence quenching of nanoparticles by chromium(VI), a method for the selective determination of chromium(VI) without the separation of chromium(III) in water was developed. Under the optimal conditions, the linear range of the calibration curve was 7.0 × 10-6 - 1.0 × 10-4 mol L-1. The detection limit was 2.8 × 10-6 mol L-1. The method is characterized by a short reaction time, stable fluorescence signals, simplicity and high selectivity. The present assay has been applied to the selective quantification of Cr(VI) in wastewater with satisfactory results.
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  • A New Method for Atmospheric Nitrogen Dioxide Measurements Using the Combination of a Stripping Coil and Fluorescence Detection
    Xinyu CHEN, Yoshiro ORO, Kenta TANAKA, Norimichi TAKENAKA, Hiroshi BAN ...
    2004 Volume 20 Issue 7 Pages 1019-1023
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1019
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    A new stripping coil for the collection of nitrogen dioxide (NO2) has been developed to increase its versatility and efficiency. Nitrogen dioxide measurements based on quantitative collection through a reaction coil into an alkaline solution has been examined. Nitrogen dioxide is collected in a 0.1 N NaOH solution. This collection system has an efficiency of nearly 100%. The absorbed nitrogen dioxide has been measured by fluorescence detection with sub-ppbv detection limits. The excitation wavelength at 360 nm and the produced emission wavelength at 405 nm were suitable for nitrite ion measurements.
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  • Determination of Trace Levels of Iron in a Seawater Sample Using Isotope Dilution/Inductively Coupled Plasma Mass Spectrometry
    Yuichi TAKAKU, Takuma HAYASHI, Ikuko OTA, Hidenao HASEGAWA, Shinji UED ...
    2004 Volume 20 Issue 7 Pages 1025-1028
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1025
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    An analytical method for trace levels of iron in a seawater sample using isotope dilution ICP-MS was developed. Preconcentration of iron and the removal of major elements in seawater such as alkali and alkaline-earth elements can be carried out quickly using a chelating resin disk by adjusting the sample pH to 3. The collision cell option of the ICP-MS instrument method was used to improve the performance of the instrument for iron measurements since ArO and ArN interferences could be reduced using this analytical method. About 4 ml min-1 helium, as the collision gas, were introduced into the cell. 40Ar14N and 40Ar16O which interfere with 54Fe and 56Fe in water had their amounts decreased by 5 orders of magnitude. Then, the isotope dilution method was used for iron determination below ng g-1 level of trace iron in four environmental reference materials (river water standard sample JAC-0031 (Japan Soc. for Analytical Chemistry), estuarine standard sample SLEW-2 (NRC Canada) and seawater standard samples CASS-3 and NASS-5 (NRC Canada)) were measured. Good agreement between analytical results and certified values of reference materials was obtained, which confirmed the effectiveness of this method.
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  • Determination of Cadmium in River Water Samples by Flame AAS after On-line Preconcentration in Mini-Column Packed with 2-Aminothiazole-modified Silica Gel
    Ilton L. ALCÂNTARA, Paulo S. ROLDAN, Gustavo R. CASTRO, Fabr&iac ...
    2004 Volume 20 Issue 7 Pages 1029-1032
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1029
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    A rapid and sensitive method was developed to determine trace levels of Cd2+ ions in an aqueous medium by flame atomic absorption spectrometry, using on-line preconcentration in a mini-column packed with 100 mg of 2-aminothiazol modified silica gel (SiAT). The Cd2+ ions were sorbed at pH 5.0. The preconcentrated Cd2+ ions were directly eluted from the column to the spectrometer’s nebulizer-burner system using 100 µL of 2 mol L-1 hydrochloric acid. A retention efficiency of over 95% was achieved. The enrichment factor (calculated as the ratio of slopes of the calibration graphs) obtained with preconcentrations in a mini-column packed with SiAT (A = -1.3 × 10-3 + 1.8 × 10-3[Cd2+]) and without preconcentrations (A = 4 × 10-5 + 3.5 × 10-5[Cd2+]), was 51 and the detection limit calculated was 0.38 µg L-1. The preconcentration procedure was applied to determine trace levels of Cd in river water samples. The optimum preconcentration conditions are discussed herein.
