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HIROTAKA OBANA, SHINJIRO HORI
1996 Volume 42 Issue 1 Pages
1-16
Published: February 29, 1996
Released on J-STAGE: May 30, 2008
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The analytical method for residual pesticides in foods is required to determine the target compounds at sub-ppm levels in various kinds of food matrix. Moreover, the number of possible residues including metabolites is over several hundreds, thus multiresidue analysis has become accepted by many analysts. Simplified extraction, minimum cleanup, and highly selective detection are quite important steps to accomplish such multi-analysis effectively. Extraction and cleanup procedures might be taken by the laboratory automation systems, instead of the manual methods, because the introduction of these systems can contribute to the improvement of quality control in analysis with reducing skilled manpower. This review describes matrix solid phase dispersion and supercritical fluid extraction in the extract section, and miniature size column and gel permeation chromatographies in the cleanup section. AED-GC and several kinds of GC-MS are also described as highly selected and sensitive detectors.
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KENICHIRO MINEGISHI, ATSUSHI TAKAHASHI
1996 Volume 42 Issue 1 Pages
17-27
Published: February 29, 1996
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The elimination and metabolism of 2, 2, 2, 3, 3-pentafluoropropanol (5-FP) were investigated in male and female rats for 7 d after a single oral administration at doses of 4, 40, and 400 mg/kg. 5-FP glucuronide and 2, 2, 3, 3, 3-pentafluoropropionic acid (5-FPA) as major metabolites were determined by head-space analysis using GC-MS in the selected ion monitoring-mode. 5-FP glucuronide and 5-FPA were found in urine and feces of both male and female rats. The cumulative excretion of 5-FP in the urine was 28.6-59.3% of the dose and only 0.46-1.28% in the feces in both sexes. A sex-related difference in urinary excretion of 5-FPA was observed in the two dose levels (4 and 40 mg/kg). The recoveries of 5-FPA in the urine of rats administered 5-FP were 10.7-11.9% in male and 33.0-38.2% in female by 7 d post treatment. The sex-related difference of biological half-lives (t
1/2) were also observed in some tissues such as liver, kidney and blood.
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YUZI TAKEKOSHI, SUSUMU KANNO, SHOZI KAWASE, TADASHI KIHO, SHIGEO UKAI
1996 Volume 42 Issue 1 Pages
28-31
Published: February 29, 1996
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We developed a method for forensic identification of minute fibers of 6-nylon and 6, 6-nylon by acid-catalyzed pyrolysis gas chromatography (PyGC). The fibers were pyrolyzed in the presence of phosphoric acid with a Curie point pyrolyzer directly connected to a gas chromatograph and a gas chromatograph/mass spectrometer. Phosphoric acid promoted production of specific volatile substances such as 3 isomers of hexenenitrile and ε-caprolactam from 6-nylon and adiponitrile from 6, 6-nylon. The phosphoric acid-catalyzed PyGC was able to identify a smaller amount of nylon fibers than the conventional non-catalyzed PyGC.
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HIDETOSHI SUGIYAMA
1996 Volume 42 Issue 1 Pages
32-37
Published: February 29, 1996
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The influence of sunlight irradiation on the chlorination of pyrene in soil was investigated in this work. The reaction products including original pyrene and chloropyrenes in soil after the irradiation were extracted with benzene-ethanol mixture (4 : 1, v/v) using a sonication technique. The extracts were then cleaned up using florisil column chromatography before GC/MS (SIM) determination. 1-Chloropyrene and dichloropyrene were formed when the soil spiked with pyrene was irradiated with sunlight in the ordinary atmospheric air. The formation of chlorinated pyrenes in soil was also found to be strongly dependent on the irradiation time, kind of soil and water contents. In addition, the formation of chlorinated pyrenes in soil was extremely depressed by the washing of the soil with water, indicating the involvement of water soluble substances as a chlorine source.
