A sensitive high performance liquid chromatographic method for the determination of N-nitrosoamines with pre-column fluorescence derivatization has been developed. N-nitrosoamines are first changed into secondary amines using denitrosation reagent, then react with acridone-N-acetyl chloride (ARC-Cl) to produce corresponding secondary amine derivatives, which exhibit a strong fluorescence. Maximum emission for ARC derivatives is 430 nm (lambda(ex) 404 nm). The labelled derivatives are very stable, less than 4% decomposition occurs after heating at 40 degrees C for 24 h. Fluorescence intensities of derivatives are higher in neutral and alkaline than in acidic solutions. This method, in conjunction with a multi-gradient program, offers a baseline resolution of the ARC derivatives from a linear acetonitrile gradient. Separation is carried out on a reverse phase C(18) column. Derivatization and chromatographic conditions are optimized. The relative standard deviation (n=6) at an analytical concentration of 10 pmol of each N-nitroamine is less than 4.5%. The detection limits at the fmol level. The method described is also suitable for analysis of other amino compounds in different biological samples. 相似文献
In situ liquid secondary ion mass spectrometry (SIMS) enabled by system for analysis at the liquid vacuum interface (SALVI) has proven to be a promising new tool to provide molecular information at solid–liquid and liquid–vacuum interfaces. However, the initial data showed that useful signals in positive ion spectra are too weak to be meaningful in most cases. In addition, it is difficult to obtain strong negative molecular ion signals when m/z>200. These two drawbacks have been the biggest obstacle towards practical use of this new analytical approach. In this study, we report that strong and reliable positive and negative molecular signals are achievable after optimizing the SIMS experimental conditions. Four model systems, including a 1,8-diazabicycloundec-7-ene (DBU)-base switchable ionic liquid, a live Shewanella oneidensis biofilm, a hydrated mammalian epithelia cell, and an electrolyte popularly used in Li ion batteries were studied. A signal enhancement of about two orders of magnitude was obtained in comparison with non-optimized conditions. Therefore, molecular ion signal intensity has become very acceptable for use of in situ liquid SIMS to study solid–liquid and liquid–vacuum interfaces.
Summary Analytical methods have been developed for the determination of organic pollutants of intermediate polarity in sewage. Water
samples are first passed through a solid phase adsorption cartridge. The analytes are then extracted from the absorbent with
supercritical CO2 into a small volume of trapping solvent. Finally, the extracts are analyzed directly by capillary gas chromatography and
gas chromatography-mass spectrometer. The various parameters (pressure, temperature, type and concentration of modifiers,
trapping solvent, flow rate and volume of supercritical fluid and equilibrium time) influencing the efficiency of extraction
were studied. Extraction efficiencies for the test compounds are >70%, and relative standard deviations are <4.6% (n=3). The
methods established were applied to the analysis of sewage at the Lanzhou Wastewater Treatment Plant, China. 66 organic pollutants
were detected, of which 15 compounds appeared in the list of priority pollutants suggested by the US EPA. 相似文献
A Fourier–Chebyshev pseudospectral method is used for the numerical simulation of incompressible flows in a three-dimensio nal channel of square cross-section with rotation. Realistic, non-periodic boundary conditions that impose no-slip conditions in two directions (spanwis e and vertical directions) are used. The Navier–Stokes equations are integrated in time using a fractional step method. The Poisson equations for pressure and the Helmholtz equation for velocity are solved using a matrix diagonalization (eigenfunction decomposition) method, through which we are able to reduce a three-dimensional matrix problem to a simple algebraic vector equation. This results in signficant savings in computer storage requirement, particularly for large-scale computations. Verification of the numerical algorithm and code is carried out by comparing with a limiting case of an exact steady state solution for a one-dimensional channel flow and also with a two-dimensional rotating channel case. Two-cell and four-cell two-dimensional flow patterns are observed in the numerical experiment. It is found that the four-cell flow pattern is stable to symmetri cal disturbances but unstable to asymmetrical disturbances. 相似文献