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  • An Enrichment Method of Molybdenum on a Cellulose Nitrate Resin for the Determination by Electrothermal Atomic Absorption Spectrometry Coupled with the Resin Suspension Injection
    Isoshi NUKATSUKA, Yutaka SHIMIZU, Kunio OHZEKI
    2004 Volume 20 Issue 7 Pages 1033-1036
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1033
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    Cellulose derivative resin (CDR) suspensions containing resin particles of cellulose nitrate (CDR(CN)), cellulose acetate (CDR(CA)), or cellulose triacetate (CDR(CTA)) were prepared as the sorbent for resin suspension injection (RSI) electrothermal atomic absorption spectrometry (ETAAS), in which fine resin particles holding a desired trace element were directly injected into the graphite tube as the suspension. To compare the sorption ability, the distribution ratios of the Mo(VI)-phenylfluorone complex were measured between the aqueous phase and the sorbents, including the CDRs mentioned above and the finely divided anion exchange resin (AR). The results showed that the sorption ability decreases in the following order: CDR(CN) ≥ AR > CDR(CA) ≥ CDR(CTA). It was concluded that CDR(CN) was able to extract more than 98% of Mo(VI), and was suitable for RSI-ETAAS as well as AR. CDR(CN) was used for the determination of Mo in NIES certified reference materials, No. 10 Rice flour-unpolished; the results showed fairly good agreements between the analytical values and the certified values.
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  • A Novel Voltammetric Method for the Direct Determination of Copper in Complex Environmental Samples
    Jianjun XIA, Wanzhi WEI, Yanbo HU, Han TAO, Ling WU
    2004 Volume 20 Issue 7 Pages 1037-1041
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1037
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    A novel voltammetry with a modified gold electrode for the direct determination of copper in environmental samples, without any pretreatment, is proposed in this paper. A porous disorganized monolayer was formed on the surface of the gold electrode by the self-assembly of mercaptoacetic acid (MAA), which could selectively permeate small molecules. Subtractive square wave anodic stripping voltammetry (SASV) was applied to determine copper, in which the underpotential deposition (UPD) of copper was used as the deposition step. The linear range was from 8 × 10-7 to 1 × 10-5 mol l-1 by the modified electrode in the presence of human serum albumin, and the determination was not interfered with common metal ions. Copper in a real environmental sample was successfully detected.
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  • New Plastic Membrane and Carbon Paste Ion Selective Electrodes for the Determination of Triprolidine
    S. I. M. ZAYED
    2004 Volume 20 Issue 7 Pages 1043-1048
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1043
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    Triprolidine (Trip) ion selective electrodes of three types: the conventional polymer membrane (I), graphite coated electrode (II) and carbon paste electrode (III), have been prepared, based on the ion pair of triprolidine hydrochloride with sodium tetraphenylborate. The electrodes exhibit a linear response with a mean calibration graph slope of 56.12, 55.00 and 54.32 mV decade-1 at 25°C for I, II and III, respectively, within the concentration ranges 1.96 × 10-5 - 1.00 × 10-2 M for I and 3.84 × 10-5 - 1.00 × 10-2 M for II and III. The detection limits are 1.13 ± 0.13 × 10-5, 1.70 ± 0.06 × 10-5 and 1.78 ± 0.05 × 10-5 M for the three electrodes, respectively. The change of pH within the ranges 4.85 - 8.75 and 4.70 - 8.50 for I and III, respectively, did not affect the electrode performance. The standard electrode potentials were determined at different temperatures and were used to calculate the isothermal coefficient of the electrode. The electrodes showed a very good selectivity for Trip with respect to a large number of inorganic cations and compounds. The standard addition method was applied to the determination of TripCl in pure solution, pharmaceutical preparations, and urine samples.
