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Tohru SAITOH, Toshihisa OHYAMA, Kiyoko TAKAMURA, Teruaki SAKURAI, Tosh ...
1997 Volume 13 Issue 1 Pages
1-4
Published: February 10, 1997
Released on J-STAGE: July 07, 2006
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When an aqueous solution of a water-soluble polymer, poly(
N-isopropylacrylamide) (PNIPAAm), was heated above 32°C, the polymer became insoluble, and then formed paste-like precipitates (polymer phase) having a very small volume fraction. A water-soluble cationic chelate, iron(II)-tris(1, 10-phenanthroline) [Fe(phen)
3]
2+, was well extracted into the polymer phase as the io
n-pair with perchlorate. On the basis of the volume fractions of the aqueous and polymer phases, the logarithmic distribution constant of the ion pair evaluated was 2.53±0.05, promising high efficiency in the concentration of the ion pair. Based on the spectra of 1-(4-hydroxyphenyl)-2, 4, 5-triphenylpyridinium hydroxide inner salt and 1-ethyl-4-carboxymethoxypyridinium iodide in the polymer phase, the polar parameters, E
T(1) and Kosower′s Z values of the PNIPAAm phase were 257 and 333kJ mol
-1. These results suggest that the solvent properties of the polymer phase correspond to those of alcoholic solvents, such as methanol or ethanol. The high extractability of the [Fe(phen)
3]
2+(ClO
4-)
2 ion pair was ascribable to the polar properties of the polymer phase.
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Toshinao ISHII, Aya SORITA, Masayoshi SAWAMURA, Hirozo KUSUNOSE, Hiroy ...
1997 Volume 13 Issue 1 Pages
5-9
Published: February 10, 1997
Released on J-STAGE: July 07, 2006
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Coomassie Brilliant Blue G-250 (CBBG) was bound to the reaction products of glutaraldehyde with various compounds containing amino group. The reaction products of acetaldehyde and malonaldehyde with the amines did not bind with CBBG, indicating that the binding was specific for the product of glutaraldehyde. The dye binding products rapidly formed in alkaline pH. Gel filtration chromatography indicated that a reaction product of more than 2 kDa has a dye- binding ability. The reaction product of glutaraldehyde with 6-aminohexanoic acid was separated with SP-Sephadex. CBBG was bound to the first eluted fraction from the column with highest affinity. The absorbance at 595nm by CBBG binding was linearly related to this lyophilized fraction at a concentration of up to 250μg/ml, suggesting its applicability to the determination of the reaction product of glutaraldehyde and amine. The present method should contribute to our understanding of the chemistry of glutaraldehyde associated with diverse fields, such as enzyme technology and biochemistry.
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Toshio TAKAYANAGI, Hiroki TANAKA, Shoji MOTOMIZU
1997 Volume 13 Issue 1 Pages
11-18
Published: February 10, 1997
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Ion association properties of four kinds of anionic divalent azo dyes were investigated in an aqueous solution containing hydrophobic quaternary ammonium ions. The dyes used in this study possessed a hydroxy and a sulfonate group, which existed as a divalent anion in an alkaline solution. In capillary electrophoresis measurements, the apparent electrophoretic mobility of the dyes decreased along with an increase in the concentration of quaternary ammonium ion (Q
+) in a migrating solution. Ion association constants of the dyes with Q
+, K
ass, were determined by a simulation method of the mobility change using a non-linear least square method, when 1:1 ion associates formed. The increase in log
Kass was about 0.07 log unit per one methylene group; that is, the hydrophobicity of a pairing ion played an important role in the ion association reaction in aqueous solutions, as well as ion association in solvent extraction systems. Nitro groups of the dyes slightly affected the ion association constants, whereas the position of the sulfonate group in the azo dyes showed a significant change in ion association constants.
