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Analytical Methods (analytical + methods)
Kinds of Analytical Methods Selected AbstractsGetting the Scale Right: A Comparison of Analytical Methods for Vulnerability Assessment and Household-level TargetingDISASTERS, Issue 2 2001Linda Stephen This paper introduces broad concepts of vulnerability, food security and famine. It argues that the concepts and theories driving development and implementation of vulnerability assessment tools are related to their utility. The review concludes that socio-geographic scale is a key issue, and challenge. It analyses three vulnerability assessment (VA) methods, using Ethiopia as a case study. Facing the challenges of vulnerability assessment and early warning requires providing accurate information at the required scale, useful for multiple decision-makers within realistic institutional capacities. [source] FEM-Simulation of Real and Artificial Microstructures of Mo-Si-B Alloys for Elastic Properties and Comparison with Analytical Methods,ADVANCED ENGINEERING MATERIALS, Issue 10 2007G. Biragoni Various three phase microstructures of Mo-Si-B alloys were simulated in tensile loading conditions using a 2D finite element method to predict the elastic properties of the composite material. Voronoi structures with the same areal fraction of phases as the real microstructures have been generated and simulated similarly. Also, with these Voronoi structures a variation of grain or phase sizes, respectively, was carried out for different compositions in order to study on the elastic properties of the composite. Finally, a comparison was made over the whole temperature range between the above numerical methods, classical analytical approaches and experimentally determined values for Young's modulus E, shear modulus G and Poisson's ratio ,. [source] Analytical Methods for Transient Flow to a Well in a Confined-Unconfined AquiferGROUND WATER, Issue 4 2008Li-Tang Hu Concurrent existence of confined and unconfined zones of an aquifer can arise owing to ground water withdrawal by pumping. Using Girinskii's potential function, Chen (1974, 1983) developed an approximate analytical solution to analyze transient ground water flow to a pumping well in an aquifer that changes from an initially confined system to a system with both unconfined and confined regimes. This article presents the details of the Chen model and then compares it with the analytical model developed by Moench and Prickett (1972) for the same problem. Hypothetical pumping test examples in which the aquifer undergoes conversion from confined to water table conditions are solved by the two analytical models and also a numerical model based on MODFLOW. Comparison of the results suggests that the solutions of the Chen model give better results than the Moench and Prickett model except when the radial distance is very large or aquifer thickness is large compared with drawdown. [source] Onion Cells After High Pressure and Thermal Processing: Comparison of Membrane Integrity Changes Using Different Analytical Methods and Impact on Tissue TextureJOURNAL OF FOOD SCIENCE, Issue 7 2010Maria E. Gonzalez Abstract:, Two different analytical methods were evaluated for their capacity to provide quantitative information on onion cell membrane permeability and integrity after high pressure and thermal processing and to study the impact of these processing treatments on cell compartmentalization and texture quality. To determine changes in cell membrane permeability and/or integrity the methodologies utilized were: (1) measurement of a biochemical product, pyruvate, formed as a result of membrane permeabilization followed by enzymatic activity and (2) leakage of electrolytes into solution. These results were compared to previously determined methods that quantified cell viability and 1H-NMR T2 of onions. These methods allowed for the monitoring of changes in the plasma and tonoplast membranes after high pressure or thermal processing. High pressure treatments consisted of 5 min holding times at 50, 100, 200, 300, or 600 MPa. Thermal treatments consisted of 30 min water bath exposure to 40, 50, 60, 70, or 90 °C. There was strong agreement between the methods in the determination of the ranges of high pressure and temperature that induce changes in the integrity of the plasma and tonoplast membranes. Membrane rupture could clearly be identified at 300 MPa and above in high pressure treatments and at 60 °C and above in the thermal treatments. Membrane destabilization effects could already be visualized following the 200 MPa and 50 °C treatments. The texture of onions was influenced by the state of the membranes and was abruptly modified once membrane integrity was lost. Practical Application:, In this study, we