Analytical Sciences

Report on the 57th Symposium on Analytical Chemistry

held in Matsuyama

Takashi MAEKAWA

1996 年 12 巻 4 号 p. 543-544
発行日: 1996年
公開日: 2007/07/27

DOIhttps://doi.org/10.2116/analsci.12.543

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Ferrocyanide-Templated Resins Prepared by Surface Template Polymerization

Isamu FUJIWARA, Mizuo MAEDA, Makoto TAKAGI

1996 年 12 巻 4 号 p. 545-549
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.545

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The ferrocyanide-templated resin was prepared by the "surface template polymerization method", using ferrocyanide ion as a template, oleylamine as a functional surfactant monomer and divinylbenzene as a matrix-forming monomer. Decyltrimethylammonium chloride (DTAC; quarternary ammonium salt) was found to be suitable as an auxiliary surfactant, when preparing the templated resin: DTAC stabilized the emulsion and was easily removed from the resin by washing with alkaline solution after the polymerization. The templated resin adsorbed ferrocyanide ions about 2 times as much as the non-templated resin. Although the structure of the complex between ferrocyanide and amino groups on the resin surface remains for further study, we found preparation conditions of the anion-templated resin using oleylamine and DTAC.

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Simultaneous Analysis of Enantiomeric Amino Acids Based on Derivatization with (S)-(+)-2-t-Butyl-2-methyl-1, 3- benzodioxole-4-carboxylic Acid and High-Performance Liquid Chromatography

Eigo ITOH, Yoshihiro NISHIDA, Yukie TOGASHI, Hiroshi OHRUI, Hiroshi ME ...

1996 年 12 巻 4 号 p. 551-556
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.551

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The fluorescent chiral derivatizing agent in the title, (S)-TBMB carboxylic acid, was applied for highly sensitive HPLC analysis of enantiomeric amino acids. Enantiomeric amino acids derivatized with the agent could be separated as the diastereomers on ODS (C-18) column and determined in less than 0.05 picomole amounts owing to the strong fluorescent chromophore of the reagent (Ex=310nm, Em=380nm). Three types of HPLC conditions with different pH values were proposed for the group analysis of amino acids: pH=5.7 for the simultaneous analysis of all amino acids, pH=4.6 for the selective analysis of polar amino acid derivatives and pH=6.0 for that of less polar ones.

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Determination of Dinophysis Toxin-3 by the LC-LC Method with Fluorometric Detection

Kazuaki AKASAKA, Hiroshi OHRUI, Hiroshi MEGURO, Takeshi YASUMOTO

1996 年 12 巻 4 号 p. 557-560
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.557

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A highly sensitive HPLC method for the determination of acid dinophysis toxins-3 (DTX-3s; 7-O-acyl-35-methylokadaic acids) by labeling 2-(anthracene-2, 3-dicarboximido)ethyl trifluoromethanesulfonate (AE-OTf) has been reported. The digestive glands of mussels or scallops were homogenized with 2-propanol, followed by extraction with hexane/ethyl acetate. After evaporation of the solvent, they were labeled with AE-OTf in dry acetonitrile. Then, after cleaning up with a silica-gel short column, the fluorescent derivatives were injected into an HPLC system. In this system, the derivatives were at first separated on a phenylated silicagel column; then, only the target fraction was introduced into a separation column (an ODS column) by a valve device for switching the column. The 7-O-palmitoyl DTX-3 derivative could be determined in the range of 1.4-284fmol (1.5-300pg) on the column. The detection limit was 0.57fmol (0.6pg, S/N=3).

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Cis-Trans Isomerization of Proline Dipeptides during Liquid Chromatography: Kinetic Analysis of the Elution Profile

Takashi NISHIKAWA, Yoshinori HAYASHI, Satomi SUZUKI, Hiroaki KUBO, Hid ...

1996 年 12 巻 4 号 p. 561-564
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.561

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A proline dipeptide, Leu-Pro, was eluted on a reversed-phase liquid chromatographic column with UV detection. Since this peptide undergoes cis-trans isomerization, various chromatographic profiles were produced. With the column kept at a low temperature, two peaks were produced, corresponding to the cis- and the trans-form. With elevation of column temperature or with increase of retention time, the peak area of the non-isomerized molecules was decreasing while the area corresponding to the isomerized molecules was increasing in a complementary manner. With further temperature elevation or with further retention time increase, only a broad peak of the isomerized molecules was produced. We demonstrate that the isomerization velocity could be estimated from the chromatograms and that the peak height of the isomerized molecules was proportional to the square root of retention time. Three other X-Pro dipeptides (Ala-Pro, Val- Pro, Phe-Pro) showed similar chromatographic behavior that was characteristic for reversible isomerization between two forms.

