An improved derivatization method for sensitive determination of fatty acids by high-performance liquid chromatography using 9-(2-hydroxylethyl)-carbazole as derivatization reagent with fluorescence detection

Summary Tagging techniques with reagents used for fluorescent detection for short and long-chain fatty acids using high-performance liquid chromatography are evaluated in terms of the tagging reactions, handing, flexibility, stability of the reagents. Emphasis is given to the applications of the tagging techniques to relatively high molecular mass fatty acids. The fatty acids or carboxylic compounds were derivatized to their corresponding esters with 9-(2-hydroxy ethyl)-carbazole (HEC) in acetonitrile at 60°C with N, N′-carbonyldiimidazole (CDI) as a coupling agent in the presence of 4-dimethylaminopyridine (DMAP). A mixture of esters of C₁−C₂₀ fatty acids was completely separated with 45 min using gradient elution on a reversed-phase C₁₈ column. The maximum fluorescence emission for the derivatized fatty acids is at 365 nm (λ_ex 293 nm). Studies on derivatization conditions indicated that fatty acids react rapidly and smoothly with HEC in the presence of CDI and DMAP in acetonitrile to give the corresponding sensitively fluorescent derivatives. The application of this method to the analysis of long chain fatty acids in plasma is also investigated. The LC separation shows good selectivity and reproducibility for fatty acids derivatives. The relative standard deviations (n=6) for each fatty acid derivative are <5.0%. The detection limits are at 38–57 fmol levels for C₁₄−C₂₀ fatty acids and lower levels for <C₁₄ fatty acids.     

新型双重电荷转移分子的二阶非线性光学性质的 理论研究

以INDO/SCI方法为基础,按完全态求和(SOS)公式编制了计算分子二阶非线性光学系数β~i~j~k和β~μ的程序。研究了1,2-二氨基-4,5-二硝基苯1和其异构体1,3-二氨基-4,6-二硝基苯2的电子光谱和二阶非线性光学性质。计算表明分子1具有与分子2几乎相等的二阶非线性极化率。但由于分子1的偶极矩明显大于分子2的,故分子1的μβ值比分子2的μβ值大的多。在此基础上,研究了2,3-二(β-苯乙烯基)-5,6-二氰基吡嗪和2,3-二(β-噻吩乙烯基)-5,6-二氰基吡嗪和2,3-二(β-噻吩乙烯基)-5,6二氰基吡嗪衍生物的电子光谱和二阶非线性光学性质。结果表明,这些化合物均具有两个相距很近的强吸收峰,它们对β值的呈加和模式。由于这类化合物特征吸收峰均位于413nm以下且具有大的μβ值,所以,它们是一类很有前途的二阶非线性光学候选材料。     

Comparison of modeling calculations with experimental results for direct current glow discharge optical emission spectrometry

A comparison is made between numerical modeling and experimental results for the electrical characteristics, the erosion rates and the optical emission intensities of various argon and copper lines in a direct current glow discharge, to verify the model calculations and to illustrate some features and limitations of the model. In order to reach good agreement with the current–voltage characteristics, the gas temperature, which was treated as an adjustable parameter, was assumed to increase slightly as a function of voltage and pressure. This assumption is in accordance with theoretical predictions and experimental observations in the literature. The erosion rates and optical emission intensities, calculated as a function of voltage and pressure, were also found to be in reasonable agreement with the experimental data. However, it appeared that still better agreement with the measured data could be reached when the gas temperature was assumed to be constant as a function of voltage. This illustrates that the effect of voltage cannot yet be completely correctly predicted for both the electrical current and the erosion rates and optical emission intensities at the same time, and that, therefore, the glow discharge behavior is not yet perfectly described in the model. This is not unexpected in view of the complexity of the model calculations and the uncertainties of some input data. However, in general, the agreement between model results and experimental data is satisfactory, so that it can be concluded that the model gives already a realistic picture of the direct current glow discharge.     