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Akiko HOKURA, Tatsuya SEKINE
1997 Volume 13 Issue 1 Pages
19-26
Published: February 10, 1997
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By spectrophotometry and by a liquid-liquid distribution method, the rate and equilibrium of the association of 2- thenoyltrifluoroacetone (Htta) with trioctylphosphine oxide (TOPO) in carbon tetrachloride-aqueous 0.1mol dm
-3 perchlorate solution systems were studied. The effect of this association on the rate and equilibrium of the solvent extraction of copper(II) in the liquid-liquid system containing these extractants was examined. The associate of these reagents in carbon tetrachloride at equilibrium was concluded to contain one TOPO, one water, and one keto form Htta molecule. The change in the distribution ratio of Htta during the two-phase agitation was larger in the presence of TOPO. The extraction of copper(II) from the aqueous phase with Htta in the presence of TOPO was higher just after the start of two-phase agitation and it decreased gradually until the equilibrium was reached. The rate of this decrease of copper(II) extraction was explained in terms of the rate of decrease in the Htta and TOPO concentrations due to their association in the organic phase.
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Qiuquan WANG, Kin-ichi TSUNODA, Hideo AKAIWA
1997 Volume 13 Issue 1 Pages
27-31
Published: February 10, 1997
Released on J-STAGE: July 07, 2006
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The extraction chromatographic behavior of zirconium(IV) and hafnium(IV) was investigated using di(1-methylheptyl) methylphosphonate (DMHP) as a stationary phase in the media of hydrochloric acid-ammonium chloride by a batch method. Through a log-log analysis and the IR spectra the extractable species has been proposed to be (DMHPH
+)
2ZrCl
62- and (DMHPH
+)
2HfCl
62-. The quantitative separation of Zr(IV) and Hf(IV) with ratios of 1:1 to 100:1 from each other has been achieved by DMHP-extraction chromatography.
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Maria BALCERZAK, Katarzyna KOMAR, Elzbieta SWIECICKA, Krzysztof KASIUR ...
1997 Volume 13 Issue 1 Pages
33-36
Published: February 10, 1997
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Osmium and ruthenium can be selectively isolated from a mixture of the noble metals by distillation in the form of OsO
4 and RuO
4. In hydrochloric (or sulfuric) acid media and in the presence of iodide, OsO
4 is selectively reduced to osmium(IV) and the OsI
62- complex is formed. Quantitative conversion of Os(VIII) into this complex takes place in 0.8M I
- solutions and in 0.04M HCl (or 0.1M H
2SO
4) within 5 (or 10min), respectively. The OsI
62- complex reacts with trioctylamine ((C
8H
17)
3N) and the ion associate ((C
8H
17)
3NH
+)
2OsI
62- is formed. The ion associate can be isolated from aqueous solutions by extraction into carbon tetrachloride. Both the OsI
62- complex and the ion pair with trioctylamine can be used for spectrophotometric determination of osmium directly in aqueous solutions or after extraction into the organic solvent. Ruthenium does not interfere with the determination of osmium in the form of the OsI
62- complex.
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Susana CABREDO, Benjamin W. SMITH, James D. WINEFORDNER
1997 Volume 13 Issue 1 Pages
37-40
Published: February 10, 1997
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The fluorescence of Dy(III) and other lanthanides is enhanced when glucose is present in the solution and the solution has been heated (15min at 175°C). The experimental evidence suggests that this is due to energy transfer between the aldehyde formed when glucose is heated and Dy. This effect was used for glucose determination in aqueous solution. A detection limit of 7μM was obtained, with a linear response to 1mM.
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Junichi SHIDA, Shinichi MATSUZAKI
1997 Volume 13 Issue 1 Pages
41-45
Published: February 10, 1997
Released on J-STAGE: July 07, 2006
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A sensitive method based on preconcentration on a membrane filter with a finely pulverized anion-exchange resin has been developed for the determination of gallium in water samples by electrothermal atomic absorption spectrometry. Gallium (10-60)ng, in 20-500ml of a sample solution, was retained as a Pyrocatechol Violet complex anion on a resin at pH 5; the resulting resin was filtered through a membrane filter. A portion of the resin with the membrane filter (3mm in diameter) was inserted into a cuvette, and the absorbance of gallium was measured at 294.4nm. The relative standard deviations for five measurements at 30ng of gallium was 5%. The detection limit was 1.5ng of gallium in 500ml (3ngGa l
-1) of the water sample. The interference of various ions was studied, and the optimum conditions were developed for the determination of gallium in mine-drainage and river-water samples.
