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Recovery Data (recovery + data)
Selected AbstractsSupported liquid membranes in hollow fiber liquid-phase microextraction (LPME) , Practical considerations in the three-phase modeJOURNAL OF SEPARATION SCIENCE, JSS, Issue 9 2007Kari Folde Bårdstu Abstract In this work, three-phase liquid-phase microextraction (LPME) based on a supported liquid membrane (SLM) sustained in the wall of a hollow fiber was investigated with special focus on optimization of the experimental procedures in terms of recovery and repeatability. Recovery data for doxepin, amitriptyline, clomipramine, and mianserin were in the range of 67.8,79.8%. Within-day repeatability data for the four basic drugs were in the range of 4.1,7.7%. No single factor was found to be responsible for these variations, and the variability was caused by several factors related to the LPME extractions as well as to the final HPLC determination. Although the volume of the SLM varied within 0.4,3.1% RSD depending on the preparation procedure, and the volume of the acceptor solution varied within 4.8% RSD, both recoveries and repeatability were found to be relative insensitive to these variations. Thus, the handling of microliters of liquid in LPME was not a very critical factor, and the preparation of the SLM was accomplished in several different ways with comparable performance. Reuse of hollow fibers was found to suffer from matrix effects due to built-up of analytes in the SLM, whereas washing of the hollow fibers in acetone was beneficial in terms of recovery, especially for the extraction of the most hydrophobic substances. Several of the organic solvents used in the literature as SLM suffered from poor long-term stability, but silicone oil AR 20 (polyphenyl-methylsiloxane), 2-nitrophenyl octyl ether (NPOE), and dodecyl acetate (DDA) all extracted with unaltered performance even after 60 days of storage at room temperature. [source] CEC-ESI ion trap MS of multiple drugs of abuseELECTROPHORESIS, Issue 7 2010Zeineb Aturki Abstract This article describes a method for the separation and determination of nine drugs of abuse in human urine, including amphetamines, cocaine, codeine, heroin and morphine. This method was based on SPE on a strong cation exchange cartridge followed by CEC-MS. The CEC experiments were performed in fused silica capillaries (100,,m×30,cm) packed with a 3,,m cyano derivatized silica stationary phase. A laboratory-made liquid junction interface was used for CEC-MS coupling. The outlet capillary column was connected with an emitter tip that was positioned in front of the MS orifice. A stable electrospray was produced at nanoliter per minute flow rates applying a hydrostatic pressure (few kPa) to the interface. The coupling of packed CEC columns with mass spectrometer as detector, using a liquid junction interface, provided several advantages such as better sensitivity, low dead volume and independent control of the conditions used for CEC separation and ESI analysis. For this purpose, preliminary experiments were carried out in CEC-UV to optimize the proper mobile phase for CEC analysis. Good separation efficiency was achieved for almost all compounds, using a mixture containing ACN and 25,mM ammonium formate buffer at pH 3 (30:70, v/v), as mobile phase and applying a voltage of 12,kV. ESI ion-trap MS detection was performed in the positive ionization mode. A spray liquid, composed by methanol,water (80:20, v/v) and 1% formic acid, was delivered at a nano-flow rate of ,200,nL/min. Under optimized CEC-ESI-MS conditions, separation of the investigated drugs was performed within 13,min. CEC-MS and CEC-MS2 spectra were obtained by providing the unambiguous confirmation of these drugs in urine samples. Method precision was determined with RSDs values ,3.3% for retention times and ,16.3% for peak areas in both intra-day and day-to-day experiments. LODs were established between 0.78 and 3.12,ng/mL for all compounds. Linearity was satisfactory in the concentration range of interest for all compounds (r2,0.995). The developed CEC-MS method was then applied to the analysis of drugs of abuse in spiked urine samples, obtaining recovery data in the range 80,95%. [source] Analysis of lamotrigine and its metabolites in human plasma and urine by micellar electrokinetic capillary chromatographyELECTROPHORESIS, Issue 4-5 2005Vincenzo Pucci Abstract A reliable micellar electrokinetic capillary chromatographic method was developed and validated for the determination of lamotrigine and its metabolites in human plasma and urine. The variation of different parameters, such as pH of the background electrolyte (BGE) and Sodium dodecyl sulfate (SDS) concentration, were evaluated in order to find optimal conditions. Best separation of the analytes was achieved using a BGE composed of 10 mM borate and 50 mM SDS, pH 9.5; melatonin was selected as the internal