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HIDETOSHI SUGIYAMA
1996 Volume 42 Issue 1 Pages
38-43
Published: February 29, 1996
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In this study, the source of chlorine and the range of wavelength on the chlorination of pyrene in soil after the sunlight irradiation in ordinary atmospheric air were investigated. Chloride ions and pyrene were added to soil, and sunlight was irradiated. The reaction products including the original pyrene and chlorinated pyrenes in soil after the irradiation were extracted with a mixture of benzene and ethanol (4 : 1, v/v) using the sonication technique. The extracts were then cleaned up using florigil column chromatography before GC-MS (SIM) determination. The formation of chlorinated pyrenes in soil washed with distilled water was found to be strongly dependent on the concentration of chloride ions spiked in soil. It was found that the chlorinated pyrenes produced in air-dried soil after the sunlight irradiation were less than those in air dried soil spiked with chlorine ions and that the formation of chlorinated pyrenes in soil was extremely depressed by the wrapping with UV cut films. Consequently, it was also found that the chlorine source to produce chlorinated pyrenes in soil after the sunlight was mainly water soluble chloride ions and that the ultraviolet light of less than 380 nm mainly affected the formation of chlorinated pyrenes.
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SHUNJIRO OGAWA, KAZUHIRO NOZAWA, YUKIKO HANASAKI, TERUHISA HIRAYAMA
1996 Volume 42 Issue 1 Pages
44-52
Published: February 29, 1996
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Photocatalytic decomposition of polychlorinated biphenyl (PCB) with semiconductor, titanium dioxide (TiO
2), as a catalyst was investigated. TiO
2 aqueous suspension containing Kanechlor KC-300 (KC-300) as PCB (an aqueous suspension method) or TiO
2 powder coated with KC-300 (a coating method) was illuminated by a 1 kW xenon lamp. KC-300 (0.05 μg/ml) in the TiO
2 aqueous suspension (0.5 mg/ml) or 100 μg of KC-300 coated on 100 mg of TiO
2 powder were perfectly decomposed within 8 h and 4 h illumination, respectively. The decomposition rate of KC-300 in the coating method was higher than that in the suspension method. No decomposition was observed without illumination in the both methods. Hydroxyl radicals play a main role in the reaction of the suspension method. In the coating method, the presence of a small amount of water in TiO
2 powder promoted the decomposition rate. The results suggested that hydroxyl radicals are also reactive species in the coating method. All of 3 chlorine atoms in a KC-300 molecule were eliminated as chloride ions during the decomposition. The coating method is expected as a simple and effective method for the decomposition of PCB. Sunlight may be available for a light source.
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TSUTOMU OHNO, YUKO ITO, EIICHI MIKAMI, YOSHITOMO IKAI, HISAO OKA, JUNK ...
1996 Volume 42 Issue 1 Pages
53-59
Published: February 29, 1996
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A simple and rapid analysis of coal tar dyes in cosmetics and foods was established using reversed phase TLC/scanning densitometry. Forty-five kinds of coal tar dyes were able to be separated completely on reversed phase TLC plates by the complementary use of 4 solvent systems. Solvent system A : acetonitrile-methanol-5% aqueous sodium sulphate solution (3 : 3 : 10, v/v), solvent system B : methyl ethyl ketone-methanol-5% aqueous sodium sulphate solution (1 : 1 : 1, v/v), solvent system C : acetonitrile-methanol-5% aqueous sodium sulphate solution (1 : 1 : 1, v/v), solvent system D : acetonitrile-dichloromethane-5% aqueous sodium sulphate solution (10 : 1 : 5, v/v). Then we measured visible absorption spectra of coal tar dyes on the developed reversed phase TLC plates by scanning densitometry to identify these coal tar dyes. The proposed method was successfully applied to the identification of coal tar dyes in commercial products.