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Yoshiaki KURAUCHI, Hiroyoshi ONO, Bo WANG, Naoyoshi EGASHIRA, Kazuya O ...
1997 Volume 13 Issue 1 Pages
47-52
Published: February 10, 1997
Released on J-STAGE: July 07, 2006
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Chitosan, whose deacetylation degree was 0.95, was N-carboxymethylated and subsequently modified with 6-amino-6-deoxy-
β-cyclodextrin. The
1H NMR spectra of the carboxymethylated chitosan (NCMC) and the
β-cyclodextrin- modified NCMC (
β-CD-NCMC) showed introductions of ca. 8.4 of the carboxymethyl groups and 8.2 of
β-CD moieties per 10 units, respectively.
β-CD-NCMC was covalently attached to a macroporous silica gel and used as a stationary phase for chiral HPLC separations of 2, 4-dinitrophenyl-α-amino acids and related racemates. The chiral discrimination was influenced more strongly by the size of an alkyl group on the chiral center of the aliphatic amino acids, compared to a Cyclobond I bearing monomeric
β-CD molecules. The distance between two aromatic moieties on the aromatic amino acids and related racemates was also discriminated. The strict recognition required the high substitution degree of the
β-CD moiety, permitting us to propose a simultaneous inclusion of the 2, 4-dinitrophenyl group and another aromatic substituent or an alkyl group with a proper size into the two adjacent CD cavities on the polymer chain.
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Mitsuru IRIKURA, Teruo TANAKA, Akira TAKADATE, Shujiro GOYA, Masaki OT ...
1997 Volume 13 Issue 1 Pages
53-58
Published: February 10, 1997
Released on J-STAGE: July 07, 2006
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The fluorescence properties of 7-anilino-4-methylcoumarin-3-(
p)-benzoic acid (AMCBA) synthesized as a fluorescent probe were measured in various solvents and in the egg albumin (EA) solution. The fluorescence of AMCBA was significantly enhanced in the nonpolar solvents and in the egg albumin solution. The binding parameters of AMCBA to EA were estimated fluorometrically. AMCBA which bound to EA was competitively displaced by several
β-blockers and sulfonamide drugs. The binding parameters of
β-blockers and sulfonamides to EA were estimated by using a displacement method. A good correlation between binding constants of sulfonamides or
β-blockers to EA and those partition coefficients was observed. These data suggest that AMCBA is one of the useful fluorescent probes for studying the binding of drugs to polymeric pharmaceutical additives, including EA.
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Naofumi SATO, Kamon SHIRAKAWA, Keisuke SUGIHARA, Tosinori KANAMORI
1997 Volume 13 Issue 1 Pages
59-65
Published: February 10, 1997
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The described chemiluminescence method enables the determination of adenine. In a dimethylformamide solution of the products of a reaction between adenine and an alkylglyoxal derivative in the presence of an acid catalyst, chemiluminescence occurs when a sodium hydroxide solution is added. This method is highly sensitive, is specific to compounds containing adenine, and produces no chemiluminescent products whatsoever in reactions with guanine and other nucleic acid bases other than adenine. The detection range for adenine in this reaction was 1.0× 10
-2 to 1.0×10
-7M, and the detection limit 1.4×10
-8M (7.0×10
-14mol per assay). The combined use with polymerase chemical reaction amplification enabled as little as 10pg of DNA to be detected.
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Yoshihisa SANO, Kiyomi KIKUCHI, Kyoichi TADANO, Kazuko HOSHI, Yasuko K ...
1997 Volume 13 Issue 1 Pages
67-73
Published: February 10, 1997
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A simple and sensitive method is described for the determination of menaquinone-4 and its metabolite menaquinone-4 epoxide in human periosteal osteoblasts. The method is based on high-performance liquid chromatography/ atmospheric pressure chemical ionization mass spectrometry, using deuterated menaquinone-4 as an internal standard. Selected reaction monitoring (SRM) is employed for selectivity and sensitivity. This enables quantification in a short period of time (within 5min) over the extended ranges 1-1000ng/ml for menaquinone-4 and 2.5-5000ng/ml for menaquinone-4 epoxide with acceptable precision and accuracy. The method was used to determine both compounds in human osteoblasts, following incubation with menaquinone-4. It is suggested that menaquinone-4 is metabolized to menaquinone-4 epoxide in bone as well as in liver, indicating the drug has the same role in
γ-carboxylation of vitamin K dependent proteins in both tissues. It is expected that this method will contribute to elucidating the pharmacological mechanism of action of menaquinone-4 on bone metabolism.
