Eisei kagaku
Print ISSN : 0013-273X
Volume 21, Issue 4
Displaying 1-13 of 13 articles from this issue
  • HIROSHI OBA, TAKEO YAMAMOTO, YURIKO IWAMURA
    1975 Volume 21 Issue 4 Pages 169-172
    Published: August 31, 1975
    Released on J-STAGE: May 30, 2008
    JOURNAL FREE ACCESS
    As one of studies on the application of microbiological assay method for sulfate using E. coli B (H), determination of sulfur content in orange leaves was examined. Preparation of sample solution was as follows : Dried orange leaves were subjected to combustion in the presence of Mg (NO3)2·6H2O as an oxidizing agent at 800°for 1 hr. The residue was dissolved in 3 N HCl, neutralized with 3 N KOH, and the solution was passed through a column of Amberlite IR-120 (H+form). The effluent was used for the microbiological assay, and the results obtained were as follows : 1) It was possible to determine sulfur content in orange leaves by microbiological assay method using Mg (NO3)2·6H2O as an oxidizing agent. 2) This microbiological method gave small standard deviation (σ=3.8%) and accurate recovery (98.1-101.5%). 3) This proposed microbiological method will make it possible to determine sulfur content in orange leaves with the amount of a sample less than that in the gravimetric method.
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  • MARIKO SHIBAHARA, RIEKO YAMAZAKI, KAZUO NISHIDA, JYUNZO SUZUKI, SHIZUO ...
    1975 Volume 21 Issue 4 Pages 173-182
    Published: August 31, 1975
    Released on J-STAGE: May 30, 2008
    JOURNAL FREE ACCESS
    Distribution of Cu, Cr, Pb, Zn, Cd, Ni, and Hg in mud of Japanese rivers of first category was investigated with 178 mud samples from the mouth of 91 rivers, collected from August to September, 1973. The mud from the rivers in San-in district on the Japan Sea coast showed the lowest amount of all the heavy metals. The samples obtained from the Tsurumi or the Yodo River, near the industrial area, showed a very high concentration of all the metals. From the calculated values of the mean and standard deviation of each metal, it was considered that the higher these two values were, the more the river was polluted. The mean value of fignition loss was 5.03%. On the basis of this value, all the river were grouped into two classes. The first group had below 5.03% of ignition loss and the other with higher value. The mean and standard deviation of heavy metals of the former group were smaller than those of latter. Marked difference in concentration of Cd and Hg was observed between the two groups, while no difference was observed in the concentration of Ni. These results indicate that the mean of each metal in the first group river may be considered as approximate value for Japanese river mud in natural state.
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  • TOSHIYUKI MITSUI, YOSHIKAZU FUJIMURA
    1975 Volume 21 Issue 4 Pages 183-187
    Published: August 31, 1975
    Released on J-STAGE: May 30, 2008
    JOURNAL FREE ACCESS
    The concentration of hydrochloric acid and potassium iodide in Dragendorff's reagent was examined in order to obtain high sensitivity in the detection of alkaloids. As the samples, caffeine, morphine, procaine, cocaine, methamphetamine, ephedrine, chloroephedrine, methylephedrine, codeine, and dihydrocodeine were used. The optimum concentrations of hydrochloric acid and potassium iodide were determined by measuring the unreacted amount of bismuth in the reaction mixture of an alkaloid and the Dragendorff's reagent containing a definite amount of these two components when using caffeine, cocaine, procaine, codeine, and dihydrocodeine. For other alkaloids, however, the optimum concentration of the two components could not be determined.
