The chemical composition of the essential oil obtained from the aerial parts ofFemlastenocarpa Boiss., a native plant of Iran, was examined by using GC and GC/MS. Twenty-six compounds constituting 97.8% of the total components detected were identified. a-Pinene (48.8%) and P-pinene (30.1%) were found to be the major components in the oil.
Dispersive liquid-liquid microextraction (DLLME) and spectrofluorimetry, coupled with chemometrics methods, are proposed in this work for the pre-concentration and determination of ofloxacin concentration in spiked human urine. Chloroform and acetonitrile were selected as the extraction and dispersive solvents by the one-variable-at-a-time process. The Box-Behnken design was used to optimize the other variables, including the volume of extraction and dispersion solvents, solution pH, and ionic strength. A linear calibration curve was obtained in the 5.0-120.0 ng mL -1 range under optimal conditions with a detection limit of 1.61 ng mL -1 and correlation coefficient of 0.9948. A relative standard deviation (RSD) of 1.13% was obtained for seven consecutive replicates. Parallel factor analysis (PARAFAC) and partial least square (PLS) modeling were applied for the multivariate calibration of the spectrofluorimetric data. To pre-process the data matrices and predict the model results, the orthogonal signal correction (OSC) was used, and the analysis results were statistically compared. The methods accuracy values for ofloxacin determination, evaluated by the root mean square errors of prediction (RMSEP) and relative standard error of prediction (RSEP), were 0.82 and 1.12 using OSC-PLS, and 0.31 and 0.42 using OSC-PARAFAC models, respectively. Ofloxacin can be reliably determined in human urine samples through the proposed procedure, according to the results.
A new chelating resin was prepared by coupling Amberlite XAD-4 with phenol through an azo spacer, then modified by allyl bromide and characterized (by elemental analysis and IR) and studied for preconcentration of Cu(II) using flame atomic absorption spectrometry (FAAS) for metal monitoring. The optimum pH value for sorption of the above mentioned metal ion was 4.5. The resin was subjected to chemical evaluation through batch binding and column chromatography of Cu(II). The chelating resin can be reused for 15 cycles of sorption-desorption without any significant change in sorption capacity. A recovery of 98% was obtained for the metal ion with 0.5 M HNO 3 as eluting agent. The equilibrium adsorption data of Cu(II) on modified resin were analyzed by Langmuir, Freundlich and Temkin models. Based on equilibrium adsorption data the Langmuir, Freundlich and Temkin constants were determined to be 0.061, 0.193 and 0.045 at pH 4.5 and 25 o C. The method was applied for the copper determination from industrial waste water sample.
This study shows that genetic algorithm (GA) is a suitable method for selecting wavelengths for partial least squares (PLS) calibration of mixtures with almost identical spectra without loss of prediction capacity employing spectrofluorimetric method. A training set of mixtures containing different concentrations of ofloxacin (OFL) and riboflavin (B2) were prepared to be used as calibration set to check the prediction ability of GA-PLS models due to spectral overlapping of these constituents. Each model was validated using a validation set and then real samples were analyzed. Linear calibration curves were obtained in the 0.5-5.0 and 2.0-10.0 µg mL-1 range for ofloxacin and riboflavin, respectively. To preprocess the data matrices, the orthogonal signal correction (OSC) was used and the analysis results were statistically compared. The methods accuracy for simultaneous determination of ofloxacin and riboflavin, were evaluated by the root mean square errors of prediction (RMSEP) which were 0.0868 and 0.158 for ofloxacin and riboflavin, respectively, and relative standard error of prediction (RSEP) which were 2.738 and 2.846 for ofloxacin and riboflavin, respectively using OSC-GA-PLS models. This procedure allows the simultaneous determination of OFL and B2 in human urine and serum samples with good reliability of the determination.
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