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Jongki HONG, Jong-Shin YOO, Seung-Yong JUNG, Kang-Jin KIM
1997 Volume 13 Issue 1 Pages
75-82
Published: February 10, 1997
Released on J-STAGE: July 07, 2006
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The photodegradation of DDT in water was examined with a high-pressure mercury lamp. A total of 17 photodegradation products of DDT including DDD, DDE and DDMU were identified by gas chromatography-mass spectrometry (GC-MS). Mass spectrometric analyses were done with electron impact (EI), methane positive chemical ionization (PCI) and electron capture negative ion chemical ionization (ENCI). The degradation rate of DDT in the presence of acetone was measured against the irradiation time. After the irradiation for 10min, 80% of DDT was converted into a number of products, including DDD, DDE, DDMU and dichlorobenzophenone, through reductive dechlorination, oxidation, isomerization and chlorination. On the basis of the identified products, the photodegradation pathways of DDT are proposed.
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Fumio MIZUTANI, Soichi YABUKI, Seiichiro IIJIMA
1997 Volume 13 Issue 1 Pages
83-87
Published: February 10, 1997
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An amperometric alcohol-sensing electrode was prepared by immobilizing alcohol oxidase (AOx) in a polyion complex membrane. Three kinds of aqueous solutions (poly(4-styrenesulfonate)-, AOx- and poly-L-lysine-containing solutions) were successively placed on the surface of a glassy carbon electrode and the electrode was allowed to dry. The anodic current (at 1V
vs. Ag/AgCl) of the enzyme electrode increased immediately after the addition of alcohols (
e.
g., ethanol), and reached a steady state within 5s. A linear response to ethanol was observed up to 0.4mM with a detection limit of 0.5μM. The polyion complex membrane showed permselectivity based on the solute size with a molecule weight cut-off of
ca. 100, which was very effective in suppressing the electrochemical interference by L-ascorbic acid and uric acid. The enzyme electrode was applied to the determination of ethanol in alcoholic drinks and soy sources. The electrode could be used for two weeks.
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Begoña ETXEBARRIA, Jos L. F. C. LIMA, Conceição B ...
1997 Volume 13 Issue 1 Pages
89-92
Published: February 10, 1997
Released on J-STAGE: July 07, 2006
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A flow injection system has been constructed for the "pseudo-titration" of chloride in electroplating baths with potentiometric detection. A silver ion-selective tubular electrode based on a homogeneous crystalline membrane was used. The FIA manifold has been developed and optimized in order to analyze samples with a chloride concentration range of 6.O×10
-2M to 2.5M. The proposed method is precise (relative standard deviation about 5%) and the results obtained by a simultaneous application of the FIA method and an automatic precipitation titration method, adopted as a reference technique, are in good agreement (
r=0.996). The sampling rate for the FIA manifold is 78 samples per hour.
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Takashi HASEBE, Junko NAGAO, Takuji KAWASHIMA
1997 Volume 13 Issue 1 Pages
93-98
Published: February 10, 1997
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A simultaneous flow injection method (FIA) was developed for the determination of acetylcholine and choline. This method is based on the determination of hydrogen peroxide (H
2O
2) produced from acetylcholine and choline by enzyme reactions. The determination of H
2O
2 was carried out by Co(II)-catalyzed luminol chemiluminescence (CL) reaction. The addition of sodium dodecylsulfate (SDS) in this CL system enhanced the CL intensity and sodium hydrogencarbonate showed an activating effect on the catalysis of Co(II) on the CL reaction. Interference of albumin for the CL reaction was removed by introducing an on-line dialysis unit and anion exchange column in the FIA system. A 10
-6mol dm
-3 level of acetylcholine and choline can be determined at a rate of 6 samples per hour (12 peaks). The method was successfully applied to the determination of acetylcholine and choline in a culture medium.