used chemical, biochemical, and histological techniques to obtain information on cell membrane permeability and onion tissue integrity after high pressure and thermal processing. Because there was strong agreement between the various methods used, it is possible to implement something relatively simple, such as ion leakage, into routine quality assurance measurements to determine the severity of preservation methods and the shelf life of processed vegetables. [source] Phthalate Esters in Foods: Sources, Occurrence, and Analytical MethodsCOMPREHENSIVE REVIEWS IN FOOD SCIENCE AND FOOD SAFETY, Issue 1 2010Xu-Liang Cao ABSTRACT:, Phthalates are a group of diesters of ortho-phthalic acid (dialkyl or alkyl aryl esters of 1,2-benzenedicarboxylic acid). Higher-molecular-weight phthalates, such as di-2-ethylhexyl phthalate (DEHP), are primarily used as plasticizers to soften polyvinyl chloride (PVC) products, while the lower-molecular-weight phthalates, such as diethyl phthalate (DEP), di-n-butyl phthalate (DBP), and butyl benzyl phthalate (BBzP), are widely used as solvents to hold color and scent in various consumer and personal care products. Phthalates have become ubiquitous environmental contaminants due to volatilization and leaching from their widespread applications, and thus contamination of the environment has become another important source for phthalates in foods in addition to migration from packaging materials. Human exposure to phthalates has been an increased concern due to the findings from toxicology studies in animals. DEHP, one of the important and widely used phthalates, is a rodent liver carcinogen. DEHP, DBP, BBzP, and several phthalate metabolites, such as monobutyl phthalate, monobenzyl phthalate, and mono-(2-ethylhexyl) phthalate, are teratogenic in animals. Since foods are the major source of exposure to phthalates, information on levels of phthalates in foods is important for human exposure assessment. The objective of this review is to identify the knowledge gaps for future investigations by reviewing levels of a wide range of phthalates in a variety of foods, such as bottled water, soft drinks, infant formula, human milk, total diet foods, and others, migration of phthalates from various food-packaging materials, and traditional and new methodologies for the determination of phthalates in foods. [source] Commercial manufacturing scale formulation and analytical characterization of therapeutic recombinant antibodiesDRUG DEVELOPMENT RESEARCH, Issue 3 2004Reed J. Harris Abstract Stable therapeutic antibody dosage forms present production technology challenges, particularly when high-concentration formulations are needed to meet the elevated dose requirements that are generally required for successful antibody therapy. Solid dosage forms, such as lyophilized powders, are generally more stable than liquid formulations. High-concentration drug products can be achieved by reconstitution of the lyophilisate in a smaller volume than its initial (pre-lyophilization) volume, but requires a significant vial overfill. High-concentration liquid formulations are becoming feasible as new techniques and technologies become available. Analytical methods to detect subtle molecular variations have been developed to demonstrate manufacturing consistency. Some molecular heterogeneity is contributed by conserved sites, such as Asn297 glycosylation and the loss of heavy chain C-terminal Lys residues. Characteristics that affect potency, stability, or immunogenicity must be elucidated for each therapeutic antibody. Drug Dev. Res. 61:137,154, 2004. © 2004 Wiley-Liss, Inc. [source] Use of dispersal,vicariance analysis in biogeography , a critiqueJOURNAL OF BIOGEOGRAPHY, Issue 1 2010Ullasa Kodandaramaiah Abstract Aim, Analytical methods are commonly used to identify historical processes of vicariance and dispersal in the evolution of taxa. Currently, dispersal,vicariance analysis implemented in the software diva is the most widely used method. Despite some recognized shortcomings of the method, it has been treated as error-free in many cases and used extensively as the sole method to reconstruct histories of taxa. In light of this, an evaluation of the limitations of the method is needed, especially in relation to several newer alternatives. Methods, In an approach similar to simulation studies in phylogenetics, I use hypothetical taxa evolving in specific geological scenarios and test how well diva reconstructs their histories. Results,diva reconstructs histories accurately when evolution has been simple; that is, where speciation is driven mainly by vicariance. Ancestral areas are wrongly identified under several conditions, including complex patterns of dispersals and within-area speciation events. Several potentially serious