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摘要
An ultrafast liquid chromatography method with fluorescence detection has been optimized for the determination of 15 polycyclic aromatic hydrocarbons (PAHs) using a recent Kinetex-C18 column (250 mm x 4.6 mm). This column has been recently packed with a new brand of porous shell particles with an average particle size of 5 mu m to separate various compounds by liquid chromatography, operating at very low pressure. After optimization of the analytical procedure, the separation of the 15 PAHs in spiked tap water samples was achieved without coeluted products in 21.5 min at 16 degrees C using an aqueous/acetonitrile mobile phase under gradient concentrations with a very low flow rate (0.7-1.0 mL min(-1)) and low pressure values (870-1590 psi = 60-110 bar), all of these conditions being interesting from an economic point of view. The synchronization of wavelength time changing and the elution time of each compound was performed to avoid baseline deviation. The validation of the whole of the experimental procedure was conducted taking into consideration the following parameters: calibration curve, linearity, limits of detection and quantification, accuracy, sensitivity, precision, and repeatability of the retention time for each PAH. The proposed analytical procedure presented adequate linearity over a concentration range from 0.025 to 10 mu g L-1 with a correlation coefficient better than 0.9980. The repeatability (relative standard deviation in percentage, n = 5) of the retention time for the different PAHs investigated ranged from 0.03% to 0.34% and the limit of detection was under 0.6 mu g L-1 for most PAHs (excepted for indeno[1,2,3-c,d]pyrene, limit of detection = 1.71 mu g L-1). The intraday and interday precisions were below 4%. The recovery of PAH in spiked tap water samples was variable, ranging from 96% to 109%, with relative standard deviation between 0.2% and 4.8%, depending on PAHs and their concentration levels.
- 出版日期2015-5
