The Organisation for Economic Co-operation and Development (OECD) is an inter-governmental organisation which is composed of 24 industrialized countries in the western bloc. OECD aims at attaining economic growth in Member countries in terms of not only quantity but also quality. One of the important aspects of quality is protection of environment. OECD has made several achievements in the international control of chemicals, e.g., consolidated actions for PCBs, mercury and cadmium, Guidelines for Testing of Chemicals, Principles of Good Laboratory Practice (GLP), Minimum Premarketing Set of Data (MPD). The present work in OECD focuses on existing chemicals for which international co-operations are strongly needed in light of the number of chemicals and the size of necessary work for them. This article outlines the achievements and the present work of the Chemicals Programme in OECD.

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Several types of drinking-water organic residues, obtained by solvent extractions from XAD-2 resin and activated carbon columns after the passage of drinking water (10 m³), were tested for mutagenic activity in TA-98 and TA-100 strains with and without the addition of S9. Direct-acting mutagens and some substances toxic to the tester strains were found to be present in these organic residues. Thin-layer chromatographic (TLC) fractionations, using polyamide plates, coupled with bioassay for mutagenicity showed that some of the major mutagens present in the XAD-2-extractable organic residues were of intermediate polarity and some were nonpolar. In contrast, those mutagens found in carbon-ether-extractable residues behaved on the TLC plates as compounds with a wide polarity range, with the strongest mutagenicity appearing among the acidic substances. Mutagenicity of these residues was inactivated by incubation with 4-nitrothiophenol as a nucleophile, but no change in activity was observed following reaction with o-phenylenediamine as a trapping reagent for mutagenic α-carboxylic compounds. In addition, it was found that mutagenicity in these organic residues was rapidly lost following heating, light irradiation or addition to alkaline solutions.

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An ion-pair high performance liquid chromatographic method was described for the simultaneous determination of thiabendazole (TBZ), diphenyl (DP) and o-phenylphenol (OPP) in citrus fruits and for the high sensitive determination of TBZ in banana. The use of ion-pair reagents such as 1-laurylsulfate for TBZ enabled the separation of three fungicides from interfering peaks. The fungicides were chromatographed on a Finepack SIL C₁₈ column with acetonitrile-methanol-water (40 : 25 : 35) mixture adjusted pH to 2.5 containing 0.01 M sodium 1-laurylsulfate as mobile phase. The three fungicides in citrus fruits were detected by fluorescence detector set at excitation (Ex) 285 nm and emission (Em) 325 nm, and TBZ in banana was detected at Ex 305 nm and Em 350 nm. The recoveries of TBZ, DP and OPP added to citrus fruits were 94.1-98.0%, 90.1-93.0%, 92.0-95.0%, respectively, and the recovery of TBZ added to banana was 92.1-94.3%. The detection limits of DP, OPP and TBZ in citrus fruits were 0.5, 0.1 and 0.1 mg/kg, respectively, and the detection limit of TBZ in banana was 0.005 mg/kg.

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To evaluate the effect of the treatment by activated sludge, the concentration of chlorhexidine (CH) in hospital or domestic waste waters before or after pretreatment was determined, in addition to microbiological and physicochemical investigations. The following were clarified : 1) The numbers of coliform group and total count in hospital waste waters were less than those in domestic one. 2) Antimicrobial activity was not observed in the domestic waste waters, whereas observed in the hospital inflow ones. 3) No change in the values of pH, biochemical oxygen demand (BOD) and chemical oxygen demand (COD) of both waste waters was observed in the hourly or daily time-course, and the values of pHs in both waste waters were neutral or weakly basic. 4) The values of BOD and COD of outflow waste waters were less than those of inflow ones. From these findings, waste waters were found to be treated appreciably with activated sludge. 5) The determined value of CH in waste waters without pretreatment gave 0.12-0.60 μg/ml and 0.20-0.70 μg/ml by colorimetric and HPLC methods, respectively. These values were almost similar to those determined by the conventional methods. On the other hands, the determined values of CH in waste waters after pretreatment with hydrochloride and Celite gave 1.62-10.30 μg/ml by both methods. These values showed about 5-20 times those determined by the conventional methods. 6) The determined values of CH in inflow and outflow waste waters after the pretreatment described above gave 1.20-4.50 μg/ml and 1.40-3.60 μg/ml by each method, respectively. These results suggested that CH in waste waters was scarcely treated with activated sludge.