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KENICHIRO MORI, KOUICHI ITOH, SUKEJI SUZUKI, HIROSHI NAKAMURA
1996 Volume 42 Issue 1 Pages
60-66
Published: February 29, 1996
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Simple and reliable methods for the qualitative and quantitative analysis of ultraviolet (UV) absorbers in cosmetics by two dimension NMR (2D-NMR) were presented. The procedure consists of the following direct method for the samples containing more than 2% of UV absorbers and of the concentration method for the samples containing less than 2% of UV absorbers. The direct method : One hundred to 300 mg of cosmetics was weighed, placed into a test tube, and added 2 ml of saturated sodium chloride solution and 1 ml of the CDCl
3 solution containing 1% of pyrazine and 0.5% of tetramethylsilane. The mixture was shaken for 10 min. and centrifuged at 3000 rpm for 10 min. The CDCl
3 solution was transferred into a NMR tube. The concentration method : Five to 50 g of samples was weighed, placed into a 200 ml separating funnel, added 80 ml of saturated sodium chloride solution, and extracted with 30 ml of chloroform for 3 times. The chloroform layer was evaporated to dryness under reduced pressure. The residue was dissolved in 1 ml of the CDCl
3 solution for NMR measurements as described in the direct method. The
13C-
1H heteronuclear shift correlated NMR spectra (HETCOR) of UV absorbers in the CDCl
3 solution were measured for the simultaneous qualitative analysis of UV absorbers by the fingerprint identification, and the relative integral intensity in their
1H-NMR signals was used for the quantitative analysis using pyrazine as an internal standard. The proposed methods were successfully applied to the analysis of UV absorbers in cosmetics.
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MASANORI SEMMA, YOSHIO ITO, KATSUHIKO NAKAMURO, YASUYOSHI SAYATO
1996 Volume 42 Issue 1 Pages
67-73
Published: February 29, 1996
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Samples collected from the municipal drinking water of Kyoto, Osaka and Kobe were analyzed by ion chromatography to clarify the ionic components of the tap water and to know how reflect the characteristics of the Lake Biwa-Yodo River water quality, because the domestic drinking water of these cities was supplied after various purification steps for the renovation of the water of the same basin of the Lake Biwa-Yodo River. Ions in the samples were found to exist reflecting both the pollution of the raw water near the intake points of the water purification plants, and the reagents used in the water treatment process of each plant. Correlation matrices of the components of the detected ions revealed that NO
3- influenced by the human activities had high correlations with Na
+ and K
+. The increase of the amount of NO
3- contained in the tap water of the cities in the lower part of the basin indicated that NO
3- produced in the upper stream could not be removed by the usual purification process. It was also found in the present study that SO
42- increased stepwise in the tap water after every treatment process at the respective purification plants. However, the levels of the detected ions were far lower in the light of the Waterworks Law of Japan and WHO Guidelines for the quality of drinking water, indicating that the water renovation of the Lake Biwa-Yodo River has been well controlled.
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YUZI TAKEKOSHI, KIYOHITO SATO, SUSUMU KANNO, SHOZI KAWASE, TADASHI KIH ...
1996 Volume 42 Issue 1 Pages
74-86
Published: February 29, 1996
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By acid-catalyzed and alkali-catalyzed pyrolysis gas chromatography (PyGC), we analyzed synthetic fibers such as acrylic, 6-nylon, 6, 6-nylon, polyester, polyurethane, vinylon, polypropylene, acetate and viscose rayon, and natural fibers such as cotton, wool, silk and hemp. Fibers were analyzed in the presence of phosphoric acid, hydrochloric acid or sodium hydroxide aqueous solution as catalysts using a gas chromatograph and a gas chromatograph/mass spectrometer equipped with a Curie point pyrolyzer. These three catalysts produced increasingly some specific volatile substances from condensation-polymerized fibers such as cotton, hemp, viscose rayon, wool, silk, 6-nylon and 6, 6-nylon, compared with conventional non-catalyzed pyrolysis. From addition-polymerized fibers such as vinylon and acrylic, however, these catalysts produced decreasingly some specific volatile substances from the fibers. This results suggested that forensic identification of minute unknown fiber samples should be performed in the combination of conventional non-catalyzed and acid-catalyzed or alkalicatalyzed PyGC. Furthermore, we investigated the mechanism of acid-catalyzed and alkali-catalyzed pyrolysis, using deuterium-labeling acid and alkali in D
2O.