Quantum magneto-transport in two-dimensional GaAs electron gases and SiGe hole gases

We have measured the low-temperature transport properties of two-dimensional (2D) GaAs electron gases and 2D SiGe hole gases. Our experimental results fall into three categories. (i) Collapse of spin-splitting and an enhanced Landé g-factor at Landau level filling factors both ν=3 and ν=1 in a 2D GaAs electron gas are observed. Our experimental results show direct evidence that the effective disorder is stronger at ν=1 than that at ν=3 over approximately the same perpendicular magnetic field range. (ii) We present evidence for spin-polarisation of a dilute 2D GaAs electron gas. The Lande g-factor of the system is estimated to be 1.66. This enhanced g value is ascribed to electron–electron interactions at ultra low carrier density limit. (iii) In a high-quality SiGe hole gas, there is a temperature-independent point in the magnetoresistivity ρ_xx and ρ_xy which is ascribed to experimental evidence for a quantum phase transition between ν=3 and ν=5. We also present a study on the temperature(T)-driven flow lines in our system.     

The fabrication and photo-induced melting of networked gold nanostructures and twisted gold nanorods

Fabrications of both networked Au nanostructured particles and twisted gold nanorods (TGNRs) suspended in water were accomplished via a laser ablation technique. They can be further purified by simple filtration. We conducted the photo-induced melting studies on these two types of nanostructures under both 532 and 1064 nm laser irradiation wavelengths. Both structural changes and their absorption spectral responses are reported. The TGNR sample contains particles with a wide distribution of aspect ratios. Its typical absorption spectrum shows a flat and continuously rising feature to the red of ca. 520 nm, which show a similarity with that of the suspended Au networks. The photo-induced melting processes corresponding to these two types of Au nanostructures demonstrate quite different spectral responses associated with their structural variations. Various observations on the wavelength- and laser power-dependence are presented. Generally, this type of photoannealing results in a formation of spherical shaped particles. Among them, we demonstrate that a spectral ‘hole’ burning can be uniquely achieved in the case of TGNRs suspension after 1064 nm low-fluence laser beam irradiation. Its contribution based on a selective melting will be addressed.     

The Stability of Icosahedral Cluster and the Range of Interaction Potential

The relation between the stability of icosahedral clusters and the range of interaction potential is discussed.We found that the stability of icosahedral clusters nay decrease with decreasing range of interaction potential. A simple formula about the critical number of icosahedral clusters and the range of interaction potential (M1/3c = A1 A2r2eff)was proposed. The calculation of the stability of icosahedral fullerence molecular clusters shows that our idea is right.``     

Synthesis, characterization and magnetism of binuclear cobalt (II) complexes bridged by tetracarboxylato groups

Three new binudear cobalt (II) complexes with extended te-tracarboxylato- bridge have been synthesized and characterized, namely [Co2 (PMTA) (bpy)4] (1), [Co2(PMTA)-(phen)4] (2) and [Co2(PMTA) (NO2phen)4] (3), where PMTA represents the tetraanion of pyroniellitic acid, and bpy, phen, NO2-phen denote 2,2'-bipyridine, 1,10-phenan-throline; 5-nirto-1, 10-plienanthroline, respectively. Based on elemental analyses, molar conductivity measurements, IR and electronic spectra studies, it is proposed that these complexes have PMTA-bridged structures and consist of two cobalt (II) ions, each in a distorted octahedral environment. These complexes were further characterized by variable temperature magnetic susceptibility measurements (4-300 K) and the observed data were successfully simulated by the equation based on the spin Hamiltonian operator, giving the exchange integral J = - 1.02 cm-1 for 1, J = -1.21 cm-1 for 2 and J = - 1.18 cm-1 for 3, respectively. These results revealed the operation of antiferromagneti     

A new result on irreducible NFSRs with respect to cascade connection

Nonlinear feedback shift registers (NFSRs) are widely used in stream cipher design as building blocks. The cascade connection of NFSRs, known as an important architecture, has been adopted in Grain family of stream ciphers. In this paper, a new sufficient condition under which an NFSR cannot be decomposed into the cascade connection of two smaller NFSRs is presented, which is easy to be verified from the algebraic normal form (ANF) of the characteristic function. In fact, our results are also applicable to nonsingular Boolean functions, which actually improve a previous research of Rhodes [6] where the characteristic functions of NFSRs cannot be contained.