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  • HIDEO ISONO, HIROSHI KOZUKA
    1975 Volume 21 Issue 4 Pages 188-193
    Published: August 31, 1975
    Released on J-STAGE: May 30, 2008
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    It is well known that 3-methylbutyrylurea is one of the metabolites of α-bromoisovalerylurea (bromvalerylurea), and the present experiment was carried out in order to find other metabolites of this hypnotic. After the administration of bromovalelrylurea to a rabbit, the urine was collected daily and passed through an anion-exchange resin column. As a result of thin-layer chromatography of the fractions eluted with dil acetic acid, a new Ninhydrin-positive spot was detected much more clearly in the first 24-hr urine than in any other cxcreted urine. From the first 24-hr urine, this substance was obtained as a pure crystalline compound. Mass spectra, infrared spectra, and other chemical analyses suggested that this Ninhydrin-positive spot is a cysteine derivative of bromvalerylurea. Finally, this compound was determined as 2-(2-amino-2-carboxyetylthio)-3-methylbutyrylurea by comparison with a synthetic compound.
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  • OSAMU SAKAGUCHI, KATSUSHI YOKOTA, SHINOBU TAKASHITA
    1975 Volume 21 Issue 4 Pages 194-198
    Published: August 31, 1975
    Released on J-STAGE: May 30, 2008
    JOURNAL FREE ACCESS
    Effect of synthetic or commercial detergents on purification process for activated sludge was investigated, and the following results were obtained. Considerable obstacle was obstacle on the purification of artificial sewage by the presence of linear alkylbenzene sulfonate (LAS) and it appeared remarkably in alkaline range (pH 8.2). Although 10 ppm of LAS did not effect the sewage purification by activated sludge, addition of more than 50 ppm markedly inhibited the removal rate of protein and LAS. It was found that biodegradation of LAS was inhibited by nutrients added in the sewage but, in spite of the presence of nutrients, higher fatty acid sulfate showed a considerabl high removal of detergent in the sewage. On the other hand about 90% of commercial synthetic detergents was degraded and, in the same manner, the presence of nutrients increased the amount of residual detergent in the supernatant after air-blowing. It was observed that TTC reduction of substrates with activated sludge was slightly inhibited by the addition of LAS in the reaction medium.
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  • TADAO SAKAI, ITSUKO OGAWA, MASAHIRO TSUBOUCHI, TOSHIHIKO KAMADA
    1975 Volume 21 Issue 4 Pages 199-203
    Published: August 31, 1975
    Released on J-STAGE: May 30, 2008
    JOURNAL FREE ACCESS
    A novel spectrophotometric method is proposed for the determination of procaine on the basis of solvent extraction. Tetrabromophenolphthalein ethyl ester (TBPE) anion, which is a monoacidic dye, is not extracted into 1, 2-dichloroethane layer from an aqueous solution. However, if TBPE is added to the aqueous solution containing procaine, the extract is colored red. Optimum pH range for the extraction of procaine from the aqueous solution is 8-9. The absorbance maximum of the extracts is at 580 nm, and the absorbance showed a linear relationship to the concentration of procaine in the aqueous solution over the range of 5×10-7 to 5×10-6 M. Procaine was found to form an associated ion-pair compound (1 : 1) with TBPE in 1, 2-dichloroethane. It seems that a kind of charge transfer complex is formed in the extract which shows a strong red color. On the other hand, when the aqueous phase contains quaternary ammonium salts, the extract is blue. In the quaternary ammonium system, it was found that an ion-pair extracted is readily dissociated in the organic phase and the blue color is attributed to the TBPE anion.
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  • SHIGERU SHIMOMURA, YASUHISA HAYASHI, HIDEYOSHI MORITA
    1975 Volume 21 Issue 4 Pages 204-208
    Published: August 31, 1975
    Released on J-STAGE: May 30, 2008
    JOURNAL FREE ACCESS
    Atomic absorption spectroscopic method for the determination of ppb levels of chromium in human urine was investigated by using the technique of a carbon tube atomizer to provide a simple and rapid means for the quantitative determination of total chromium. In order to establish the optimum conditions for the determination of chromium in a sample, various factors such as atomization efficiency including ashing or drying conditions, effect of acids, and matrices were studied. Under the optimum conditions established, the detection limit of the method for S/N = 2 was evaluated as 2×10-11 g and the linearlity of the absobance vs. concentration was good up to 3 ng of chromium. The precision was estimated to be 2.65% (relative standard deviation) from the results of 10 injections of 50 μl of synthetic urine solution containing 20 ppb of chromium, and the recovery of chromium added to synthetic and human urine samples before wet ashing was in the renge of 95-104%. Interference by matrices such as salts and organics in the samples could be eliminated by this technique of double atomization. Chromium concentration in urine from 13 normal subjects ranged from 0.4 to 26.4 ng/ml, which is similar to recent values obtained by several workers.