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TOMOHIRO YANO, YUMI OBATA, MIKAKO UCHIDA, TOMIO ICHIKAWA
1996 Volume 42 Issue 1 Pages
87-91
Published: February 29, 1996
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We investigated of the relation between oxidative stress on nuclei and spontaneous lung tumorigenesis in mice. An unsaturation index of fatty acids, the levels of active oxygen formed and thiobarbituric acid reactive substances in pulmonary nuclei of A/J strain were higher than those in the nuclei of C3H/He and C57BL/6Cr strains. In vitro active oxygen-dependent DNA nicking capacity via nuclear electron-transferring systems in lungs of A/J strain was also stronger than those in the lungs of the other two strains, while the nuclear α-tocopherol level in the A/J strain was lowest of the three. The differences of these parameters in the lungs among the three strains were in agreement with the strain differences of the lung tumorigenesis. These results suggest that the spontaneous development of lung tumors relates to some degree on the level of oxidative stress on the nuclei.
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HIDETOSHI SUGIYAMA
1996 Volume 42 Issue 1 Pages
92-95
Published: February 29, 1996
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An analytical method for the determination of 1-chloropyrene and dichloropyrene in soil samples was developed. These compounds were extracted from soil with benzene-ethanol mixture (4 : 1, v/v), using ultrasonic irradiation for 10 min, and then centrifugal separation at 3000 rpm. The supernatant was concentrated to dryness and re-dissolved into 3 ml of n-hexane. This solution was cleaned up by Florisil column chromatography, using n-hexane, and then n-hexane containing 15% diethyl ether. The latter fraction was concentrated to 2 ml for the GC/MS (SIM) determination of chlorinated pyrenes. The recoveries of 1-chloropyrene and dichloropyrene were 86 and 90%, respectively. The limits of the determination were 1 ppb and 0.5 ppb, respectively. This analytical method was also applied to the soil samples collected from Yokohama and Kawasaki cities.
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MISAKO TSUJI, MASAHITO HAYASHI, MASAHIRO MATSUOKA, TASUKU TAKAMATSU
1996 Volume 42 Issue 1 Pages
96-100
Published: February 29, 1996
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A non-suppressor ion chromatographic determination of sulfur in cosmetic products containing powders has been studied by converting sulfur to sulfate ion. The pretreatment of samples was almost the same as the one for gravimetric analysis, which includes a neutralization process with hydrochloric acid. But the removal of powders was necessary before the oxidation process due to their interference. It was also revealed that a large amount of chloride ion existing in the sample solution greatly affected characteristics of an eluent, and consequently eluted by incorporating a part of the sulfate ion. The method was modified to dilute the test solution to adjust the concentration of the chloride ions at less than 30 mM, and applied to the cosmetic products containing 2.7% sulfur. The results were satisfactory with R.S.D. of 1.14% and 99.1% recovery.
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HIROMI MORI, TAKAHIKO SATO, HISAMITSU NAGASE, MISA ANDOU, YOSHIMICHI S ...