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Enzyme Immunoassay for Ursodeoxycholic Acid 7-N-Acetylglucosaminides in Human Urine

Toshifumi NIWA, Kazuhiro FUJITA, Toko KASUYA, Shigeo IKEGAWA, Junichi ...

1996 年 12 巻 4 号 p. 565-568
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.565

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A specific enzyme immunoassay (EIA) for ursodeoxycholic acid 7-N acetylglucosaminides (UDCA-7-NAGs), novel metabolites of ursodeoxycholic acid, has been developed. The EIA was based upon antisera elicited against the glycine conjugated UDCA-7-NAG-bovine serum albumin conjugate and horseradish peroxidase-labeled-UDCA-7-NAG. The sensitivity was significantly improved by the utilization of the bridge heterologous combination system. An appropriate dose response curve of EIA for glycine conjugated UDCA-7-NAG was obtained in the range of 0.3-6ng/tube. The specificity of ETA proved to be satisfactory in terms of cross-reactivities to related bile acids. The proposed method is useful for the determination of UDCA-7-NAGs in human urine with acceptable reliability.

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Equilibrium Study on Interactions between Proteins and Bile-Salt Micelles by Micellar Electrokinetic Chromatography

Tohru SAITOH, Teruyuki FUKUDA, Hirofumi TANI, Tamio KAMIDATE, Hiroto W ...

1996 年 12 巻 4 号 p. 569-573
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.569

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Interactions between proteins and bile-salt micelles were evaluated on the basis of the binding constants, which were obtained from the migration of proteins in micellar electrokinetic chromatography. The binding constants, K_b=[P_b]/ ([P_w][B]), where [P_b] is the concentration of a protein binding with a bile-salt, [P_w] free protein concentration, and [B] the concentration of bile salt present in the micelles, were successfully determined from the slope of a linear curve of the capacity factor (k′) of the protein against [B]. The binding constants were almost identical to those obtained by a gel- filtration method. The value of K_b increased with increasing the hydrophobicity of the bile salt or that of the protein.

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Separation and Direct Photometric Determination of Inorganic Anions by Capillary Zone Electrophoresis Using Suppressed Electroosmosis

Toshio TAKAYANAGI, Eiko WADA, Shoji MOTOMIZU

1996 年 12 巻 4 号 p. 575-579
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.575

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A simple, sensitive and separative method for the photometric determination of inorganic anions was developed on the basis of suppressed electroosmosis by using a common silica capillary and a simple migrating solution. During the analysis of analyte anions by capillary zone electrophoresis, electroosmotic flow in a silica capillary was suppressed by using low-pH migrating solutions containing sodium sulfate. The stacking effect of sulfate ion was utilized for analyte concentration. Four kinds of inorganic analyte anions examined were detected in sharp signals, and the separation of a nitrate and a nitrite ion was improved by using the low-pH migrating solution with no decrease in detection sensitivity. Calibration graphs for nitrate and nitrite ions showed good linearity in the concentration ranges from about 10^-5 to 10^-4mol dm^-3, with the detection limit for nitrate ion 4×10^-6mol dm^-3. Separations of organic anions, such as aromatic sulfonate and carboxylate ions, were also examined; many of them were well separated by the proposed migrating solution. Those organic anions did not interfere with the determination of the inorganic anions.

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Rapid Electroconcentration in a Tube of 25-40 Microliters under a Relatively Low Applied Voltage

Shinya KITAGAWA, Tsutomu ARAGAKI, Takao TSUDA, Takatoshi MATSUMOTO

1996 年 12 巻 4 号 p. 581-586
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.581

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Electroconcentration can be performed using a very simple apparatus and a simple operational procedure. The apparatus is composed of one tube, two electrodes and a power supply. The total sample solution employed for electroconcentration was just 25-40μl. After a tube of silicone rubber (i.d. 1mm, 30-50mm long) was filled with a sample solution, an electric voltage was applied along the tube, and a charged solute was forced to migrate to the end of the tube. With an application of 200-400V for only 2-4min, the concentration of the solute was enhanced up to 10 times. In the present electroconcentration, the sample is concentrated in a few microliters. Electroconcentration by electrode transfer is also proposed.

