Development of a precolumn derivatization method for the determination of free amines in wastewater by high-performance liquid chromatography via fluorescent detection with 9-(2-hydroxyethyl)acridone

A simple, sensitive, and mild method for the determination of amino compounds based on a condensation reaction with fluorescence detection has been developed. 9-(2-Hydroxyethyl)acridone reacts with coupling agent N,N-carbonyldiimidazole at ambient temperature to form activated amide intermediate 9-(2-acridone)oxyethylcarbonylimidazole (AOCD). The amide intermediate (AOCD) preferably reacts with amino compounds under mild reactions in the presence of 4-(dimethylamino)pyridine (base catalyst) in acetonitrile to give the corresponding sensitively fluorescent derivatives with an excitation maximum lambda(ex) 404 mn and an emission maximum at lambda(em) 440 nm. The labeled derivatives exhibit high stability under reversed-phase conditions. The fluorescence intensities of derivatives in various solvents or at different temperatures were investigated. The method, in conjunction with a gradient elution, offers a baseline resolution of the common amine derivatives on a reversed-phase C-18 column. The LC separation for the derivatized amines shows good reproducibility with acetonitrile-water including 2.5% DMF as mobile phase. The relative standard deviations (n = 6) for each amine derivative are <4.5%. The detection limits (at a signal-to-noise ratio of 3) per injection were 0.16-12.8 ng/mL. Further research for the field of application, based on the AOCD amide intermediate as derivatization reagent, for the determination of free amines in real water samples is achieved.

Analysis of aromatic amines by high-performance liquid chromatography with pre-column derivatization by 2-(9-carbazole)-ethyl-chloroformate

2-(9-Carbazole)-ethyl-chloroformate (CEOC), a novel pre-column fluorescence derivatization reagent, has been developed for the analysis of aromatic amines. Taking five monocyclic aromatic amines (o-toluidine, aniline, 3,4-dimethylaniline, N-ethyl-p-toluidine, and p-phenylenediamine) as testing compounds, derivatization conditions such as pH of borate buffer, reaction time and fluorescent tagging reagent concentration have been investigated. By a one-step procedure, CEOC reacts readily with the aromatic amines to form stable derivatives with excitation and emission wavelengths, respectively, at 293 and 360 nm. This derivatization reaction could be finished within 20 min even at room temperature. The peak shapes of the derivatized aromatic amines can be improved greatly without any addition of competition amines into the mobile phase. Furthermore, this method can offer excellent quantitative precision with high tolerance of the matrix of samples. (C) 2003 Elsevier B.V. All rights reserved.

Determination of peptides and amino acids from wool and beer with sensitive fluorescent reagent 2-(9-carbazole)-ethyl chloroformate by reverse phase high-performance liquid chromotography and liquid chromotography mass spectrometry

A new method for the sensitive determination of amino acids and peptides using the tagging reagent 2-(9-carbazole)-ethyl chloroformate (CEOC) with fluorescence (FL) detection has been developed. Identification of derivatives was carried out by liquid chromotography mass spectrometry. The chromophore in the 2-(9-fluorenyl)-ethyl chloroformate (FMOC) reagent was replaced by carbazole, which resulted in a sensitive fluorescence lerivatizing agent CEOC. CEOC can easily and quickly label peptides and amino acids. Derivatives are stable enough to be efficiently analyzed by high-performance liquid chromatography. Studies on derivatization demonstrate excellent derivative yields over the pH range 8.8-10.0. Maximal yields close to 100% are observed with three- to fourfold molar reagent excess. Derivatives exhibit strong fluorescence and allow direct injection of the reaction mixture with no significant disturbance from the major fluorescent reagent degradation by-products, such as 2(9-carbazole)-ethanol and bis-(2-(9-carbazole)-ethyl) carbonate. In addition, the detection responses for CEOC derivatives are compared to those obtained with FMOC. The ratios AC(CEOC)/AC(FMOC) = 1.00-1.82 for fluorescence (FL) response and AC'(CEOC)/AC'(FMOC) = 1.00-1.21 for ultraviolet (UV) response are observed (here, AC and AC' are, respectively, FL and UV F response). Separation of the derivatized peptides and amino acids has been optimized on a Hypersil BDS C18 column. Excellent linear responses are observed. This method was used successfully to analyze protein hydrolysates from wool and from direct-derivatized beer. (C) 2003 Elsevier Science (USA). All rights reserved.

