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1.
A large-volume (100 microl) injection-ETAAS with W-treated PG furnace combined with a phosphate modifier was applied to the determination of unpolluted levels of Cd in tap, snow and river-water samples. The limit of detection of 1.1 ng l(-1) was observed for a 4 w/v% NH4H2PO4 modifer. Matrix interference studies were tested for major ion species well found in fresh water. The direct determination of Cd in certified river water (12 +/- 2 ng l(-1)) was carried out and the observed value was in agreement with the certified one. The good recoveries of Cd added to real environmental water samples were also observed. This method was applied to the determination of Cd in unpolluted environmental water samples. 相似文献
2.
Yoshiyuki Watabe Takuya Kondo Hiroe Imai Masatoshi Morita Nobuo Tanaka Jun Haginaka Ken Hosoya 《Analytical sciences》2004,20(1):133-137
A new high-performance liquid chromatography (HPLC) method has been developed to detect ultra-low concentrations of bisphenol-A (BPA) (below 1 ng/L (ppt)) using column switching electrochemical detection (ECD). The results were superior to those obtained from manual pretreatment procedure with membrane stationary phase. BPA is inherently ubiquitous in the environment, including tools and solvents used for its analysis; to obtain meaningful results, therefore, the concentration of the overall BPA contamination must be below the detection limit for BPA using the analytical system. Therefore, purified water for preparing the standard BPA solution must be filtered with a hydrophobic membrane to suppress BPA background levels of contamination. In addition, we investigated methods for effectively preserving environmental water containing BPA. The addition of a small amount of ethylenediaminetetraacetic acid (EDTA) provided good recovery even after overnight storage. By employing these precautionary measures and procedures to reduce BPA contamination from the analytical procedure, we could accurately determine l(-10) ppt of BPA in environmental water samples using a column switching HPLC system. 相似文献
3.
Kazuhiko Nakano Toshihiro Nakamura Izumi Nakai Akira Kawase Makoto Imai Mikio Hasegawa Yohichi Ishibashi Isamu Inamoto Kazuhuyu Sudou Masaru Kozaki Akira Tsuruta Akihiro Ono Kazutoshi Kakita Mamoru Sakata 《Analytical sciences》2006,22(9):1265-1268
The Japan Society for Analytical Chemistry has developed some new plastic certified reference materials (CRMs) for the analysis of mercury in polyester disks using XRF analysis. These CRMs (named as JSAC 0621-0625) were prepared by casting polyesters including a toluene solution of organometallic compounds as a standard. Concentrations of the five levels of mercury ranged from 0 to 250 mg/kg. Homogeneity tests of prepared disks had shown excellent results. Interlaboratory comparison study for the certification was performed by 15 laboratory participants. The z-scores in robust statistical method was applied for the evaluation of outliers. The certified values were assigned after discarding outliers. The uncertainties of certified values were determined as the confidence levels of 95%. 相似文献
4.
A fluorimetric determination method for N-arachidonoylethanolamine (anandamide) was developed using a precolumn fluorescence derivatization followed by coupled-column high-performance liquid chromatography (HPLC). Anandamide extracted from the rat brain tissue was derivatized with 4-N-chloroformylmethyl-N-methylamino-7-N, N-dimethylaminosulfonyl-2,1,3-benzoxadiazole (DBD-COCl), purified by a solid-phase extraction (Emporetrade mark), and assayed by the coupled-column HPLC. The HPLC consisted of phenyl (100 x 4.6 mm i.d. ) and octadecylsilica columns (250 x 4.6 mm i.d.), both connected by a six-port valve. The concentration of anandamide in rat brain was 3. 37 +/- 0.73 pmol/g with 6.47 and 3.57% of intra- and inter-day precisions, respectively. Using this method, we investigated the alteration of anandamide concentration in rat brain 30 min after administration of anandamide (2 mg/kg, i.p.) to rats pretreated with or without phenylmethylsulfonyl fluoride (PMSF; 30 mg/kg, i.p.), an inhibitor of amidohydrolase. In rats pretreated with PMSF, the brain concentration of anandamide was approx. 16-fold higher than that of rats without PMSF (p < 0.01). 相似文献
5.