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Electrospray Mass Spectrometric Detection of Unstable Rhenium Complexes as Reaction Intermediates of Photochemical CO₂-Fixation

Hisao HORI, Osamu ISHITANI, Kazuhide KOIKE, Koji TAKEUCHI, Takashi IBU ...

1996 年 12 巻 4 号 p. 587-590
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.587

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Reaction intermediates of CO₂-photofixation using [Re(bpy)(CO)₃PPh₃]⁺(bpy=2, 2′-bipyridine) have been studied by electrospray mass spectrometry. A triethanolamine (TEOA) complex, [Re(bpy)(CO)₃(TEOA)]⁺, was detected for the first time as a key intermediate. Electrospray mass spectrometry was found quite useful for detecting and identifying unstable photoreaction intermediates of rhenium complexes.

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Effect of Hydrogen Addition to the Discharge Gas in Radio-Frequency Argon Glow-Discharge Mass Spectrometry for Nonconducting Samples

Tomokazu TANAKA, Motoya MATSUNO, Jin-Chun WOO, Hiroshi KAWAGUCHI

1996 年 12 巻 4 号 p. 591-595
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.591

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The addition of a small amount of H₂ into Ar considerably decreased the signal intensity for a sintered zirconium oxide (ZrO₂) sample when the discharge was operated at an rf power less than 100W, while it increased the ion intensity of the analyte for a brass sample. Although the sputtering rate of the ZrO₂ sample varied with the concentration of added H₂, no apparent correlation between the sputtering rate and the ion intensity was observed. When the discharge was operated at 200W, the addition of H₂ significantly increased the ion intensity for the ZrO₂ sample. For a sintered silicon carbide (SiC) sample, a similar behavior of the ion signals was observed, though they changed from suppression to enhancement at an rf power lower than that for a ZrO₂ sample. This was probably due to the higher electric conductivity of SiC compared to that of ZrO₂. When He was added into Ar, the analyte-ion intensity varied similarly to the case of H₂. An increase in the ion intensity was also observed when N₂ or O₂ was added at a concentration range of 10-20wt% in Ar, although the behavior was observed for a discharge operated at a relatively high rf power of 200W.

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Experimental and Theoretical Analyses on Factors Affecting the Performance of Polypyrrole/Glucose Oxidase Biosensor: Permeability Aspect of Polypyrrole Film

Min-Chol SHIN, Hyun C. YOON, Hak-Sung KIM

1996 年 12 巻 4 号 p. 597-604
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.597

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The effects of film thickness and enzyme concentration in the electrodeposition solution on the analytical performance of polypyrrole/glucose oxidase (PPy/GOD) biosensor were investigated. The optimum film thickness which maximizes the catalytic current of the electrode was observed at a given enzyme concentration, and this optimum thickness moved down to a thinner region with increasing concentration of enzyme. On the basis of the above results, the conditions for electrochemical deposition of the polypyrrole films were optimized. Theoretical analyses were conducted to elucidate the experimental results. The effect of electrodeposition conditions on the analytical performance of the PPy/GOD biosensor was evaluated in terms of response characteristics, sensitivity, and operational stability.

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Multi-Element Determination by a Cold Neutron-Induced Prompt Gamma-Ray Analysis

Chushiro YONEZAWA

1996 年 12 巻 4 号 p. 605-613
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.605

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A non-destructive multi-element determination using a cold neutron-induced prompt γ-ray analysis (PGA) has been investigated. The elements H, C, N, Na, Mg, Al, Si, P, S, Cl, K, Ca, Ti, Mn, Fe, Co, Cd, Sm, Gd and Hg were determined by a comparative standardization using the cold neutron guided beams of JRR-3M (upgraded Japan Research Reactor No. 3). To accurately determine the amounts of elements, possible interferences by other elements and background counts were examined and evaluated. Many elements in several reference materials, such as geological, environmental, and biological samples, coal and fuel oil, were determined, and the accuracy and precision of a multi-element determination were estimated. Toxic elements as, such Cd and Hg, at μg/g levels were accurately determined in environmental samples. The detection ma limits in various trices were from 25 to 820ng/g for Cd, Sm and Gd, 1.1 to 820μg/g for H, Na, S, Cl, K, Ti, Mn, Co and Hg, and 0.031 to 10% for C, N, Mg, Al, Si, P, Ca and Fe.

