Development of a novel potentiometric titration method for determination of polypropylene degradation

In this study, a novel potentiometric titration of hydroperoxide in degraded polypropylene (PP) is proposed. This titration is quite sensitive compared with the conventional ones such as UV and manual titrations, and its detection limit was about 2 meq/kg. The sensitivity was equal to that of molecular weight measurement by GPC for the degraded PP and, in addition, the volatilization behavior of the hydroperoxide could be detected. This titration was found to be very effective for the determination of PP degradation.     

Development of a regenerable cell culture system that senses and releases dead cells

We developed a rapidly regenerable cell culture system in which the cell culture substrate detects cell death and selectively releases the dead cells. This culture material was achieved by combining a detector that responds to the signal from the dead cells and an actuator to release the dead cells. Benzo-18-crown-6-acrylamide (BCAm) with a pendant crown ether receptor was used as the sensor to recognize cellular signals and N-isopropylacrylamide (NIPAM) was used as the actuator. This copolymer of NIPAM and BCAm can respond to potassium ions and change its nature from hydrophobic to hydrophilic at the culture temperature of 37 degrees C. Living cells concentrate potassium ion internally; when cells die, potassium ions are released. The polymer surface recognizes the potassium ions released from the dead cells, the NIPAM hydrates, and the dead cells are selectively detached. This in vitro culture system is a novel one in which artificial culture materials work cooperatively with cellular metabolism by responding to this signal from the cells, thereby realizing in vitro tissue regeneration partly mimicking the mechanisms of in vivo homeostasis.     

Photochemistry of 3-aryl-2-isoxazoline1

3-Phenyl-2-isoxazoline (1) was irradiated to give 4-phenyl-2-oxazoline (3), β-aminoaldehyde (14) and benzonitrile from its π-π^* singlet excited state. Several related derivatives afforded similar photoproducts on irradiation. The quantum yields of the photoreactions were dependent on the magnitudes of the singlet energies of the 2-isoxazolines. p-Cyanophenyl-2-isoxazoline (1c) formed a one-to-one photoadduct (22) with benzene.     

Stopped-flow spectrophotometric determination of nM level of Pb(II) using 5,10,15,20-terakis(1-methylpyridinium-4-yl)porphine

A spectrophotometric determination method for nM levels of Pb(II) has been developed using a stopped-flow spectrophotometer with cationic water-soluble porphyrin. The stopped-flow spectrophotometer allows the monitoring of the incorporation reaction of the Pb(II) ion into 5,10,15,20-terakis(1-methylpyridinium-4-yl)porphine (TMPYP) within a narrow time window (2.5 s) at pH 10.5–12.0 before the Pb-TMPYP complex is replaced with other foreign metal ions, since usually the Pb-TMPYP complex is very labile and readily replaced with other metal ions. This improved the selectivity of Pb(II) determination as compared to the conventional spectrophotometric determination of Pb(II) using water-soluble porphyrins.     

Generation of alkoxycarbenium ion pools from thioacetals and applications to glycosylation chemistry

[reaction: see text] Alkoxycarbenium ions have been generated and accumulated as "cation pools" by the low-temperature electrochemical oxidation of alpha-phenylthioethers. Although an unsuccessful attempt to accumulate glycosyl cations was made, a one-pot method for electrochemical glycosylation, which involves anodic oxidation of thioglycosides to generate glycosyl cation equivalents followed by their reactions with glycosyl acceptors, has been developed.     

Improvement of chemical analysis of antibiotics. IX. A simple method for residual tetracyclines analysis in honey using a tandem cartridge clean-up system

A simple, rapid and precise analytical method for the residual tetracyclines in honey has been established using a tandem cartridge clean-up system (prepacked reversed-phase and ion-exchange cartridges) followed by high-performance liquid chromatography. The recoveries of oxytetracycline (OTC), tetracycline (TC), chlortetracycline (CTC) and doxycycline (DC) from honey spiked at a level of 1.0 ppm are 87.1, 85.3, 98.0 and 99.0%, respectively, with coefficients of variation of 1.1-3.9%. The detection limits in honey are 0.02 ppm for OTC and TC, and 0.05 ppm for CTC and DC, respectively. The time required for the analysis of four samples is only 1 h.     

Synthesis of the common left-half part of pectenotoxins

The common left-half [C31-C33(OC1-C7)-C40] part of pectenotoxins has been synthesized convergently from the C31-C35, C36-C40, and C1-C7 parts. The C31-C35 part, prepared via a new route shorter than our previous route, was coupled with the C36-C40 part through reductive lithiation and addition reactions to give an adduct stereoselectively, which was converted to a cyclic acetal corresponding to the C31-C40 part. The left-half was synthesized by a three-step process including esterification of the C31-C40 part with the C1-C7 part.     

Diinsertion of fluorenylidene into a sulfur-sulfur bond of diaryl disulfides

Upon irradiation (>340 nm) of a benzene solution of diazofluorene with di-p-tolyl- or di-p-anisyl disulfide, the corresponding 9,9′-bis(arylmercapto)bifluorenyl was afforded in moderate to good yield accompanied by formation of 9,9′-bis(arylmercapto)fluorene. The major reaction pathway is considered to be a disulfur ylide formation followed by two times of successive Stevens rearrangement or by concerted electron redistribution via [2,3]sigmatropic rearrangement.     

Determination of plasma protein binding of propafenone in rats, dogs and humans by highly sensitive gas chromatography-mass spectrometry

A highly sensitive method for the determination of propafenone in plasma has been established using gas chromatography-mass spectrometry with the deuterium-labelled compound as an internal standard. Plasma levels as low as 1 ng/ml were measured using 0.5-ml plasma samples. Plasma protein binding of the drug in rats, dogs and humans in vitro and in vivo was determined by the proposed method. About 90% of the drug was bound to the plasma protein in all species in vitro (20-500 ng/ml) and 69-88% in rats, 90-95% in dogs and 77-89% in humans after oral administration of the drug at doses of 50 mg/kg, 5 mg/kg and 200 mg per person, respectively.     

Evaluation of prognosis in patients with old myocardial infarction--using 201Tl myocardial scintigraphy and 99mTc cardiac scintigraphy

To evaluate the prognosis in 57 patients with old myocardial infarctions, 201Tl myocardial scintigraphy and 99mTc-HSA gated blood pool scan had been done as a 5-year follow up study. We subdivided into two groups; group I (over 60 years) and group II (under 60 years). Cardiac index (CI) and right ventricular ejection fraction (RVEF) did not change significantly, however left ventricular ejection fraction (LVEF) changed significantly (p less than 0.05). Correlationship between CAG score and delta LVEF by handgrip exercise test was y = -1.34 x +3.61 (n = 44, r = -0.400, p less than 0.01). Otherwise, Tl defect ratio between first and final examination did not show the significant change in two groups. In conclusion, nuclear examination (cardiac function and myocardial blood flow) is significant to evaluate the prognosis in patients with myocardial infarction.