drawbacks in using diva for inferences in biogeography are discussed. These include the inability to distinguish between contiguous range expansions and across-barrier dispersals, a low probability of invoking extinctions, incorrect constraints set on the maximum number of areas by the user, and analysing the ingroup taxa without sister groups. Main conclusions, Most problems with inferences based on diva are linked to the inflexibility and simplicity of the assumptions used in the method. These are frequently invalid, resulting in spurious reconstructions. I argue that it might be dangerous to rely solely on diva optimization to infer the history of a group. I also argue that diva is not ideally suited to distinguishing between dispersal and vicariance because it cannot a priori take into account the age of divergences relative to the timing of barrier formation. I suggest that other alternative methods can be used to corroborate the findings in diva, increasing the robustness of biogeographic hypotheses. I compare some important alternatives and conclude that model-based approaches are promising. [source] Development of liquid chromatography/mass spectrometry methods for the quantitative analysis of herbal medicine in biological fluids: a reviewBIOMEDICAL CHROMATOGRAPHY, Issue 1 2010Michael J. Gray Abstract The development of liquid chromatography,mass spectrometry (LC-MS) and tandem MS/MS for the analysis of bioactive components and their metabolites of herbal medicines in biological fluids is reviewed with the aim of providing an overview of the current techniques and methods used. The issues and challenges associated with various stages of the analytical method development are discussed using Ginkgo biloba and Panax ginseng as case studies. LC-MS offers selectivity and specificity in both the chromatographic separation and detection steps. This is necessary in order to measure compounds at extremely low concentrations as is often observed in plasma and urine samples. Traditional methods of detection (UV,visible) do not offer sufficient selectivity and specificity needed. The strategies and pitfalls involved with the measurement of such compounds are discussed in this review. Matrix effects, ,unseen' matrix suppression and enhancement ionization effects can significantly reduce the accuracy and precision of the measurement. The impact of the correct choice of chromatography column formats on signal-to-noise ratio is also discussed. Analytical methods from sample preparation to mass spectrometric detection is outlined in order to provide good direction for analysts intent on the measurement of bioavailable compounds from herbal medicines in plasma and urine samples. Copyright © 2009 John Wiley & Sons, Ltd. [source] Preclinical Manufacture of Anti-HER2 Liposome-Inserting, scFv-PEG-Lipid Conjugate.BIOTECHNOLOGY PROGRESS, Issue 1 2005Analytical methods optimized for micellar F5cys-MP-PEG(2000)-DPSE protein-lipopolymer conjugate are presented. The apparent micelle molecular weight, determined by size exclusion chromatography, ranged from 330 to 960 kDa. The F5cys antibody and conjugate melting points, determined by differential scanning calorimetry, were near 82 °C. Traditional methods for characterizing monodisperse protein species were inapplicable to conjugate analysis. The isoelectric point of F5cys (9.2) and the conjugate (8.9) were determined by capillary isoelectric focusing (cIEF) after addition of the zwitterionic detergent CHAPS to the buffer. Conjugate incubation with phospholipase B selectively removed DSPE lipid groups and dispersed the conjugate prior to separation by chromatographic methods. Alternatively, adding 2-propanol (29.4 vol %) and n -butanol (4.5 vol %) to buffers for salt-gradient cation exchange chromatography provided gentler, nonenzymatic dispersion, resulting in well-resolved peaks. This method was used to assess stability, identify contaminants, establish lot-to-lot comparability, and determine the average chromatographic purity (93%) for conjugate lots, described previously. The F5cys amino acid content was confirmed after conjugation. The expected conjugate avidity for immobilized HER-2/neu was measured by bimolecular interaction analysis (BIAcore). Mock therapeutic assemblies were made by conjugate insertion into preformed doxorubicin-encapsulating liposomes for antibody-directed uptake of doxorubicin by HER2-overexpressing cancer cells in vitro. Together these developed assays established that the manufacturing method as described in the first part of this study consistently produced F5cys-MP-PEG(2000)-DSPE having sufficient purity, stability, and functionality for use in preclinical toxicology investigations. [source] Good practice in head and neck fine needle aspiration cytology as assessed by