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Quantitative Analysis of the Infrared Absorptivities of Nitric Acid Ices Aerosol Existing in Polar Stratospheric Clouds

T.-L. TSO, M.-T. LEU

1996 年 12 巻 4 号 p. 615-622
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.615

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The infrared absorptivities of nitric acid ices formed from vapors containing water and nitric acid were investigated by means of a Fourier-transform infrared spectrometer operated at a wavelength resolution of 1.0cm^-1 (triangular apodization). The solid films were prepared on the surface of a gold-coated, polished copper plate at a temperature of 153 K to 198 K. After collecting the infrared spectra, the substrates were vaporized and condensed into a U-tube for quantitative analyses of H₂O and HNO₃ using a quadrupole mass spectrometer. Amorphous forms of nitric acid ices and four crystalline hydrates (nitric acid monohydrate (NAM), nitric acid dihydrate (NAD), and nitric acid trihydrate (both α-NAT and β-NAT forms)) were identified and their infrared absorptivities measured. The infrared spectra were interpreted in terms of the known spectra of oxonium and nitrate ions. Possible implications for remote sensing and the analysis of polar stratospheric clouds using these infrared spectra are discussed.

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Determination of Arsenic and Selenium in River Water by Hydride Generation Inductively Coupled Plasma-Mass Spectrometry with High Resolution

Hisatake NARASAKI, Jun Yan CAO

1996 年 12 巻 4 号 p. 623-627
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.623

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Hydride generated in a mixing coil was separated in a gas-liquid separator which was closed with an electromagnetic pinch valve and then swept continuously into the torch of a high-resolution inductively coupled plasma-mass spectrometer. The system was operated with variable speed-peristaltic pumps by manipulating electromagnetic relays and a timer. Water vapor in the hydride gas was removed by inserting a glass trap immersed in an ice bath. Interference with transition matals was eliminated by using Chelex 100 resin. The detection limits (3 times the signal-to-noise ratio) of arsenic and selenium are 0.03 and 0.06ng/ml, respectively, at a resolution of 10000. The accuracies checked with biological standard reference materials obtained from the National Institute of Science and Technology (NIST), USA, and the National Research Council (NRC), Canada, were within the certified values. The arsenic and selenium contents in river water were determined by the present method.

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Nickel and Strontium Nitrates as Modifier for the Determination of Selenium in Urine by Zeeman Platform Graphite-Furnace Atomic Absorption Spectrometry

Yan-Zhong LIANG, Mei LI, Zhu RAO

1996 年 12 巻 4 号 p. 629-633
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.629

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A mixture of nickel and strontium nitrates has been proved to be suitable and feasible for the determination of selenium in urine by graphite-furnace atomic absorption spectrometry with respect to the thermal stabilization and minimization of urine matrix interferences. Thermal pretreatment temperature of 1400°C and 900°C can be utilized in aqueous standard solution and 1:3 diluted urine with the proposed modifier, respectively. The results demonstrate that nickel and strontium nitrate mixed modifier can significantly remove or depress troublesome interference caused by sulfate, phosphate and concomitant metal ions. The graphite furnace temperature program and modifier mass have been optimized. The amount of mixed modifier required for stabilizing selenium and suppressing the effect of urine matrix is markedly lower than those documented in the literature, which reduces the risk of graphite furnace contamination. The effects of different atomizer surfaces on the selenium sensitivity were compared in this work. Better recoveries were obtained for different urine samples in the presence of nickel and strontium nitrates.

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Elimination of Chemical Interference in the Determination of Cadmium by Flame Atomic Absorption Spectrometry

M. A. MOSTAFA

1996 年 12 巻 4 号 p. 635-640
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.635

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The interfering effects of some foreign species in a flame atomic absorption spectrometric determination of cadmium are discussed. The elimination of these interfering effects using 2.5×10^-3mol l^-1 ammonium pyrrolidine dithiocarbamate (APDC) and 0.05mol l^-1 KCN, each, was individually performed. The mechanism concerning their releasing effect is illustrated. A new analytical procedure has been elaborated for the determination of cadmium in its complexes and in synthetic mixtures.

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Speciation of Aluminum in Urine

Jun WU, Chao Yan ZHOU, Ming Keong WONG, Hian Kee LEE, Hua CHI, Choon N ...