1996 Volume 42 Issue 1 Pages
101-109
Published: February 29, 1996
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When the patients are carried into hospital and suspected to take pesticides, rapid identification of the intaked pesticides is necessary. We have investigated a rapid and simple screening method for the identification of pesticides in the case of toxicosis in general hospitals using thin layer chromatography (TLC). Thirty common pesticides were selected and analyzed with two developing solvent systems {I. n-hexane : acetone=4 : 1 (marker : methyl yellow), II. chloroform : acetone=9 : 1 (marker : methyl red)}. In this research, we used the silica gel plate mixed with a fluorescent substance (FM plate, WAKO), on which the pesticide spots emited a peculiar color by UV irradiation. This method does not need any toxic reagents or a draft chamber. Nineteen pesticides were detected with small detection limits of less than 0.5 μg and eleven pesticides were with those of 2.5-25μg. These detectable limits were adequate for the screening. Standard deviations of Rf values were very small. Pesticides added to water or synthetic gastric juice were efficiently recovered, and the time taken for the analysis was 1-1.5 h.
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RENTSE WANG, CHINTHIN WANG, KUOCHIN HUANG, TACHEN LIN, TENG CHANG PAN
1996 Volume 42 Issue 1 Pages
110-113
Published: February 29, 1996
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A simple and rapid analytical method for the determination of glucuronic and ascorbic acid in oral and pharmaceutical preparations was developed. This method not only showed good results for organic acids including citric, tartaric, malic, fumaric, latic, succinic, acetic and aspartic acid in oral and pharmaceutical preparations but also in health drinks. The detection limits of this method are about 0.04 to 0.1 mg within the coefficient of variation of about 6%. The entire analytical procedure can be accomplished within 40 min. without pretreatment. Using this method, a leading electrolyte solution was prepared with 7 parts of 0.1% polyvinyl alcohol in 0.01 N HCl, buffered at pH 3.0 with β-alanine and 3 parts of methanol. A solution of 0.01 N n-caproic acid was used as the terminal electrolyte. There was a two stage migration procedure : the first stage in a 10 mm i.d.×10 cm tube with 250 μA current for 10 min, and the second stage in a 5 mm i.d. 15 cm tube with 100 μA current for 10 min. The oven temperature was kept at 25°C. The nitrogen carrier gas was introduced at 0.25 kg/cm
2 pressure.
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HIROYASU YAMAZAKI, YOKO TOYODA, MEGUMI MATSUO, TAKAKO YAMAGUCHI, YASUO ...
1996 Volume 42 Issue 1 Pages
P1
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YASUJI HOJO, SAKIKO YANO
1996 Volume 42 Issue 1 Pages
P2
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SHIGETADA KOZAI, YASUTAKA KOZAKI, HISAO MATSUMOTO
1996 Volume 42 Issue 1 Pages
P3
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TETSUSHI WATANABE, TERUHISA HIRAYAMA, JOELLEN LEWTAS
1996 Volume 42 Issue 1 Pages
P4
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KAZUAKI KAWAI
1996 Volume 42 Issue 1 Pages
P5
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HIDETO JINNO, NAOKO HATAKEYAMA, NOBUMITSU HANIOKA, REIKO YODA, TETSUJI ...
1996 Volume 42 Issue 1 Pages
P6
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MASAO SATO, MIKIKO HAMAYA, JUNKO YAMAKI, CHIHARU TOHYAMA, M.D. APOSTOL ...
1996 Volume 42 Issue 1 Pages
P7
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IKUE ASAHI, MASAO KOYAMA, NOBUMASA IMURA, AKIRA NAGANUMA
1996 Volume 42 Issue 1 Pages
P8
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NARUMI SUGIHARA, TATSUYA SUETSUGU, KOJI FURUNO
1996 Volume 42 Issue 1 Pages
P9
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TOSHIHIDE SUZUKI, MIHO KOMATSU, HIDEO ISONO
1996 Volume 42 Issue 1 Pages
P10
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HITOSHI HARADA, IKUKO CHIBA, YASUNOBU SUKETA
1996 Volume 42 Issue 1 Pages
P11
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KEIZO UMEGAKI, HIROMI URAMOTO, JUNKO SUZUKI, TAKATOSHI ESASHI
1996 Volume 42 Issue 1 Pages
P12
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TOMOKO TAKEISHI, KAZUKO HATANO, KOJI ARIZONO, TOSHIHIKO ARIYOSHI
1996 Volume 42 Issue 1 Pages
P13
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YUICHIRO KAYANO, KAZUHITO WATANABE, TAMIHIDE MATSUNAGA, IKUO YAMAMOTO, ...