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  • RYUZO TAKESHITA, HIROSHI YOSHIDA
    1975 Volume 21 Issue 4 Pages 209-215
    Published: August 31, 1975
    Released on J-STAGE: May 30, 2008
    JOURNAL FREE ACCESS
    A reliable method for the determination of anion-active surfactants in natural and waste waters is described. The method consists of cleanup on an Amberlite XAD 2 column and determination by colorimetry using Methylene Blue. The sample was directly passed through the column, and the column was washed with 0.05 N sodium hydroxide solution. The surfactants taken up by the resin were eluted with a mixture of acetone and aqueous ammonia. After evaporation of acetone from the effluent, the surfactants were determined as sodium 4-(2-dodecyl) benzenesulfonate by the Methylene Blue method. Compared to the values obtained without the clean-up, those obtained by the proposed method were always lower. This indicates that some of the so-called Methylene Blue Active Substances were removed by the clean-up procedure. Even in samples containing surfactants at very low levels, the surfactants could be concentrated by loading a large amount of the sample over the column. Average recovery of sodium 4-(2-dodecyl) benzenesulfonate from water fortified at levels of 50 and 100 μg was 100.5%.
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  • HIDEO SAWADA, AKIRA HARA
    1975 Volume 21 Issue 4 Pages 216-220
    Published: August 31, 1975
    Released on J-STAGE: May 30, 2008
    JOURNAL FREE ACCESS
    A colorimetric determination for the toxicological analysis of cloxazolam, 10-chloro-11b-(2-chlorophenyl)-2, 3, 5, 6, 7, 11b-hexahydrobenzo [6, 7]-1, 4-diazepin [5, 4-b] oxazol-6-one, in pharmaceutical preparations, aqueous solution, and body fluids is described. The method is based on the Bratton-Marshall procedure for 2-amino-5, 2'-dichlorobenzophenone obtained by hydrolysis with 10% hydrochloric acid in a boiling water bath. Color of the azo dye, which was extracted with butanol saturated with water, was determined by spectrometry at 555 nm. The Beer-Lambert law was established over the range of 0.2-8.0 μg/ml. Cloxazolam in body fluid and aqueous solution was determined after extraction into ethyl acetate and then hydrolysis to the benzophenone derivatives. These results showed a very acceptable recovery and reproducibility in the order of 101.6% from aqueous solution, 97.1% from urine, and 99.9% from serum. This method can be applied to the determination of cloxazolam and its metabolites in body fluid for routine forensic toxicological analysis.
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  • HIROKO SATOH, YUKIO KUROIWA
    1975 Volume 21 Issue 4 Pages 221-224
    Published: August 31, 1975
    Released on J-STAGE: May 30, 2008
    JOURNAL FREE ACCESS
    The application of radioimmunoassay for using anti-phenobarbital antibody is described. 1) Barbiturate was identified by this method using 0.1 ml of serum drawn from a person in coma after an attempted suicide. 2) Phenobarbital or its metabolites excreted in the urine of a human receiving phenobarbital in a dose of 40 mg/44 kg can be detected for almost 3 weeks by this method. 3) Unknown minor metabolites were found from the urine of rat receiving phenobarbital by this method combined with thin-layer chromatography. These results were discussed in relation to the specificity of the antibodies.