1996 年 12 巻 4 号 p. 641-645
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.641

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A procedure has been developed for the speciation of aluminum in urine samples of four normal subjects fed required diet on two dates. Three fractions of aluminum species, i.e., labile monomeric ions, non-labile monomeric ions along with labile complexes, and non-labile complexes were classified and determined by the combination of ion-exchange (IE), fluorometric spectrometry and graphite-furnace atomic absorption spectrometry (GF-AAS) techniques. The results showed that the aluminum in urine was mainly in non-labile complex forms.

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Sensitive Spectrofluorometric Determination of Vanadium with Sodium 1, 2-Dihydroxyanthraquinone-3-sulfonate in Cationic Micellar Medium

Ana GARCÍA CAMPAÑA, Fermn ALS BARRERO, Manuel ROMÁ ...

1996 年 12 巻 4 号 p. 647-651
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.647

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A spectrofluorometric method is described for the determination of vanadium(V) based on its complexation reaction with sodium 1, 2-dihydroxyanthraquinone-3-sulfonate in presence of hexadecyltrimethylammonium bromide. The fluorescence is monitored at 607nm with excitation at 505nm. The experimental variables and interferences in this determination have been studied. The detection limit is 3.0ng ml^-1 and the linear range is between 10 and 1000ng ml^-1. The method has been applied to the determination of vanadium in clams and seawater with satisfactory precision.

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Determination of the Pesticide Carbaryl by Microemulsion Room-Temperature Phosphorescence in Real Samples

Antonio SEGURA CARRETERO, Carmen CRUCES BLANCO, Alberto FERNÁND ...

1996 年 12 巻 4 号 p. 653-657
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.653

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A room-temperature phosphorescence method for the determination of the pesticide carbaryl is described. The proposed method is based on the formation of a microemulsion obtained by mixing an apolar solvent with the surfactant sodium dodecyl sulfate as the micellar medium in the presence of thallium nitrate as the external heavy atom salt. To avoid the oxygen quenching, a sodium sulfite solution was used. A complete and exhaustive statistical analysis of experimental data by a multivariate optimization approach was performed to establish the optimum experimental variables. Good results have been obtained when the insecticide have been analyzed in synthetic and real samples.

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Electron Microscopic Observation of the Reduction Process of Indium Oxide to Indium Metal and on the Formation of a Palladium-Indium Intermetallic Compound in a Thermal Pretreatment Process in Graphite-Furnace Atomic Absorption Spectrometry

Kazuo YASUDA, Yoshihiro HIRANO, Takeo KAMINO, Toshie YAGUCHI, Kichinos ...

1996 年 12 巻 4 号 p. 659-663
発行日: 1996年
公開日: 2007/07/27

DOIhttps://doi.org/10.2116/analsci.12.659

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Determination of Urinary Creatinine by Liquid Ionization Mass Spectrometry

Yukio YOKOYAMA, Naoyuki OHMORI, Masahiko TSUCHIYA

1996 年 12 巻 4 号 p. 665-667
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.665

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Solid-Phase Spectrophotometric Determination of Titanium(IV) Using 4, 4′-Diantipyrylmethane

Isoshi NUKATSUKA, Risako SATOH, Yohko WADA, Kunio OHZEKI

1996 年 12 巻 4 号 p. 669-671
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.669

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Speciation of Water-Soluble Boron Compounds in Radish Roots by Size Exclusion HPLC/ICP-MS

Toshiro MATSUNAGA, Tadashi ISHII, Hisao WATANABE

1996 年 12 巻 4 号 p. 673-675
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.673

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Crystal Structure of 2-Amino-5-chlorobenzophenone

Nora L. VASCO-MENDEZ, Kaliyamoorthy PANNEERSELVAM, Enrique RUDINO-PINE ...

1996 年 12 巻 4 号 p. 677-678
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.677

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Molecular Structure of (1R*, 8S*)-9-Amino-2, 3, 5, 6, 7, 8- hexahydro-1H-cyclopenta[b]quinoline-1, 8-diol

Toshiya KOMATSU, Kimiko KOBAYASHI, Tadashi NAKATA, Masashi YANO, Ken-i ...

1996 年 12 巻 4 号 p. 679-680
発行日: 1996/08/10
公開日: 2006/07/04

DOIhttps://doi.org/10.2116/analsci.12.679

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