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.

Synthesis and characteristics of composite chiral stationary phases based on cellulose derivatives

Composite chiral stationary phases (CSPs) were prepared on the basis of cellulose derivatives coated or bonded onto silica. "Molecular exterior" type CSPs were prepared by mixing together two different cellulose tris-derivatives before or after being coated or bonded onto silica, and the "molecular interior" type was obtained by synthesizing non-regioselectively heterosubstituted cellulose derivatives coated or bonded onto silica. For the sake of comparison, the individual phases were also prepared with corresponding cellulose derivatives by coating or bonding approaches, respectively. All of the prepared CSPs were characterized and their chiral recognition properties were evaluated by HPLC with several test racemates. The experimental results demonstrated that the "molecular exterior" CSPs generally exhibit chiral recognition capacities intermediate between those of the two individual phases. However, in the separation of some racemates higher enantioselectivity may be achieved on the "molecular interior" phases than on individual phases, thus broadening the application range of a single cellulose-based CSP.

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.

浅析旱作农业技术在黄土高原退耕还林(草)之后的作用——为朱总理’99,8,7讲话而作

针对朱基总理 1 999年 8月 7日讲话精神和旱农技术在特殊的自然条件和社会条件下为了良化农田生态环境和持续增产所采取的一整套用地与养地相结合的技术体系。文章着重的分析了培肥地力、轮作倒茬、化学技术、选育品种、节水、立体种植、地膜覆盖、水土保持耕作法八种技术 ,充分利用光、热、水、气、土、肥资源而取得明显的社会效益、经济效益和生态效益 ,剖析了旱作技术在农业持续、稳定、健康发展中的作用和改善农业生态环境的显著地位 ,供同类地区的决策者和研究者借鉴

微波消解-ICP-AES法同时测定蛹虫草中8种微量元素

选用硝酸和过氧化氢作为消解剂,采用微波技术消解蛹虫草样品,用电感耦合等离子体发射光谱(ICP-AES)法同时测定其中K、P、Ca、Mg、Cu、Fe、Zn、Mn共8种微量元素的含量。进行微波消解条件的优化选择及分析线性、精密度和回收率等实验,建立同时测定蛹虫草中多种微量元素的微波消解-ICP-AES方法。本方法所测元素的标准曲线均有良好的线性关系,以猪肉粉国家标准物质GBW08522为对照进行验证,其回收率为91%～106%,相对标准偏差(RSD)<3.0%;该法加标回收率为90%～108%,RSD<3.0%,具有较好的准确度和精密度,是一种快速、准确而高效的分析方法。测定结果表明,蛹虫草富含有K、P、Mg、Ca、Zn元素。

中国东北8种藓类植物染色体数目

本文对中国东北 8种藓类植物染色体数目进行了报道。其中赤茎藓Pleuroziumschreberi (Brid .)Mitt.,n =5 ;塔藓Hylocomiumsplendens (Hedw .)B .S .G .,n =11;粗肋羽藓Thuidiumrecognitum (Hedw .)Lindb .,n =11;绿羽藓T .assimile (Mitt.)Jaeg .,n =11;四齿藓TetraphispellucidaHedw .,n =8;侧枝匐灯藓Plagiomniummaximoviczii (Lindb .)Kop .,n =6 ;尖叶匐灯藓P .cuspidatum (Hedw .)Kop .,n =12 ;具缘提灯藓Mniummarginatum (With .)Beauv .,n =6。绿羽藓的染色体数目为首次报道 ,赤茎藓 ,塔藓 ,粗肋羽藓和四齿藓为国内首次报道

Two novel triphenylamine-substituted poly(p-phenylenevinylene) derivatives: synthesis, photo- and electroluminescent properties

Two novel triphenylamine-substituted poly(p-phenylenevinylene) derivatives, P1 and P2, have been successfully synthesized through the Witting-Horner reaction. The structures and properties of the monomers and the resulting polymers were characterized by using H-1 NMR, FT-IR, GPC, TGA, UV-vis absorption spectroscopy, cyclic voltammetry (CV) and electroluminescence (EL) spectroscopy

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