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.

Trends in heavy metal levels in the dissolved and particulate phase in the Dutch rhine-meuse (MAAS) delta*

Levels of the heavy metals Cd, Cr, Cu, Pb and Zn, in both the dissolved and particulate phase, were determined in two sampling campaigns in August 1978 and August 1984 in the Dutch Rhine-Meuse (Maas) Delta. Besides the heavy metal concentrations, other important parameters were determined, such as the concentrations of seston, chlorophyll and nutrients. The concentrations of dissolved Cd and of Cd, Pb and Cu in particulate matter were much higher in 1978 than in 1984, especially for Cd. This may be due to the strict regulations implemented in Germany to reduce the pollution of natural waters by heavy metals. The correlation between the high Cd content and the chlorophyll content is explained by the binding of Cd to living and dead organisms. The distribution of the metals between the dissolved and the particulate phase, indicated by the distribution quotient Kd , increases from low values of Kd for Cu and Zn, to higher values for Cd and Cr, and the highest values for Pb. The differences are explained by various binding forms of each of these metals in natural waters

the ebb-tidal delta of the venice lagoon,Italy

Very high-resolution seismic lines were collected offshore the Venice Lagoon in the framework of the Co.Ri.La'New very high resolution seismic methods to study the Venice Lagoon subsoil' project. The 140 km boomer profiles led to the identification of a convex-upward,lens-shaped body just outside the Lido inlet,one of the three lagoon inlets,which has been interpreted as an ebb-tidal delta.The comparison between the scismostratigraphic setting og this deposit, as revealed by the seismic lines,and the analyses of historicalbathymetric maps highlighted the key role of human interventions in the formation and evolution of the Lido inlet cbb-tidal delta.To preserve the lagoon environment but also to ensure a navigable way, human interventions at the Lidoinlet,performed since the fourteenth centtury, caused profound variations in the inlet dynamics,ldading to a progressive increase in the sediment dispersion from the lagoon interior towards the sea. The ebb-tidal delta of the Lido nilet is thus a very recent feature compared with the formation of the Venice lagoon and formed mainly as a consequence of the construction of the two jetties that have bound the inlet form AD 1886 to the present day.

农田防护林主带间距离的确定——基于林带结构与风速降低的关系(英文)

本文通过对9条分布均匀、相对较窄的不同疏透度(透光疏透度,下同)(0.13～0.33)的树木林带和不同疏透度(0.00～0.80)风障组合的野外风速观测,确定了树木林带和风障的最适疏透度分别为0.25和0.13。基于林带结构(疏透度)与风速降低的关系,确定了林带主带间距离的主要参数,即,林带结构系数(δ)和以主害风为代表的小气候参数(Lrp)。另外,通过对林带树木的野外调查,应用树木解析技术确定林带成林高(H0)。因此,树木林带的主带间距可以通过林带结构系数、希望降低风速的比例和树木生长模型来确定。本文以杨树林带为例,具体确定了杨树林带的主带间距。该研究结果不仅适于树木林带的设计,同时适于其它生物材料或人工风障的设计。图4表5参40。

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。

Landscape change detection of the newly created wetland in Yellow River Delta

Four models are employed in the landscape change detection of the newly created wetland. The models include ones for patch connectivity. ecological diversity, human impact intensity and mean center of land cover. The landscape data of the newly created wetland in Yellow River Delta in 1984, 1991, and 1996 are produced from the unsupervised classification and the supervised classification on the basis of integrating Landsat TM images of the newly created wetland in the four seasons of the each year. The result from operating the models into the data shows that the newly created wetland landscape in Yellow River Delta had a great chance. The driving focus of the change are mainly from natural evolution of the newly created wetland and rapid population growth, especially non-peasant population growth in Yellow River Delta because a considerable amount of oil and gas fields have been found in the Yellow River Delta. For preventing the newly created wetland from more destruction and conserving benign Succession of the ecosystems in the newly created wetland, six measures are suggested on the basis of research results. (C) 2003 Elsevier Science B.V. All rights reserved.

Application of rough set-based analysis to extract spatial relationship indicator rules: An example of land use in Pearl River Delta

Spatial relations, reflecting the complex association between geographical phenomena and environments, are very important in the solution of geographical issues. Different spatial relations can be expressed by indicators which are useful for the analysis of geographical issues. Urbanization, an important geographical issue, is considered in this paper. The spatial relationship indicators concerning urbanization are expressed with a decision table. Thereafter, the spatial relationship indicator rules are extracted based on the application of rough set theory. The extraction process of spatial relationship indicator rules is illustrated with data from the urban and rural areas of Shenzhen and Hong Kong, located in the Pearl River Delta. Land use vector data of 1995 and 2000 are used. The extracted spatial relationship indicator rules of 1995 are used to identify the urban and rural areas in Zhongshan, Zhuhai and Macao. The identification accuracy is approximately 96.3%. Similar procedures are used to extract the spatial relationship indicator rules of 2000 for the urban and rural areas in Zhongshan, Zhuhai and Macao. An identification accuracy of about 83.6% is obtained.