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  • Enhanced Reduction and Determination of Trace Thyroxine at Carbon Paste Electrode in the Presence of Trace Cetyltrimethylammonium Bromide
    Chengguo HU, Qiong HE, Qing LI, Shengshui HU
    2004 Volume 20 Issue 7 Pages 1049-1054
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1049
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    The electrochemical response of thyroxine (T4) at a carbon paste electrode (CPE) in the presence of cetyltrimethylammonium bromide (CTAB) was investigated. It gave a well-defined oxidation peak at 0.80 V and a sensitive reduction peak at 0.40 V. Compared with the indiscernible signal in the absence of CTAB, the reduction current of T4 at CPE was greatly enhanced in the presence of CTAB, due to the interactions between T4, CTAB and the hydrophobic electrode surface. The electrode process of T4 was explored by cyclic voltammetry and chronocoulometry. The effect of surfactants on the reduction reaction proved that bromide ions (Br-) in CTAB might form special ion complexes with T4 via a special interaction with the iodine atoms on T4, which would activate the reduction of T4. The sensitive and selective reduction of T4 in this system was applied to the determination of T4 in drugs; a detection limit of 6.5 × 10-9 M was obtained (σ = 3).
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  • A Chitosan-Multiwall Carbon Nanotube Modified Electrode for Simultaneous Detection of Dopamine and Ascorbic Acid
    Lingyan JIANG, Chuanyin LIU, Liping JIANG, Zhen PENG, Guanghan LU
    2004 Volume 20 Issue 7 Pages 1055-1059
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1055
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    A chemically modified electrode based on a chitosan-multiwall carbon nanotube (MWNT) coated glassy carbon electrode (GCE) is described, which exhibits an attractive ability to determine dopamine (DA) and ascorbic acid (AA) simultaneously. The modified electrode exhibited a high differential pulse voltammetry (DPV) current response to DA at 0.144 V and AA at -0.029 V (vs. SCE) in a 0.1 mol l-1 phosphate buffer solution (pH = 7.2). The properties and behaviors of the chitosan-multiwall carbon nanotube modified electrode (MC/GCE) were characterized using cyclic voltammetry (CV) and DPV methods. The mechanism for the discrimination of dopamine from ascorbic acid at MC/GCE is discussed. The linear calibration range for DA and AA were 5 × 10-7 mol l-1 to 1 × 10-4 mol l-1 (r = 0.997), and 5 × 10-6 mol l-1 to 1 × 10-3 mol l-1 (r = 0.996), respectively. The MC/GCE showed good sensitivity, selectivity and stability.
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  • Preparation of a New Type of Fiber Adsorbent Attached with Silica Microparticles
    Takao TSUDA, Mahoro HISANAGA, Takanori INAGAKI, Shinya KITAGAWA, Kanji ...
    2004 Volume 20 Issue 7 Pages 1061-1064
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1061
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    A new type of fiber adsorbent attached with silica microparticles was prepared. The silica microparticles were formed by the polymerization of silica oligomers on glass fibers, which were woven into a glass filter. The surface of the silica microparticles was chemically modified by bonding C18-ligands. SEM images indicated that the diameter of the uniform and spherical silica microparticles fixed on glass fibers was on the order of micrometers. It was confirmed that the glass filter adsorbent was effective for the adsorptive removal of toluene of low concentrations.
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  • Sensitive Determination of Domoic Acid Using High-Performance Liquid Chromatography with Electrogenerated Tris(2,2′-bipyridine)ruthenium(III) Chemiluminescence Detection
    Hitoshi KODAMATANI, Keiitsu SAITO, Nobumitsu NIINA, Shigeo YAMAZAKI, A ...