standard. Isolation of lamotrigine and its metabolites from plasma and urine was accomplished with an original solid-phase extraction procedure using hydrophilic-lypophilic balance cartridges. Good absolute recovery data and satisfactory precision values were obtained. The calibration plots for lamotrigine and its metabolites were linear over the 1,20 ,g/mL concentration range. Sensitivity was satisfactory; the limits of detection and quantitation of lamotrigine were 500 ng/mL and 1 ,g/mL, respectively. The application of the method to real plasma samples from epileptic patients under therapy with lamotrigine gave good results in terms of accuracy and selectivity, and in agreement with those obtained with an high-performance liquid chromatography (HPLC) method.* [source] Bayesian hierarchical generalized linear models for a geographical subset of recovery dataENVIRONMETRICS, Issue 2 2002Daniela Cocchi Abstract The aim of this work is to check whether modifications in the length of the hunting seasons had an effect on the chance of reproduction of different species of ringed birds. We start from a national data set of ringing-recovered data on three species of game birds. Only data on birds recovered as juveniles are used. Data on recoveries are organized in a 4-way contingency table. Several generalized linear models are proposed for the counts of recovered birds. Bayesian hierarchical modeling is particularly suitable for this kind of data, for which an over-dispersion parameter can be introduced at the second level of the hierarchy. Maximum Likelihood and Bayesian solutions are computed for the different models: the Bayesian framework, in particular under an individual modeling of over-dispersion, exhibits the best fit in terms of Bayesian p -value. The results show that the modification in the length of the hunting seasons does not produce equal benefits for the three species considered. Copyright © 2002 John Wiley & Sons, Ltd. [source] Factors influencing Soay sheep survivalJOURNAL OF THE ROYAL STATISTICAL SOCIETY: SERIES C (APPLIED STATISTICS), Issue 4 2000E. A. Catchpole We present a survival analysis of Soay sheep mark recapture and recovery data. Unlike previous conditional analyses, it is not necessary to assume equality of recovery and recapture probabilities; instead these are estimated by maximum likelihood. Male and female sheep are treated separately, with the higher numbers and survival probabilities of the females resulting in a more complex model than that used for the males. In both cases, however, age and time aspects need to be included and there is a strong indication of a reduction in survival for sheep aged 7 years or more. Time variation in survival is related to the size of the population and selected weather variables, by using logistic regression. The size of the population significantly affects the survival probabilities of male and female lambs, and of female sheep aged 7 or more years. March rainfall and a measure of the North Atlantic oscillation are found to influence survival significantly for all age groups considered, for both males and females. Either of these weather variables can be used in a model. Several phenotypic and genotypic individual covariates are also fitted. The only covariate which is found to influence survival significantly is the type of horn of first-year female sheep. There is a substantial variation in the recovery probabilities over time, reflecting in part the increased effort when a population crash was expected. The goodness of fit of the model is checked by using graphical procedures. [source] Demography and population viability of polar bears in the Gulf of Boothia, NunavutMARINE MAMMAL SCIENCE, Issue 4 2009Mitchell K. Taylor Abstract We estimated demographic parameters and harvest risks for polar bears (Ursus maritimus) inhabiting the Gulf of Boothia, Nunavut, from 1976 to 2000. We computed survival and abundance from capture,recapture and recovery data (630 marks) using a Burnham joint live,dead model implemented in program MARK. Annual mean total survival (including harvest) was 0.889 ± 0.179 (x,± 1 SE) for cubs, 0.883 ± 0.087 for subadults (ages 1,4), 0.919 ± 0.044 for adult females, and 0.917 ± 0.041 for adult males. Abundance in the last 3 yr of study was 1,592 ± 361 bears. Mean size of newborn litters was 1.648 ± 0.098 cubs. By age 7, 0.97 ± 0.30 of available females were producing litters. Harvest averaged 38.4 ± 4.2 bears/year in the last 5 yr of study; however, the 2002,2007 kill averaged 56.4 bears/yr. We used a harvested Population Viability Analysis (PVA) to examine impacts of increasing rates of harvest. We estimated the current population growth rate, ,H, to be 1.025 ± 0.032. Although this suggests the population is growing, progressive environmental changes may require more frequent population inventory studies to maintain the same levels of harvest risk. [source] |