Accelerated glycosylation under frozen conditions

O-Glycosylations using thiomethyl glycosides as donors were compared under both frozen and unfrozen conditions. In the presence of MeOTf as a promoter, enormous rate acceleration was observed when the glycosylation was conducted in p-xylene below its freezing point.     

Determination of metal-binding proteins in soft tissues of rock oyster by neutron activation analysis and particle induced X-ray emission

In this work, we determined the levels of trace metals in protein fractions isolated from rock oysters by neutron activation analysis (NAA) and particle induced X-ray emission (PIXE). Proteins were extracted from mantles and hepatopancreases of rock oysters and fractionated by size-exclusion high performance liquid chromatography (HPLC). The protein fractions from mantles and hepatopancreases are found to be abundant in Fe, Cu, Zn, Mn, Pb, and Ag. HPLC profiles of Fe, Cu, Zn, and Ag indicate that those elements are bound to proteins extracted from mantles and hepatopancreases.     

Preparation and certification of the new reference materials; plastics (disk form, JSAC 0621-0625) for determination of mercury using x-ray fluorescent analysis.

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%.     

Comparisons of elemental concentrations in hair of the inhabitants of heavy metal polluted areas with those of normal Japanese

Human hair collected from the mercury, arsenic and cadmium polluted areas has been analysed by instrumental neutron activation method. The concentrations of 27 elements were compared with those of normal Japanese. Correlation coefficients of logarithmic concentrations between the elements were calculated and their significance levels were determined. Factor contribution and factor loadings of the elements were calculated for each factor by making use of principal component analysis. The factor score of each sample was also calculated for each factor to examine the effects of the contamination by heavy metals on individuals.     

Asymmetric interaction of optically active polymers with asymmetric small molecules. IV. Effect of hydrophobic groups on asymmetric interaction

In order to investigate the mechanism of the asymmetric interaction between optically active polymers and small molecules, optically active copolymers of N-acrylyl L-amino acids(N-acrylyl-L -phenylalanine, N-acrylyl-L -tryptophan, and N-acrylyl-L -leucine, respectively) and N,N′-hexamethylene diacrylylamide were synthesized, and interaction of these polymers with the optical isomers of phenylalanine and tryptophan was investigated. In the interaction of these acidic polymers with amino acids performed at pH 5.0, significant difference in amount of adsorption between the D and L isomers of amino acids were observed, and the L form of amino acids was adsorbed preferentially. The interaction between optically active small molecules was also investigated: these results showed a similarity to the results for interaction between optically active polymers and amino acids. In some instances of asymmetric interaction the influence of hydrophobic interaction between a polymer and substrate was clearly perceived. The stereoselective effects on the asymmetric interaction are discussed.     

Determination of sultopride and tiapride in serum by gas chromatography using a surface ionisation detector

A sensitive and selective method has been developed for the determination of sultopride and tiapride in serum using gas chromatography with a surface ionisation detector. No interfering peaks from endogenous substances were observed. The method showed good reproducibility and accuracy, and the standard curve was linear up to 2 micrograms/ml with a correlation coefficient of 0.999. This method is applicable to pharmacokinetic studies and therapeutic drug monitoring of sultopride and tiapride.     

Synthesis and analgesic activity of novel heterocycles, [1]benzothiopyrano[3,4-b]pyrrole derivatives

In order to develop analgesic compounds possessing a sulfur atom in the alicyclic ring, novel cis-fused heterocycles, [1]benzothiopyrano[3,4-b]pyrrole derivatives (II) were synthesized via a unique cyclization reaction starting from 4-(4-methoxyphenylthio)-2-butanone (1) or 6-methoxy-3,4-dihydro-2H-1-benzothiopyran-4-one (7). The analgesic effects of benzothiopyranopyrroles (16, 18) were measured by means of the writhing test. The phenolic derivative 18 completely inhibited the appearance of writhing at the dose of 50 mg/kg, but the methoxy derivative 16 had no analgesic effect.     

Clinical usefulness of a trypsin radioimmunoassay kit

From the clinical use of RIA-gnost trypsin kit, the following results were obtained. 1. Standard curve showed a steep and good curve was shown. 2. Incubation: The condition for the first incubation was set at the room temperature for 10-24 hours and that for the second incubation at the room temperature for 3-5 hours. With these settings, satisfactory results were obtained. 3. Reproducibility and recovery: The C.V. of the reproducibility and the recovery were considered superior, and the values were below 10% and +/- 3%, respectively. 4. Correlation between trypsin and serum elestase-1: An excellent positive correlation (coefficient of correlation r = 0.889) was shown. 5. Serum trypsin concentration of normal and pancreatic diseases: The normal range was from 100 to 500 ng/ml. Acute pancreatitis rose obviously. Diabetes mellitus and chronic pancreatitis was below 500 ng/ml and the pancreatic cancer showed a tendency to scatter in the range of 50-1,250 ng/ml. The above results indicated that serum trypsin can be easily measured with high precision by using this method. Thus the method is considered useful for the diagnosis of pancreatic diseases.