An enzymatic method for the kinetic measurement of L-asparaginase activity and L-asparagine with an ammonia gas-sensing electrode

A simple kinetic method to assay L-asparaginase and L-asparagine with an ammonia gas-sensing electrode is described. The method is based upon the de-amination of L-asparagine by L-asparaginase from Escherichia coli, resulting in the production of ammonia. The initial rate (mV/min) of ammonia release is proportional to the activity of L-asparaginase and also to the concentration of L-asparagine in the presence of a large amount of the enzyme. Optimal temperature, buffer composition and pH for the assays are specified. L-Asparaginase was determined in the range of 0.4-1.6 U in a 0.1 ml sample; the recovery was 98.1-103.8% for 16 determinations and sigma n was 1.59. L-Asparagine was determined in the concentration range of 1 x 10(-4)--1 x 10(-3) M with sigma n-1 1.92. The method was applied to the determination of 1-5 x 10(-4) M asparagine added to human serum with sigma n-1 1.96 for 5 determinations.     

Solubility of RE elements into Ba−Cu−O melts and the enthalpy of dissolution

The liquidus compositions of Y, Sm, Gd, Dy and Yb for a melt with a Ba to Cu ratio of 3 to 5 has been investigated by a) dipping thermally equilibrated (held in the furnace for at least 10 min) MgO single crystals into the melt and analyzing the melt stuck to the MgO by ICP; b) dipping a relatively cool not thermally equilibrated Al₂O₃ polycrystalline rod into the melt (i.e. effective quenching) and analyzing the melt stuck to the rod by ICP. The measurements have been made in the temperature range from approximately 950° C up to about 1300° C. Following thermodynamic calculations, expressions for the liquidus lines are derived and the enthalpy of dissolution for the various RE123 and RE211 are calculated to be nearly the same for the same melt composition. Nevertheless a small increase of the enthalpy of dissolution with increasing peritetic temperature could be detected.     

Polymerization of aromatic aldehydes. II. Cationic cyclopolymerization of phthalaldehyde

Phthalaldehyde was found to undergo cyclopolymerization with ease by several cationic catalysts and by γ-ray irradiation. The polymer was composed entirely of the dioxyphthalan unit, as confirmed by infrared spectroscopy and ready decomposition to monomer. The enhanced polymerizability of phthalaldehyde as compared with other aromatic aldehydes was explained in terms of the intermediate-type or, preferably, concerted propagation scheme. The conversion reached a saturation value of 87% in about 1 hr in methylene chloride at ?78°C, indicating an equilibrium polymerization. The ceiling temperature of the polymerization was ?43°C, as estimated from the relation between the saturation yield and polymerization temperature. The enthalpy and entropy of propagation were ?5.3 kcal/mole and ?23.0 eu, respectively. Since the molecular weight of the polymer was proportional to conversion, the propagating chain end was considered to be “living” in this system. The rate constant for propagation was calculated to be 0.18 1/mole-sec in methylene chloride at ?78°C with BF₃OEt₂ catalyst.     

Improved synthesis of paroxetine hydrochloride propan-2-ol solvate through one of metabolites in humans, and characterization of the solvate crystals

Paroxetine, a potent and selective inhibitor of 5-hydroxytryptamine (serotonin) uptake, was prepared through a piperidine derivative, which was reported to be one of the paroxetine metabolites in humans. Thus, the piperidine derivative was converted to its N-tert-butoxycarbonyl (N-Boc) derivative, which was then converted to N-Boc paroxetine. Paroxetine hydrochloride propan-2-ol (isopropyl alcohol (IPA)) solvate crystals were directly obtained from the N-Boc paroxetine by adding hydrogen chloride to the N-Boc paroxetine IPA solution. The amount of IPA content in the crystals was reduced by drying with a continuous change of powder X-ray diffraction patterns. Other characterizations of the solvate crystals were also conducted.     

One-pot synthesis of cyclic triamides with a triangular cavity from trans-stilbene and diphenylacetylene monomers

Base-promoted self-condensation reactions of trans-stilbene and diphenylacetylene monomers bearing 4-alkylamino and 4'-methoxycarbonyl groups were investigated. Reactions of N-propyl monomers under pseudohigh-dilution conditions (a THF solution of monomer was added dropwise to a THF solution of LiHMDS) afforded the corresponding cyclic triamides in good yields. X-ray crystallographic analysis showed that these cyclic triamides possessed an almost equilateral triangle structure with a cavity surrounded by tilted benzene rings.     

Extractability of radiocesium from processed green tea leaves with hot water: the first emergent tea leaves harvested after the TEPCO’s Fukushima Daiichi Nuclear Power Plant accident

In some tea tree planting areas within 300 km from the TEPCO’s Fukushima Daiichi Nuclear Power Plant (FNPP), it was found that newly emerged tea plant leaves for green tea contained two radiocesium species (cesium-134 and cesium-137). In this study, using processed green tea leaves for drinking, extraction ratios of radiocesium under several brew conditions were observed. When 90 °C water was used, 50–70% of radiocesium was extracted into the water, while 54–60% of radiocesium was extracted with 60 °C water. A part of radiocesium would be removed from leaves if the leaves were washed with 20 and 60 °C water before brewing, and the efficiencies were 11 and 32%, respectively. Newly emerged camellia leaves were used to simulate the radiocesium removal ratio from raw tea leaves by washing and boiling; radioactivity concentration was decreased to 60% of the original concentration with washing and 10 min boiling. From these results, it was found that almost half of the radiocesium would not be removed from raw or processed tea leaves. The values obtained in the present study could be used for internal radiation dose estimation from tea leaves.