Comparison of high-performance liquid chromatography with electrochemical detection and gas chromatography-mass fragmentography for the assay of salsolinol, dopamine and dopamine metabolites in food and beverage samples

High-performance liquid chromatography with electrochemical detection (HPLC-ED) and combined gas chromatography--mass spectrometry in the single-ion monitoring mode (GC--MS-SIM) have been used for the determination of salsolinol, dopamine, 3,4-dihydroxyphenylacetic acid, 3,4-dihydroxyphenylethanol and norepinephrine in a selection of food and beverage samples. The unique specificity of the SIM mode allows a simple one-step extraction to be used even for complex sample matrices. We have been able to demonstrate the quantitative and qualitative advantages offered by GC--MS over HPLC--ED by direct comparison of the chromatographic data obtained. We demonstrate that the specificity of SIM and the benefits offered by the incorporation of deuterated internal standards make GC--MS-SIM the method of choice for valid identification and precise quantitation of salsolinol, dopamine and dopamine metabolites in a complex sample matrix.     

On-line dual-wavelenth instrumentation for antomatic correction of light scattering interference in dispersive atomic fluorescence spectrometry

The design basis of a dual detection channel spectrometer for general application in atomic fluorescence analysis is discussed. Low frequency modulation of the radiation from a single light source is employed with one channel set at a fluorescence wavelength while the second channel measures the magnitude of scattering at a non-fluorescent wavelength. The instrument has been applied to the analysis of trace Au and Cd in high scattering matrix solutions. The statistical treatment of data, and the method of calculating detection limits, is discussed.     

The effect of HNO(3), HCl and HBr on the fluorescence of the aluminium complex of 1-(2-pyridylazo)-2-naphthol and an improved fluorometric procedure for determination of aluminium

The fluorescence of the aluminium complex of 1-(2-pyridylazo)-2-naphthol (PAN) is both stabilized and enhanced by 10(-3)M HNO(3) . HCl or HBr. Other acids tested have no effect. An improved flourometric procedure with a detection limit of 0.001 ppm, increased precision and reduced interferences over the existing Al-PAN method is described. It is satisfactory for the determination of aluminium in bronze when an ion-exchange separation is used, but is not suitable for the determination of aluminium in plants. The acidified Al-PAN is unsuitable for the determination of nickel(II) and fluoride by fluorescence quenching.     

Tm~(3+)掺杂Ge-Ga-Se玻璃中红外发光特性与多声子弛豫分析

用熔融急冷法制备了系列不同Tm3+掺杂浓度的Ge30Ga5Se65玻璃样品,测试了样品折射率、拉曼光谱、吸收光谱以及800nm激光泵浦下的近红外及中红外波段荧光光谱和荧光寿命。用Judd-Ofelt理论计算了Tm3+在Ge30Ga5Se65玻璃中的强度参数Ωi(i=2,4,6)、自发辐射跃迁概率A、荧光分支比β和辐射寿命τrad等光谱参数。讨论了800nm激光泵浦下掺杂1Wt%Tm3+样品在近红外1.23,1.48和1.8μm处的发光特性及各量子效率,研究了800nm激光泵浦下的样品中红外荧光特性与掺杂浓度之间的关系,计算了常温下该基质玻璃中Tm3+:3H5→3F4跃迁对于3.8μm处的多声子弛豫速率Wmp和Ge30Ga5Se65玻璃基质中多声子弛豫常数W(0)和电子-声子结合常数α值。结果表明Ge30Ga5Se65硒基玻璃较低的声子能量可以大大降低稀土离子能级间跃迁的多声子弛豫概率,从而提高中红外荧光发光效率,因此硒基玻璃作为稀土离子的掺杂基质材料对实现中红外荧光输出是非常有利的。     

On Problems in the Calculus of Variations in Increasingly Elongated Domains

This paper deals with minimization problems in the calculus of variations set in a sequence of domains, the size of which tends to infinity in certain directions and such that the data only depend on the coordinates in the directions that remain constant. The authors study the asymptotic behavior of minimizers in various situations and show that they converge in an appropriate sense toward minimizers of a related energy functional in the constant directions.     

CONSERVATION OF ENDANGERED ENDEMIC SEABIRDS WITHIN A MULTI‐PREDATOR CONTEXT: THE BARAU'S PETREL IN RÉUNION ISLAND

Abstract Seabirds breeding on islands are vulnerable to introduced predators, such as rats and cats, and the removal of such predators is generally viewed as a priority for seabird conservation and restoration. However, multiple invasive mammal species interacting may generate unexpected outcomes following the removal (eradication) of one species. Generally these indirect interactions are not well understood or demonstrated. We propose and study a prey (seabird)‐mesopredator (rat)‐superpredator (cat) model, taking into account the juvenile stages in the prey population, in order to direct conservation management for seabird conservation. We give a more biologically realistic differential system than those studied before (Courchamp et al. [1999] ; Fan et al. [2005] ), in particular for long‐lived seabird species. We present a theoretical study and show existence and uniqueness of a positive solution as well as a qualitative study of the equilibria that may appear. Because standard numerical methods, usually implemented in scientific softwares, can fail to give the right biological approximations ( Anguelov et al. [2009] ), we propose a reliable algorithm that preserves most of the qualitative properties of the continuous system, using the theory of nonstandard finite difference methods. Finally, we use biologically realistic parameters available for the representative Barau's petrel (Pinet et al. [2008] ), an endemic species from Réunion island, to present numerical simulations that support the theoretical study. Cats play the major role in seabird prey population dynamics. Seasonality in seabird breeding delays but does not prevent extinction. In all scenarios, cat control (or preferably eradication) is imperative to prevent extinction of vulnerable long‐lived seabirds, like the Barau's petrel.     

EESI-MS监测ZrOCl2·8H2O催化的Paal-Knorr反应

用电喷雾萃取电离质谱（EESI-MS）离线监测甲醇中,ZrOCl₂·8H₂O催化的苯胺和2,5-己二酮的Paal-Knorr反应,检测到中间体m/z 204和m/z 208,产物m/z 172和产物二聚体m/z 343的准分子离子信号,并对其进行了结构分析。     

International inter-comparison exercise on $${}^{153}\hbox {Sm}$$

Samarium-153 (\({}^{153}\hbox {Sm}\)) is a short-lived radionuclide that decays to stable europium-153 via beta emission, with subsequent de-excitation via gamma emission and internal conversion. Historical measurements of \({}^{153}\hbox {Sm}\) by gamma spectrometry and beta liquid scintillation counting have shown a low bias compared to beta proportional counting. In order to investigate this, four national laboratories jointly conducted an experimental inter-comparison exercise on a certified \({}^{153}\hbox {Sm}\) sample, created from neutron activation of samarium-152. Radiometric measurements were conducted using gamma spectrometry, liquid scintillation counting, gas proportional counting, and passivated implanted planar silicon detectors and compared across the four institutions against the certified value. The results from this experiment are presented together with a number of conclusions which suggest that the current published cumulative fission yield for \({}^{153}\hbox {Sm}\), as used by many laboratories, is approximately 15% high and is the likely cause of the previously observed bias.     

Library of biphenyl privileged substructures using a safety-catch linker approach

A biphenyl privileged structure library containing three attachment points were synthesized using a catechol-based safety-catch linker strategy. The method requires the attachment of a bromo-acid to the linker, followed by a Pd-catalyzed Suzuki cross-coupling reaction. Further derivatization, activation of the linker with strong acid and aminolysis afforded the respective products in high purity and good overall yield. To show the versatility of the synthesis, a 199-member library was generated. The library samples both conformational and chemical diversity about a well-known privileged substructure.