Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection

A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d₅ was used as an internal standard. The linear ranges were 0.01-5.0 μg mL⁻¹ for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 μg mL⁻¹ for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation ≧0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 μg mL⁻¹ of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio ≧ 3) in urine was 5 ng mL⁻¹ for MA and MDMA and 10 ng mL⁻¹ for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.     

Catalytic activity of carbon-supported iridium oxide for oxygen reduction reaction as a Pt-free catalyst in polymer electrolyte fuel cell

Iridium oxide supported on Vulcan XC-72 carbon black (IrO₂/C) as a cathode catalyst for polymer electrolyte fuel cell (PEFC) has been characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD) measurement. The IrO₂ particles were 8-160 nm in diameter. The oxygen electroreduction activity was studied by cyclic voltammetry (CV). It was found that IrO₂/C had high oxygen reduction reaction (ORR) activity. The performance of the membrane electrode assemble (MEA) was also tested in a single PEFC and showed that IrO₂/C catalyst would be potential candidates for use as cathode catalyst in PEFC.     

Ramanujan type congruences for the Klingen-Eisenstein series

In the case of Siegel modular forms of degree \(n\) , we prove that, for almost all prime ideals \(\mathfrak {p}\) in any ring of algebraic integers, mod \(\mathfrak {p}^m\) cusp forms are congruent to true cusp forms of the same weight. As an application we give congruences for the Klingen-Eisenstein series and cusp forms, which can be regarded as a generalization of Ramanujan’s congruence. We will conclude by giving numerical examples.     

Quadrangulations on 3-Colored Point Sets with Steiner Points and Their Winding Numbers

Let P be a point set on the plane, and consider whether P is quadrangulatable, that is, whether there exists a 2-connected plane graph G with each edge a straight segment such that V(G) = P, that the outer cycle of G coincides with the convex hull Conv(P) of P, and that each finite face of G is quadrilateral. It is easy to see that it is possible if and only if an even number of points of P lie on Conv(P). Hence we give a k-coloring to P, and consider the same problem, avoiding edges joining two vertices of P with the same color. In this case, we always assume that the number of points of P lying on Conv(P) is even and that any two consecutive points on Conv(P) have distinct colors. However, for every k ≥ 2, there is a k-colored non-quadrangulatable point set P. So we introduce Steiner points, which can be put in any position of the interior of Conv(P) and each of which may be colored by any of the k colors. When k = 2, Alvarez et al. proved that if a point set P on the plane consists of \({\frac{n}{2}}\) red and \({\frac{n}{2}}\) blue points in general position, then adding Steiner points Q with \({|Q| \leq \lfloor \frac{n-2}{6} \rfloor + \lfloor \frac{n}{4} \rfloor +1}\) , P ∪ Q is quadrangulatable, but there exists a non-quadrangulatable 3-colored point set for which no matter how many Steiner points are added. In this paper, we define the winding number for a 3-colored point set P, and prove that a 3-colored point set P in general position with a finite set Q of Steiner points added is quadrangulatable if and only if the winding number of P is zero. When P ∪ Q is quadrangulatable, we prove \({|Q| \leq \frac{7n+34m-48}{18}}\) , where |P| = n and the number of points of P in Conv(P) is 2m.     

A generalization of the Erdős–Ko–Rado theorem to t-designs in certain semilattices

The Erd?s–Ko–Rado theorem is extended to designs in semilattices with certain conditions. As an application, we show the intersection theorems for the Hamming schemes, the Johnson schemes, bilinear forms schemes, Grassmann schemes, signed sets, partial permutations and restricted signed sets.     

“Click polyester”: Synthesis of polyesters containing triazole units in the main chain via safe and rapid “click” chemistry and their properties

Click Cu(I)‐catalyzed polymerizations of diynes that contained ester linkages and diazides were performed to produce polyesters (click polyesters) of large molecular weights [(～1.0–7.0 ) × 10⁴], that contained main‐chain 1,4‐disubstitued triazoles in excellent yields. Incorporation of triazole improved the thermal properties and magnified the even‐odd effect of the methylene chain length. We also found that, by changing the positions of the triazole rings, the thermal properties of the polyesters could be controlled. The use of in situ azidation was a safe reaction, as explosive diazides are not used. In addition, the microwave heating was found to accelerate the polymerization rates. This is the first study that has applied click chemistry for the synthesis of a series of polyesters. © 2010 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 48: 4207–4218, 2010     

Theoretical study on quantum dynamics of bose system interacting with photon field

We investigate the quantum dynamics of two‐boson and two‐level systems interacting with a one‐mode photon field. The time evolution of the population for each state is calculated in terms of the Jaynes–Cummings model. We find the collapses and revivals of the order parameter for the Bose–Einstein condensation. © 2001 John Wiley & Sons, Inc. Int J Quantum Chem 84: 401–408, 2001     

Surface pre-melting and surface flattening of Bi nanofilms on Si(1 1 1)-7 × 7

We report on the in situ observation of temperature-driven drastic morphology evolution and surface pre-melting of the Bi(0 0 1) nanofilm deposited on the Si(1 1 1)-7 × 7 surface by use of spot-profile-analyzing low-energy electron diffraction (SPA-LEED). Surface step density of the single-crystalline, epitaxial Bi(0 0 1) film decreases above 350 K in a critical manner. On annealed Bi(0 0 1) films, we have detected surface pre-melting with a transition temperature of 350 K, which yields reversible diffraction intensity drop in addition to the harmonic Debye-Waller behavior. The observed surface flattening of the as-deposited film is driven by the increased amount of mobile adatoms created through the surface pre-melting.     

Energetic properties of nio surface examined by heat-of-adsorption measurement

Heat of adsorption and isotherm of water vapor on NiO samples were measured simultaneously at 301 K to examine the energetic properties of the surface. They revealed that NiO has a relatively uniform surface. The heat of adsorption ranging 80–90 kJ·mol^–1 indicates the production of surface hydroxyl groups on the (100) plane of NiO. It is relatively small compared with that of other metal oxides, which suggests a weak nature of the Ni²⁺ ion sites for chemisorption of water. It is suspected that half of the surface Ni²⁺ ions are covered with hydroxyl groups and the remainings act as relatively strong physisorption sites for water molecules.The authors are grateful for the help of Prof. S. Kittaka of Okayama University of Science in taking electron micrographs. This work was partly supported by Grant-in-Aid for Scientific Research No. 02640348 from the Ministry of Education, Science and Culture of Japanese Government.