    2004 Volume 20 Issue 7 Pages 1065-1068
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1065
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    A new sensitive determination method of domoic acid based on the chemiluminescent reaction of tris(2,2′-bipyridine)ruthenium(III) has been developed. The method exhibited good reproducibility. The relative standard deviation of six replicate measurements was 1.6% for 10 ng ml-1. A calibration graph, based on a standard domoic acid solution, was linear over the range of 1 - 500 ng ml-1 (coefficient of correlation, r2 = 0.9995) and the detection limit was 8 pg (signal-to-noise ratio = 3) without any preconcentration and derivatization steps. This new method was successfully applied to a real sample of blue mussels spiked with 2 µg g-1 domoic acid.
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  • Direct Detection of a Phase Change in PdO/CeO2 Supported on χ-Al2O3 by Means of in situ High-Temperature Measurements of XRD and FTIR
    Eiji KANEZAKI, Suminori TANAKA, Kei-ichiro MURAI, Toshihiro MORIGA, Ju ...
    2004 Volume 20 Issue 7 Pages 1069-1073
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1069
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    Phase changes between PdO and Pd metal can be directly detected in PdO/CeO2 catalysts supported on χ-Al2O3 by means of in situ high-temperature measurements of X-ray diffraction and FT-IR in relation to the catalytic activity for the methane oxidation of microcrystalline PdO. Reversible changes in the solid phases are observed from PdO to Pd and Pd to PdO under O2-deficient and O2-excess atmospheres, respectively. Nanosizes of PdO and Pd crystallites, the distorted PdO crystal structure along the (110) plane, and also a distorted Pd metal crystal structure along the (200) plane as well as the large surface area elucidate the high catalytic activity for the methane oxidation of PdO/CeO2 catalysts prepared with an atomic ratio of Pd:Ce = 1:1.
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  • Terbium-Sensitized Fluorescence Method for the Determination of Pazufloxacin Mesilate and Its Application
    Shilv CHEN, Hongwu MA, Huichun ZHAO, Ruiqing FENG, Linpei JIN
    2004 Volume 20 Issue 7 Pages 1075-1078
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1075
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    A simple, rapid and highly sensitive fluorometric method for the determination of pazufloxacin mesilate (PZFX) is described. It is based on the formation of the complex [Tb(PZFX)2]3+, which shows the intensive characteristic bands of Tb3+. Optimum conditions for the determination were investigated. Under the optimum experimental condition, the fluorescence intensity responds linearly to the PZFX concentration in the range of 2.0 × 10-8 - 5.0 × 10-6 mol/l with a detection limit of 6.2 × 10-9 mol/l. The method has been successfully applied to the determination of PZFX in urine and serum samples.
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  • Simultaneous XRD-DSC Measurements of Water-2-Propanol at Sub-Zero Temperatures
    Yuko NISHIMOTO, Yoichi KANEKI, Akira KISHI
    2004 Volume 20 Issue 7 Pages 1079-1082
    Published: 2004
    Released on J-STAGE: December 07, 2004
    DOIhttps://doi.org/10.2116/analsci.20.1079
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    A simultaneous low-temperature X-ray powder-diffractometric (XRD)-DSC technique was applied to the solid state and melting process of frozen aqueous solutions of 2-propanol. 1H NMR spectra were also obtained at low temperatures. The chemical shifts of the CH3 proton and the CH proton can be classified into four temperature regions: higher than -20°C, around -20°C, -50 to -20°C, and lower than -50°C. In the XRD data, five small diffraction peaks for 2 θ at 21.0°, 25.2°, 27.8°, 31.1° and 32.1° can be attributed to the peritectic, while five diffraction peaks at 22.5°, 24°, 25.6°, 33.4° and 39.8° can be attributed to ice; these peaks are due to the hexagonal form of ice, which disappears upon melting. However, the diffraction peak at 33.4° showed a different pattern than the other peaks due to hexagonal ice. These results indicate that the temperature dependence of the diffraction peak at 33.4° for 2θ is related to the formation of hydrogen bonds between 2-propanol and water. The simultaneous XRD-DSC technique was effective for investigating this water-alcohol mixture at low temperatures.
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