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Hai-Long Wu, Yu-Qi FENG, Masami SHIBUKAWA, Koichi OGUMA
1997 Volume 13 Issue 1 Pages
99-108
Published: February 10, 1997
Released on J-STAGE: July 07, 2006
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This paper describes an alternative algorithm for a simultaneous multicomponent analysis with three-mode three- dimensional array data generated by liquid chromatography with diode array detection (LC-DAD). The algorithm is mainly based on a combination of two-step Moore-Penrose pseudoinverse computations based on a truncated singular value decomposition (TSVD) and one-step direct bilinear decomposition. It is modeled with a series of pure or mixed reference samples and then used to analyze several unknown samples. The algorithm was evaluated by Monte-Carlo simulations of two synthetic LC-DAD data sets with different noise levels, and applied to the simultaneous determination of chlorobenzene and toluene by means of HPLC with a photodiode array detector. The obtained results show that the proposed algorithm is suitable for simultaneous determinations of several components, of which the chromatographic peaks and absorption spectra heavily overlap each other, provided that their three-dimensional data have trilinear properties.
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Masanori UEDA, Yoshinobu BABA
1997 Volume 13 Issue 1 Pages
109-112
Published: 1997
Released on J-STAGE: July 27, 2007
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Dongri JIN, Keiji TAKEHANA, Toshimasa TOYO'OKA
1997 Volume 13 Issue 1 Pages
113-115
Published: 1997
Released on J-STAGE: July 27, 2007
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Satoshi KUSAKABE, Yasushi ANAZAWA
1997 Volume 13 Issue 1 Pages
117-119
Published: February 10, 1997
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Qingyun CAI, Wei WEI, Ronghui WANG, Lihua NIE, Shouzhuo YAO
1997 Volume 13 Issue 1 Pages
121-125
Published: February 10, 1997
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Shoji IMAI, Masaki MINEZAKI, Yasuhisa HAYASHI, Chiaki JINDOH
1997 Volume 13 Issue 1 Pages
127-130
Published: February 10, 1997
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Anant P. ARGEKAR, Ashok K. SHETTY
1997 Volume 13 Issue 1 Pages
131-135
Published: February 10, 1997
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Hiroshi NIWA, Takashi YASUI, Akio YUCHI, Hiromichi YAMADA, Hiroko WADA
1997 Volume 13 Issue 1 Pages
137-140
Published: February 10, 1997
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Muneyuki KOHRI, Koichi SATO, Kunikazu IDE, Yoshinori INOUE, Haruno OKO ...
1997 Volume 13 Issue 1 Pages
141-143
Published: February 10, 1997
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Xue-Mei HUANG, Min ZHU, Lu-Yuan MAO, Han-Xi SHEN
1997 Volume 13 Issue 1 Pages
145-147
Published: February 10, 1997
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Conception S. MENDOZA, Tomoki SIGENOBU, Kenichi SODEYAMA, Satsuo KAMAT ...
1997 Volume 13 Issue 1 Pages
149-151
Published: February 10, 1997
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Takashi ISHIYAMA, Tatsuhiko TANAKA
1997 Volume 13 Issue 1 Pages
153-154
Published: February 10, 1997
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Yoshifumi AKAMA, Masatsugu KAJITANI, Toru SUGIYAMA, Akira SUGIMORI
1997 Volume 13 Issue 1 Pages
155-157
Published: February 10, 1997
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Masaaki IWATA, Kimiko KOBAYASHI, Sei TSUBOYAMA
1997 Volume 13 Issue 1 Pages
159-160
Published: February 10, 1997
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Concepcion S. MENDOZA, Satsuo KAMATA, Masaru KAWAMINAMI
1997 Volume 13 Issue 1 Pages
161-163
Published: February 10, 1997
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Takashi YOKOYAMA, Kenji KOHARA, Haruo AKASHI, Michio ZENKI
1997 Volume 13 Issue 1 Pages
165-166
Published: February 10, 1997
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