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We examined aerobic biodegradation of sodium linear alkylbenzenesulfonate (LAS), sodium alkyl sulfate (AS), sodium alkylpoly (oxyethylene) sulfate (AES), sodium alkylphenylpoly (oxyethylene) sulfate (NES), sodium α-olefinsulfonate (AOS), sodium salt of fatty acid (soap), alkyl poly (oxyethylene) ether (AE) and p-alkylphenyl poly (oxyethylene) ether (APE) by bacterial sources from sewage sediments. In the course of biodegradation, the production of CO₂ was determined as the final products of carbon sources. The relationship between chemical structure and biodegradability of surfactants was compared. In terms of the final extent of biodegradation, the results of the aerobic biodegradabilities of surfactants were as follows : (AS, LAS, AE, AES, soap, AOS)»APE>NES. AS, LAS, AE, AES, soap and AOS were degraded to CO₂ to the same extent as glucose, but the time required to reach the final extent varied from 5 to more than 15 d depending on the chemical structure of surfactant. On the other hand, APE and NES were extremely resistant to aerobic biodegradations.

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Simultaneous determination of nine kinds of triazine herbicides was described. The pesticides were extracted from the sample with acetone, diluted with 10% NaCl solution, and re-extracted with dichloromethane. The organic layer was concentrated and purified with Florisil column chromatography. Nine pesticides on the column were quantitatively recovered with 100 ml of ethyl ether-ethyl acetate (1 : 1) mixture solution after washing with 50 ml of hexane-ether (1 : 1) mixture solution. The eluate was concentrated and determined with a flame thermionic detector by gas chromatography. Recoveries of nine pesticides (prometone, propazine, atrazine, simazine, prometryn, ametryn, simetryn, dimethametryn, metribuzin) added to carrot, orange, soy bean and unpolished-rice at 0.5 ppm were within the range of 62.4-92.6%. The detection limit for each pesticide in the sample by the proposed method was 0.05 ppm.

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In order to carry out a rapid analysis of amino acids, proteins and related materials without troublesome pretreatment, application of pyrolysis gas chromatography (PGC) for these samples was investigated. Highly resolved pyrograms were obtained from these materials by using Curie point pyrolyser and fused-silica capillary column with moderate polarity. At first, PGC of 21 major L-α-amino acids was studied, and 18 of them were identified by using 1 μg of each sample. Secondly, PGC of protein samples, such as egg white lysozyme, wool fiber, etc. was examined. The major peaks observed on these pyrograms were well assigned, and it was possible to discriminate trace protein samples by comparison with the differences in the amino acid residues.

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The chlorpromazine in the human blood or urine was determined by GC/MS. Trace amounts of chlorpromazine in the human blood or urine could not be completely extracted with organic solvent. However, the extraction efficiency was about 98-102% when aqueous solution saturated with tri-n-propylamine was added to the blood or urine. The recommended procedures are as follows : Place 20 ml blood or urine containing less than 1000 ng of chlorpromazine, 15% sodium carbonate aqueous solution, 1 ml of aqueous solution saturated with tri-n-propylamine, and 10 ml of benzene in 50 ml separatory funnel. Shake it for 2 min and centrifuge for 2 min at 3500 rpm in a 50 ml centrifuge tube. Place 5 ml of the benzene phase, and 1 ml of n-tricosane benzene solution (573 ng/ml) as an internal standard. Concentrate benzene on a water bath to 0.3 ml at 80±5°C. Determine the chlorpromazine by GC/MS. The extraction efficiency was 98% when as little as 10 ng of chlorpromazine·HCl was tested. When the amount of chlorpromazine in the human blood or urine was less than 28.8 μg, the extraction efficiency of chlorpromazine was higher in the presence of tri-n-propylamine compared to that without the base.

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Mice were injected with organic solvents and fatty acids, and the concentration of metallothionein in the mouse tissues was determined. The following results were obtained. 1. The metallothionein concentration in the liver increased by the injections of n-heptane, n-hexane and benzene. 2. The Zn-thionein concentration increased to 323±44 μg/g after the injection of n-heptane injection, and the acute cadmium toxicity was prevented by pre-injection of n-heptane. 3. The concentration of metallothionein in the mouse liver increased by the injections of oleic acid and linoleic acid. These results demonstrate that the concentration of metallothionein in the mouse liver increased by the organic solvents and fatty acids.

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n-Hexane was injected s.c. into normal mice to examine its influences on metallothionein concentration, and the following results were obtained. 1. The metallothionein concentration in the mouse pancreas decreased dose-dependently after the injection of n-hexane. 2. Metallothionein-bound zinc in the pancreas decreased to 51% after the injection of n-hexane and a decrease of metallothionein-bound zinc was more than that of metallothionein-unbound zinc. 3. The concentration of zinc-induced metallothionein in the mouse pancreas decreased by the simultaneous injection of n-hexane, and cadmium-induced metallothionein also decreased by the preinjection of n-hexane. These results indicate that the metallothionein concentration in the normal mouse pancreas decreased by the injection of n-hexane.