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  • YOSHIAKI YAGITA, KUNIO TANAKA, TOSHIO SEKIGUCHI, MASAO KANDA, ISAO MAT ...
    1975 Volume 21 Issue 4 Pages 225-227
    Published: August 31, 1975
    Released on J-STAGE: May 30, 2008
    JOURNAL FREE ACCESS
    Atomic absorption spectrophotometry was applied instead of the current colorimetric determination (official) for the rapid determination of microamounts of lead in iron oxide used as a raw material for cosmetics and it was found that this spectrophotometric method was more accurate and speedy than the colorimetry and that the method of standard addition, using non-absorbing line of lead at 2802 Å, was more practical than the method using a masking agent for determination of lead contained in iron oxide. Procedure is as follows : Iron oxide (1-3 grams) is accurately weighed and dissolved in 30 ml of a mixture of hydrochloric acid (1→2)-nitric acid (29 : 1) and diluted to 50 ml with water. To 8 ml each of this iron oxide solution, 2 ml of the standard lead solution containing 0, 2, 4, or 6 μg/ml of lead is added and the content of lead is determined and calculated, using the difference between the absorbance valne at 2833 Å and 2802 Å. This method is recommended for the rapid determination of 1→50 ppm of lead in iron oxide and the coefficient of variation was about 3%.
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  • KIYOSHI EGAWA, CHIKAKO YOSHIHARA, KYOKO KITAHARA, YUMIKO NAKAYAMA, FUM ...
    1975 Volume 21 Issue 4 Pages 228-234
    Published: August 31, 1975
    Released on J-STAGE: May 30, 2008
    JOURNAL FREE ACCESS
    Effect of cosmetic bases on the antiseptic effect was examined with 7 kinds of 4 types of antiseptics and bactericides chiefly used in cosmetics and 14 kinds of 5 types of nonionic surfactants, on 3 strains of microorganisms. Experiments were made to see the effect of the structure and number of carbon atoms in the alkyl chain in nonionic surfactants on the antiseptic and bactericidal action of these agents, and the following results were obtained. 1) Nonionic surfactants were found generally to inhibit various antiseptics, and this inhibitive action was found to be the strongest in the polyoxyethylenesorbitan alkyl ester type. 2) Nonionic surfactants with larger numder of carbon atoms tended to have greater effect on the antiseptic and bactericidal actions. 3) The inhibitive concentration of nonionic surfactants paralleled the bactericidal concentration. 4) Inhibitive action of nonionic surfactants was found to become stronger with increasing moles of ethylene oxide added. 5) Inhibitive action of nonionic surfactants was found to vary with strain of microorganisms, and the gram-negative organisms used in the experiment tended to receive stronger inhibition than the gram-negative bacteria.
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  • YASUHIDE TONOGAI, YOSHIO ITO, MASAHIRO IWAIDA, HIROKO SANO
    1975 Volume 21 Issue 4 Pages 235-237
    Published: August 31, 1975
    Released on J-STAGE: May 30, 2008
    JOURNAL FREE ACCESS
    A method was developed for the separation and determination of three preservatives (fungicides), diphenyl (DP), o-phenylphenol (OPP) and thiabendazole (TB) in citrus fruits. The fruit was extracted with ethyl acetate, and the extract was concentrated. The solution, obtained by adding xylene to the concentrate and subsequently concentrating the mixture, was loaded on an alumina column (1.5×8 cm). After washing the column with hexane, DP was eluted with ethyl acetate and both OPP and TB with a mixture of aqueous ammonia and methanol (1 : 4). They were determined by submitting the fractions to gas-chromatography using two detectors, which were FID for the determination of DP and OPP and ECD for TB. Recoveries of DP (2 ppm), OPP (0.8 ppm), and TB (0.5 ppm) added to citrus fruits were 96.1, 95.4, and 93.7%, respectively. This method was successfully applied for the determination of three preservatives in lemons, oranges, and grapefruits.
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