秸秆覆盖量对农田土面蒸发的影响

为研究秸秆量与夏玉米农田保墒效果之间关系,【方法】结合小区试验和微型蒸发皿定量观测,研究了0、0.6、0.9、1.2 kg/m24种不同秸秆覆盖量对农田土面蒸发的影响规律。【结果】试验表明在无种植情况下,秸秆覆盖大于0.6 kg/m2时,能明显影响和保持0￣50 cm土层的土壤含水量。秸秆覆盖量大于0.9 kg/m2时,保墒效果不再明显增加。结合干旱小区玉米试验发现,秸秆覆盖量在0.6￣0.9kg/m2范围时,玉米增产效果明显。【结论】秸秆覆盖量为0.6￣0.9 kg/m2范围时,可获得较好的保水和增产效果。

蛭弧菌BDG-9质粒不稳定性研究

本文建立了研究难于单独连续培养的专性蛭弧菌质粒稳定性的方法体系。应用此方法体系发现并证明了在专性蛭弧菌BDG9中所含的质粒pSTⅠ存在着独特的质粒缺失现象,当蛭弧菌BDG9单独培养时,在通常决定质粒稳定性的复制功能和分配功能都正常的情况之下,随着细胞的传代,质粒pSTⅠ逐渐丢失,蛭弧菌的生长繁殖也逐渐停止,表明质粒pSTⅠ的存在对BDG9细胞单独生长有重要作用。

Red-light-emitting iridium complexes with hole-transporting 9-arylcarbazole moieties for electrophosphorescence efficiency/color purity trade-off optimizationE

The synthesis, structures, photophysics, electrochemistry and electrophosphorescent properties of new red phosphorescent cyclometalated iridium(III) isoquinoline complexes, bearing 9-arylcarbazolyl chromophores, are reported. The functional properties of these red phosphors correlate well with the results of density functional theory calculations

Red-Light-Emitting Iridium Complexes with Hole-Transporting 9-Arylcarbazole Moieties for Electrophosphorescence Efficiency/ Color Purity Trade-off Optimization

The synthesis, structures, photophysics, electrochemistry and electrophosphorescent properties of new red phosphorescent cyclometalated iridium(III) isoquinoline complexes, bearing 9-arylcarbazolyl chromophores, are reported. The functional properties of these red phosphors correlate well with the results of density functional theory calculations. The highest occupied molecular orbital levels of these complexes are raised by the integration of a carbazole unit to the iridium isoquinoline core so that the hole-transporting ability is improved in the resulting complexes relative to those with I-phenylisoquinoline ligands. All of the complexes are highly thermally stable and emit an intense red light at room temperature with relatively short lifetimes that are beneficial for highly efficient organic light-emitting diodes (OLEDs).

Hole-transporting polymers containing carbazol-3,9-diyl and 1,4-phenylene fragments in the main chain

New carbazole-based polymers, which contain various content of electro-active fragments in the main chain connected via alkylene spacers, have been synthesized by Ni(0)-catalyzed Yamamoto-type aryl-aryl coupling reactions. These compounds represent amorphous materials of high thermal stability with glass-transition temperatures of 139-151 degrees C and thermal decomposition starting at temperatures above 400 degrees C. UV-vis absorption and photoluminescence emission spectra of the materials confirmed that the conjugated segments in the macromolecules are rather short.

Mo的掺杂对Ce_(0.8)Gd_(0.2)O_(1.9)烧结温度及电性能的影响

掺杂的CeO2基固体电解质因其在中低温条件下(500￣700℃)具有高氧离子电导率而成为有希望的IT-SOFCs(intermediate temperature-solid oxide fuel

Facile synthesis of 9,10-diarylphenanthrenes and poly(9,10-diarylphenanthrene)s

One-pot reduction of 9,10-diaryl-9,10-dihydrophenanthrene-9,10-diols to 9,10-diarylphenanthrenes was achieved with Zn/H+ in acetic acid. Accordingly, various novel phenanthrenes and polyphenanthrenes with efficient blue emission were easily synthesized.