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The behavior of reaction products formed by the ozonation of naphthoresorcinol and of eight carbonyl compounds which were identified in the reaction mixture of ozonated naphthoresorcinol was investigated. During ozonation of naphthoresorcinol, o-phthalic acid and muconic acid reached the maximum concentrations at the beginning of the ozonation, followed by maleic acid and glyoxal and finally by mesoxalic acid, oxalic acid and formic acid increased during further ozonation. No change of the concentration of glyoxylic acid was observed during the ozonation. The ozonation of the eight carbonyl compounds identified demonstrated the following degradation pathways. The ozonolysis of o-phthalic acid occurred through three pathways, leading to maleic acid, mesoxalic acid and glyoxal, which were further degraded to glyoxylic acid, oxalic acid and formic acid. However, muconic acid was not formed by the ozonation of o-phthalic acid and degraded by two pathways through each of maleic acid and glyoxal. Gas chromatography-mass spectrometry indicated that o-carboxy-α-hydroxycinnamic acid may be one of the intermediates to o-phthalic acid or muconic acid. The degradation mechanisms of naphthoresorcinol by aqueous ozonation are discussed on the basis of these results.

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The identification method for Legionella species which was difficult to be identified with biochemical test was investigated by Comparing cellular fatty acid composition. First, a simple and rapid analytical method for the determination of cellular fatty acids of Legionella species by gas chromatography (GC) was developed. Cell cluster (about 50 mg) in 1 ml of 2 N sodium hydroxide-methanol solution was heated at 70°C with ultrasonication for 20 minutes. Then methyl esterification was carried out with 1 ml of 2 N hydrochloric acid-methanol solution. After extracting with 2 ml of hexane, the hexane layer was washed with water. The fatty acid composition was determined by GC and GC-MS on a Unisole-3000 column. This methyl esterification method was very useful in its simplicity, rapidity and reproducibility. Second, standard strains of Legionella species were investigated. All of 9 type strains of L. pneumophila (serogroup 1-9) contained plenty of i-C 16 : 0 and 5 type strains of L. bozemanii (serogroup 1, 2), L. dumoffii, L. gormanii and L. micdadei contained much of a-C 15 : 0. It was recognized that the composition ratio of fatty acid was not influenced by incubation period and medium. Next, radar charts of 4 axial coordinate for Legionella species were drawn with the peak area ratios of 4 branched fatty acids (i-C 14 : 0, i-C 16 : 0 as iso- and a-C 15 : 0, a-C 17 : 0 as antiiso-). Consequently this radar chart of L. pneumophila differed distinctly from others. These findings suggested that the proposed method in comparison with the composition patterns of 4 branched fatty acids was useful for the rapid and chemical identification of Legionella species.

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A method was described for quantitative analysis of glycyrrhizin in cosmetic lotions and creams. Glycyrrhizin was separated from the cosmetic base and other ingredients by bi-layer (upper ; celite, lower ; silica gel) column chromatography with methanol containing 0.5% acetic acid. The eluate was washed with n-hexane. The methanol layer was concentrated in vacuo and determined by high-performance liquid chromatography (HPLC) on Develosil ODS using a mobile phase of acetonitrile-1% acetic acid (35 : 65). Methyl salicylate was employed as an internal standard. Recoveries of glycyrrhizin obtained from model cosmetics were more than 96% and coefficients of variation were less than 2.2%. This method with clean-up procedure on bi-layer column chromatography was much suitable for the determination of glycyrrhizin in cosmetic lotions and creams.

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The simple method by cold-vapor atomic absorption spectrophotometry was studied for the samples co-existing organic substances by the rapid determination of mercury using alkaline tin (II) reduction. It is known that in the presence of tin (II) organomercury compounds such as methyl-, ethylmercury chloride and phenylmercury nitrate are reduced to inorganic mercury (II) in alkaline with a certain amount of copper (II) ion. But the reduction of organomercury compounds cannot proceed in the presence of potassium zinc cyanide as a masking agent for silver ion which is effective for the complicated environmental samples. However, the present paper shows that the addition of a large amount of copper (II) ion resolved this complicated problem. The reason for the remarkable effect of copper (II) ion was on the reduction of organomercuy compounds was therefore discussed. These aspects gave a simple method without time-consuming pre-treatment step in the samples which contained several organic substances. This method was applied for the determination of mercury in wastewater or biological samples with satisfactory results. The detection limit and precision of this method were 0.2 μg/l and 3%, respectively.

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Total hardness and concentrations of calcium and magnesium, and partly detection of nitrous ion and ammonium ion in tap water, well water, mineral water drinks, etc., in the summer of 1987 in Tokyo and the around areas, and the survey of taste for mineral water drinks were investigated. The average hardness in tap water and well water were about 69 ppm and 96 ppm (as the amount of CaCO₃), respectively, and the average concentrations of calcium and magnesium were about 19 ppm and 5 ppm, respectively, in tap water and about 22 ppm and 8 ppm, respectively, in well water. Tap water stored in a water tank of a building showed rather low hardness, compared with tap water unstored in the tank. Nitrous ion or ammonium ion was detected in 9 out of 13 the stored tap water samples and more than halves of well water and natural water samples. It indicates that tap water in the water tank and ground water were contaminated. The order of good taste for mineral water sample (total hardness 27-650 ppm) was almost the same as that of lowness of water hardness.

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