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Method Sensitivity (method + sensitivity)
Selected AbstractsAnalysis of 51 persistent organic pollutants in soil by means of ultrasonic solvent extraction and stir bar sorptive extraction GC-MSJOURNAL OF SEPARATION SCIENCE, JSS, Issue 20 2008Marta Martínez-Parreńo Abstract A novel method based on ultrasonic solvent extraction and stir bar sorptive extraction (SBSE) for the analysis of 51 persistent organic pollutants including organochlorine pesticides (OCPs), polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), and polybrominated diphenylethers (PBDEs) in soil samples was developed. The different parameters that affect both the extraction of analytes from the soil samples, such as solvent selection, solvent volume, mass of soil, and extraction time, and the partitioning from the solvent/water mixture to the PDMS were studied. The final selected conditions consisted of the extraction of 1 g of soil with 15 mL methanol by sonication for 30 min. The methanol extract was mixed with 85 mL of Milli-Q water and extracted by means of SBSE for 14 h at 900 rpm. The stir bars were analyzed by thermal desorption-GC-mass spectometry (TD-GC-MS). The effects of the matrix on the recovery of the various pollutants under the developed method were studied using two soils with very different physicochemical properties. Method sensitivity, linearity, repeatability, and reproducibility were also studied. Validation and accuracy of the method were conducted by analyzing two commercial certified reference materials (CRMs). The main advantage of this method resides in the fact that a small amount of a nontoxic solvent (methanol) is needed for the extraction of only 1 g of solid sample allowing LODs ranging from 0.01 to 2.0 ,g/kg. Repeatability and reproducibility variations were lower than 20% for all investigated compounds. Results of the CRMs verify the high accuracy of this method. [source] Separation of peptides by open-tubular capillary electrochromatography using Fe(III)-deuteroporphyrin as a covalently attached stationary phaseELECTROPHORESIS, Issue 13 2009Ángel Yone Abstract The separation of seven biologically active peptides was attempted by open-tubular capillary electrochromatography in fused-silica capillaries chemically modified with iron (III)-deuteroporphyrin using UV-absorption detection at 214,nm. The effect of BGE pH and content of organic solvent modifier was investigated. The best separations were obtained in 25,mM phosphate (BGE), pH 4.0, containing 5%,v/v ACN and 10,mM hydroquinone, which was added to prevent gas bubble formation. Considering the method sensitivity, lower concentration LODs were obtained for all peptides in their open-tubular capillary electrochromatography separation as compared with their CZE separation in bare fused-silica capillary. The iron (III)-deuteroporphyrin column proved to be highly stable over time and showed acceptable precision of migration times and corrected peak areas (RSD in the range 2,4%). [source] Near-field mapping of surface refractive-index distributionsLASER PHYSICS LETTERS, Issue 9 2005I.P. Radko Abstract Scanning near-field optical microscopy (SNOM) in reflection is employed for high-resolution mapping of surface refractive-index distributions. Two different single-mode optical fibers with step-index profiles are characterized using a reflection SNOM setup, in which cross-polarized detection is employed to increase the contrast in optical images and, thereby, the method sensitivity. The SNOM images exhibit a clear ring-shaped structure associated with the fiber step-index profile, indicating that surface refractive-index variations being smaller than 10,2 can be detected. It is found that the quantitative interpretation of SNOM images requires accurate characterization of a fiber tip used, because the detected optical signal is a result of interference between the optical fields reflected by the sample surface and by the fiber tip itself. The possibilities and limitations of this experimental technique are discussed. (© 2005 by Astro, Ltd. Published exclusively by WILEY-VCH Verlag GmbH & Co. KGaA) [source] Development of a simultaneous liquid,liquid extraction and chiral derivatization method for stereospecific GC-MS analysis of amphetamine-type stimulants in human urine using fractional factorial designBIOMEDICAL CHROMATOGRAPHY, Issue 9 2008W. R. Wan Aasim Abstract A stereospecific gas chromatography,mass spectrometry analysis method for amphetamine-type stimulants in human urine was recently developed. For maximum efficiency, liquid,liquid extraction and chiral derivatization of the analytes using (R)-(,)- , -methoxy- , -(trifluoromethyl)phenylacetyl chloride were performed simultaneously. The effects of (1) use of saturated sodium chloride in 2.0 m sodium hydroxide, (2) extraction solvent volume, (3) percentage of triethylamine, (4) derivatization reagent volume, (5) sample mixing time, (6) incubation temperature and (7) incubation time on method sensitivity and variability were assessed using a two-level, eight-run Plackett,Burman design followed by a fold-over design. The use of saturated sodium chloride solution and the derivatization reagent volume were significant factors (ANOVA, p < 0.01). The saturated sodium chloride solution decreased sensitivity whereas an increased volume of derivatization reagent increased sensitivity. Calibration curves for all analytes were linear between 5 and 500 µg/L, with correlation coefficients of >0.99. Detection limits were ,2.3 µg/L and quantitation limits ,7.7 µg/L. Reproducibility was good, with relative standard deviation values at <20%. Recovery exceeded 100% for most analytes. The experimental design enabled easy and rapid identification of significant factors using a minimal number of samples. This method has good potential for studies requiring rapid and sensitive stereospecific quantification of amphetamine-type stimulants. Copyright © 2008 John Wiley & Sons, Ltd. [source] Utility-Based Optimization of Combination Therapy Using Ordinal Toxicity and Efficacy in Phase I/II TrialsBIOMETRICS, Issue 2 2010Nadine Houede Summary An outcome-adaptive Bayesian design is proposed for choosing the optimal dose pair of a chemotherapeutic agent and a biological agent used in combination in a phase I/II clinical trial. Patient outcome is characterized as a vector of two ordinal variables accounting for toxicity and treatment efficacy. A generalization of the Aranda-Ordaz model (1981,,Biometrika,68, 357,363) is used for the marginal outcome probabilities as functions of a dose pair, and a Gaussian copula is assumed to obtain joint distributions. Numerical utilities of all elementary patient outcomes, allowing the possibility that efficacy is inevaluable due to severe toxicity, are obtained using an elicitation method aimed to establish consensus among the physicians planning the trial. For each successive patient cohort, a dose pair is chosen to maximize the posterior mean utility. The method is illustrated by a trial in bladder cancer, including simulation studies of the method's sensitivity to prior parameters, the numerical utilities, correlation between the outcomes, sample size, cohort size, and starting dose pair. [source] | ||||||||||