1996 Volume 42 Issue 1 Pages
P14
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KENICHIRO OGURA, TAKAHITO NISHIYAMA, HARUHIRO OKUDA, AKIRA HIRATSUKA, ...
1996 Volume 42 Issue 1 Pages
P15
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ATSUKO ADACHI, RIEMI SAWADA, KYOKO SHIDA, EIKO NAKAMURA, TADASHI KOBAY ...
1996 Volume 42 Issue 1 Pages
P16
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MASAKI WATANABE, MASAKATSU TEZUKA
1996 Volume 42 Issue 1 Pages
P17
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YASUMITSU OGRA, MASAYOSHI OHMICHI, KAZUO T. SUZUKI
1996 Volume 42 Issue 1 Pages
P18
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JINKO SAWASHITA, YUKA KODAMA, ATSUSHI TAKEDA, SHOJI OKADA
1996 Volume 42 Issue 1 Pages
P19
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ATSUSHI MISHIMA, CHIKA YAMAMOTO, YASUYUKI FUJIWARA, MICHIKO SAKAMOTO, ...
1996 Volume 42 Issue 1 Pages
P20
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YASUYUKI FUJIWARA, SHIGERU SAKURAI, MICHIKO SAKAMOTO, TOSHIYUKI KAJI
1996 Volume 42 Issue 1 Pages
P21
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SHINO HOMMATAKEDA, MASAMI ISHIDO, YOSHITO KUMAGAI, NOBUHIRO SHIMOJO
1996 Volume 42 Issue 1 Pages
P22
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MAKIKO ITOH, MASAYOSHI OHMICHI, KAZUO T. SUZUKI
1996 Volume 42 Issue 1 Pages
P23
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YASUJI HOJO, AYAKO OKADO
1996 Volume 42 Issue 1 Pages
P24
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IPPEI NAKAGAWA, KYOKO MIURA, NOBUMASA IMURA
1996 Volume 42 Issue 1 Pages
P25
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YOSHITO KUMAGAI, REIKO URANAKA, SAHO MIZUKADO, SHINO HOMMA-TAKEDA, NOB ...
1996 Volume 42 Issue 1 Pages
P26
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MEGUMI YAMAMOTO, ATSUHIRO NAKANO, HIDEMITSU HOU, KUNIHIKO NAKAMURA, TE ...
1996 Volume 42 Issue 1 Pages
P27
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TATSUMI ADACHI, AKIRA YASUTAKE, KIMIKO HIRAYAMA
1996 Volume 42 Issue 1 Pages
P28
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SHINJI YONEDA, IZUMI SADAKATA, MASAYOSHI OHMICHI, KAZUO T. SUZUKI
1996 Volume 42 Issue 1 Pages
P29
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MICHIKO SAKAMOTO, IWAO FUKAMI
1996 Volume 42 Issue 1 Pages
P30
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HIROAKI SHIRAKURA, MIHO ISHII, HIROSHI KUMAGAI, TOSHIAKI KOIZUMI, KAZU ...
1996 Volume 42 Issue 1 Pages
P31
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MASANORI SEMMA, YOSHIO ITO, KATSUHIKO NAKAMURO, YASUYOSHI SAYATO
1996 Volume 42 Issue 1 Pages
P32
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KIYOYUKI WATANABE, KUNIO OKADA, TAKASHI KATSU
1996 Volume 42 Issue 1 Pages
P33
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HIROYUKI KATAOKA, SEIKO SHINDO, MARI KURISU, MASAMI MAKITA
1996 Volume 42 Issue 1 Pages
P34
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SHIGEYUKI KITAMURA, KIYOSHI TATSUMI
1996 Volume 42 Issue 1 Pages
P35
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