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11.
V. J. Barwick S. L. R. Ellison M. J. Q. Rafferty R. S. Gill 《Accreditation and quality assurance》2000,5(3):104-113
A protocol has been developed illustrating the link between validation experiments and measurement uncertainty evaluation.
The application of the protocol is illustrated with reference to a method for the determination of three markers (CI solvent
red 24, quinizarin and CI solvent yellow 124) in fuel oil samples. The method requires the extraction of the markers from
the sample matrix by solid phase extraction followed by quantification by high performance liquid chromatography (HPLC) with
diode array detection. The uncertainties for the determination of the markers were evaluated using data from precision and
trueness studies using representative sample matrices spiked at a range of concentrations, and from ruggedness studies of
the extraction and HPLC stages.
Received: 10 April 1999 · Accepted: 24 September 1999 相似文献
12.
Juan José Berzas Nevado Juana Rodríguez Flores Francisco Javier Guzmán Bernardo 《Analytica chimica acta》2006,559(1):9-14
A simple, rapid and sensitive procedure using solid phase extraction and capillary zone electrophoresis for the determination of propranolol (a beta-blocker) and one of its metabolites, N-desisopropylpropranolol, has been developed and validated. The optimum separation of both analytes was obtained in a 37 cm × 75 μm fused silica capillary using 20 mmol/L phosphate buffer (pH 2.2) as electrolyte, at 25 kV and 30 °C, and hydrodynamic injection for 5 s. Prior to the electrophoretic separation, the samples were cleaned up and concentrated using a C18 cartridge and then, eluted with methanol, allowing a concentration factor of 30.Good results were obtained in terms of precision, accuracy and linearity. The limits of detection were 28 and 30 μg/L for N-desisopropylpropranolol and propranolol, respectively. Additionally, a robustness test of the method was carried out using the Plackett-Burman fractional factorial model with a matrix of 15 experiments.The presented method has been applied to the determination of both compounds in human urine. 相似文献
13.
Rodríguez-Flores J Berzas Nevado JJ Contento Salcedo AM Cabello Díaz MP 《Journal of chromatography. A》2005,1068(1):175-182
The viability of nonaqueous capillary electrophoresis (NACE) was investigated for determination of gleevec and its main metabolite in human urine using a fused-silica capillary. Baseline separation of the studied solutes was obtained using a nonaqueous solution composed of 12 mM ammonium acetate and 87.6 mM acetic acid in methanol-acetonitrile (ACN) (80:20, v:v) providing analysis time shorter than 3 min. Different aspects including stability of the solutions, linearity, accuracy and precision were studied in order to validate the method in the urine matrix. Detection limits of 24 microg L(-1) for gleevec and its metabolite were obtained. A robustness test of the method was carried out using the Plackett-Burman fractional factorial model with a matrix of 15 experiments. The developed method is simple, rapid and sensitive and has been used to determine gleveec and its metabolite at clinically relevant levels in human urine. Before NACE determination, a solid-phase extraction (SPE) procedure with a C18 cartridge was necessary. Real determination of these analytes in two patient urines were done. 相似文献