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41.
Two different spectrofluorimetric methods for the determination of piroxicam (PX) in serum are presented and discussed. One of them is based on the use of three-way fluorescence data and multivariate calibration performed with parallel factor analysis (PARAFAC) and self-weighted alternating trilinear decomposition (SWATLD). This methodology exploits the so-called second-order advantage of the three-way data, allowing to obtain the concentration of the studied analyte in the presence of any number of uncalibrated (serum) components. The method was developed following two different procedures: internal standard addition and external calibration with standard solutions, which were compared and discussed. The second approach investigated is based on the combination of solid-phase extraction (SPE) and room temperature fluorimetry. Both methods here presented yield satisfactory results. The concentration range in which PX could be determined in serum was 1–10 μg ml−1. The limits of quantification for the experimental solutions using the chemometric approach were 0.09 μg ml−1 for the standard addition mode and 0.12 μg ml−1 using external calibration (both for PARAFAC and SWATLD algorithms). In the solid-surface fluorimetric method, the calibration graph was linear up to 0.22 μg ml−1 and the limit of quantification was 0.02 μg ml−1. 相似文献
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Martí MP Pino J Boqué R Busto O Guasch J 《Analytical and bioanalytical chemistry》2005,382(2):440-443
The aromatic composition of sugar cane spirits and, in general, of alcoholic beverages, is mainly influenced by the ageing process in wood barrels. There are several factors that affect the quality of the final aged product, but the time of the storage in the barrel is perhaps the most important one. Ageing time must therefore be controlled in order to detect counterfeits; however, this parameter is very difficult to control and, at present, there is no analytical method available to determine it. We propose a quantitative method for determining the ageing time of sugar cane spirits in oak barrels by using an electronic nose based on coupling directly a headspace sampler to a mass spectrometer (HS-MS), and multivariate calibration. The method developed is simple and provides, in 5 min, the ageing time of spirits with an accuracy of about 1 month. 相似文献
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一种基于流动注射梯度技术识别异常峰及校正的方法 总被引:1,自引:0,他引:1
基于流动注射梯度信息提出了一种利用梯度比均值进行定量的校正方法。方法具有在线自动判别和修复异常峰并自行校正的功能,和通用的标准系列定量方法相比,两者测定精度相当。但本文提出的方法抗干扰能力明显优于后者,可适用于在线过程监测。 相似文献
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R. Centoducatte E. P. Muniz F. E. Jorge M. T. Barreto 《Journal of Molecular Structure》2004,680(1-3):143-147
The molecular improved generator coordinate Hartree–Fock (MIGCHF) method is used to generate accurate basis sets of primitive Gaussian-type functions for the H2O molecule. Sequences of increasing size atom centered basis sets are employed to explore the accuracy that can be achieved with this method. Using the O(24s14p8d5f2g1h);H(22s9p5d2f1g) basis set, the HF and second-order electron correlation energies of the H2O ground state at the experimental geometry are computed as −76.0674680 and −0.3491935 hartree, respectively. The HF energy is in error by 20 μhartree and the second-order correlation energy corresponds to 96.5% of an estimate of the limiting value. The relevance of the present calculations is to show the accuracy that can be achieved in studies of small polyatomic molecules with the MIGCHF method. 相似文献
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Patricia C DamianiMariano D Borraccetti Alejandro C Olivieri 《Analytica chimica acta》2002,471(1):87-96
A direct method for the simultaneous determination of naproxen and salicylate in human serum is reported, based on a combination of spectrofluorometric measurements with two multivariate calibration techniques: partial least-squares (PLS-1) and the novel net analyte preprocessing (NAP). The method is rapid, selective and sensitive, and is based on the measurement of the fluorescence spectra of NH3 alkalinized whole human sera at the excitation wavelength of 315 nm. It can be applied within the ranges of concentrations 50-200 ng ml−1 for naproxen and 100-300 ng ml−1 for salicylate. The employed chemometric techniques have been compared on the basis of the statistical indicators for calibration and validation. Reproducibility and interference studies in abnormal sera have also been carried out. 相似文献
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Delatour T 《Analytical and bioanalytical chemistry》2004,380(3):515-523
Liquid chromatography–tandem mass spectrometry (LC-MS/MS) is a versatile coupling system which combines both selectivity and sensitivity and certainty. Hence, it is generally considered as the most reliable technique to quantify chemical compounds in complex matrices. In the present paper, we evaluate the performance of LC-MS/MS methods for the quantification of 3-nitrotyrosine in human urine in order to point out its dependence on the design of the quantification method, and emphasize the role of matrix effects in the performance. We compare external and internal calibrations, isotope dilution and isotopomer-based exact matching. The role of both sample preparation and multiple transitions monitoring is particularly addressed. 相似文献