Treatment of l(14S)-β-canadine methochloride (1b) and d(14R)-β-canadine methochloride (1c) with organometals gave d- (2b) and l-2,3-methylenedioxy-9,10-dimethoxyochotensanes (2c), respectively. The structures of these derivatives were proved by chemical and spectral means. The CD spectra of 2b showed Davydov split extrema centered at 284 nm with a positive first Cotton effect, while 2c showed the antipodal curve of 2b. Consequently, the absolute configurations of 2b and 2c were concluded the 14R and 14S, respectively.Application of the anionic rearrangement to N-methyltharictricavine chloride (15) led to 2,3 - methylenedioxy - 9,10 - dimethoxy - 13 - methylochotensane (18) together with the Hofmann methines 16 and 17. The stereochemistry of 18 was confirmed in terms of the nuclear Overhauser effects. 相似文献
6.
M. Yoshida M. Asano M. Kumakura R. Katakai T. Mashimo H. Yuasa K. Imai H. Yamanaka 《Colloid and polymer science》1990,268(8):726-730
A sequential polydepsipeptide containing a tripeptide sequence L-alanyl-Lalanyl-ethyl L-glutamyl and an-hydroxy acid L-lactic acid, poly(Ala-Ala-Glu(OEt)-Lac), was synthesized to prepare the microspherical particles by the solvent evaporation process. In this case, the solvents play the most important role for the preparation of polydepsipeptide microspheres and, as an example, when 200 mg of the polydepsipeptide dissolved in 10 ml of 98/2% chloroform/dichloroacetic acid mixture was stirred at 400 rpm and 30 C, the microspherical particles with mean diameter of 58m were formed after pouring into 200 ml of 1% (w/v) poly(vinyl alcohol) solution. 17-Estradiol was incorporated into the particles, and the resulting particles were found to contain 5 mg of drug per 25 mg of the particle. The in vivo release of drug from the microspherical formulation was evaluated by measuring the pharmacological influence on rat prostate. It was found that the sufficient amount of drug, keeping the effective pharmacological influence, is supplied during the first 12-week period, followed by an incomplete supplying of drug intil the implant is perfectly degraded in vivo in the 25th week from the start of implantation. 相似文献
7.
Tsuyoshi Miura Satoshi Tsujino Kohtaro Goto Midori Noguchi Manabu Node Nobuyuki Imai 《Tetrahedron》2005,61(27):6518-6526
The use of the bisfluorous chain-type propanoyl (Bfp) group as a fluorous protective group made it possible to rapidly synthesize the Gb2 and Gb3 oligosaccharide derivatives by a simple fluorous-organic extraction purification. Furthermore, the fluorescence-labeled Gb2 and Gb3 oligosaccharides were prepared as a potential Vero Toxins detecting reagent. 相似文献
8.
9.
Yoshitane Imai Kakuhiro Kawaguchi Tomohiro Sato Michiya Fujiki Yoshio Matsubara 《Tetrahedron letters》2007,48(16):2927-2930
By using (1R,2R)-1,2-diphenylethylenediamine as a chiral molecule and 2-anthracenecarboxylic acid as a fluorescent molecule, we created a chiral supramolecular organic fluorophore having circularly polarized luminescence properties in the solid-state. 相似文献
10.
Yoshio Imai N. N. Maldar Masa-Aki Kakimoto 《Journal of polymer science. Part A, Polymer chemistry》1984,22(9):2189-2196
2,5-Bis(4-aminophenyl)-3,4-diphenylthiophene, a polyimide-forming monomer, was prepared in three steps starting from benzyl chloride and sulfur. Novel polyimides were synthesized from the diamine and pyromellitic dianhydride or 3,3′, 4,4′-benzophenonetetracarboxylic dianhydride (BTDA). Polymerization was carried out either by the usual two-step procedure that included ring-opening polyaddition giving polyamic acids, followed by cyclodehydration to polyimides, or by the direct one-pot procedure involving cyclodehydration in situ. The polyimide derived from the diamine and BTDA, especially that prepared by the one-pot procedure in m-cresol containing isoquinoline, is soluble in various organic solvents and gave a yellow, transparent, tough, and flexible film. Solubility of this polyimide varied by the preparative method and by the copolymerization with bis(4-aminophenyl) ether. All the polyimides are highly thermally stable and exhibited no appreciable decomposition up to 450°C in air and nitrogen atmospheres. 相似文献