CUSUMCYTOPATHOLOGY, Issue 6 2002I. A. Robinson Providing data as evidence of good practice is becoming imperative to meet the demands of professional revalidation and clinical governance. Sensitivity and specificity are common performance measures in fine needle aspiration (FNA) but are vulnerable to discordant analytical methods. We introduce a CUSUM technique and show how it may be used to show attainment and maintenance of proficiency in head and neck (H&N) FNA. In addition, we show how it can be used to compare practices and demonstrate different performance for FNAs from different tissues; a fact that must be recognized by anyone devising minimum performance values. [source] Role of Pap Test terminology and age in the detection of carcinoma invasive and carcinoma in situ in medically underserved California womenDIAGNOSTIC CYTOPATHOLOGY, Issue 4 2004Lydia P. Howell M.D. Abstract Our goals were to evaluate Pap Test findings classified by the Bethesda system, and follow up biopsies from participants in the California Breast and Cervical Cancer Control Program (Ca-BCCCP) for: 1) correlation in the detection of carcinoma in situ (CIS) and carcinoma invasive (CI), and 2) age-related trends, with discussion in the context of the 2001 ASCCP Management Guidelines. Women (n = 52,339) who had their initial screening Pap Tests with Ca-BCCCP between January 1995,December 1999 were followed for diagnostic services through December 2000. Descriptive and analytical methods were used in the analysis. Of the Pap results, 81.9% were negative, 10.6% showed infection, 4.7% showed an epithelial abnormality as defined by the Bethesda system (atypical squamous cells of undertermined significance (ASCUS), low-grade squamous intraepithelial lesion (LSIL), or high-grade squamous intraepithelial lesion (HSIL)), 0.1% showed squamous-cell cancer (SCC), and 2.7% showed other or unsatisfactory. Subsequent to the initial Pap Test, follow-up results of carcinoma in situ (CIS) and carcinoma invasive (CI) accounted for 0.36% and 0.05% of the population, respectively. Among HSIL Pap Tests (n = 285), 40.7% had follow-up showing CIS. Among SCC Pap Tests, 17.9% had follow-up results of CIS and 28.6% CI. Of the 191 patients with CIS as a follow-up finding, the initial Pap smear showed: HSIL 60.7%, SCC 2.6%, LSIL 10.5%, ASCUS 13.6%, and negative or infection 9.9%. Of the 27 patients with CI, the initial Pap Test showed: HSIL 40.7%, SCC 29.6%, LSIL 7.4%, ASCUS 7.4%, and negative or infection 11.1%. Pap diagnoses of other or unsatisfactory accounted for 2.6% of the Pap results from patients with CIS and 3.7% of Pap results from patients with CI. Except for LSIL, there was an increasing age trend in the number of cases in each of Pap results, with the exception of age 65+ yr. However, the ratio of LSIL and ASCUS to negative cases decreased with age. (P < 0.0001 and 0.0293, respectively). HSIL Pap results indicate a reasonably high probability of CIS and CI. However, approximately 1/3 of patients with CIS and 1/4 of patients with CI presented with Pap diagnoses of less severity than HSIL. When a negative Pap Test result is chosen as reference group, there is a negative age trend for LSIL and ASCUS, and no age trend for other results. These findings all have important implications in the design of follow-up strategies, and support the 2001 ASCCP Consensus Guidelines for the Management of Women with Cervical Abnormalities. Diagn. Cytopathol. 2004;30:227,234. © 2004 Wiley-Liss, Inc. [source] Rapid evolution and the convergence of ecological and evolutionary timeECOLOGY LETTERS, Issue 10 2005Nelson G. Hairston Jr Abstract Recent studies have documented rates of evolution of ecologically important phenotypes sufficiently fast that they have the potential to impact the outcome of ecological interactions while they are underway. Observations of this type go against accepted wisdom that ecological and evolutionary dynamics occur at very different time scales. While some authors have evaluated the rapidity of a measured evolutionary rate by comparing it to the overall distribution of measured evolutionary rates, we believe that ecologists are mainly interested in rapid evolution because of its potential to impinge on ecological processes. We therefore propose that rapid evolution be defined as a genetic change occurring rapidly enough to have a measurable impact on simultaneous ecological change. Using this definition we propose a framework for decomposing rates of ecological change into components driven by simultaneous evolutionary change and by change in a non-evolutionary factor (e.g. density dependent population dynamics, abiotic environmental change). Evolution is judged to be rapid in this ecological context if its contribution to ecological change is large relative to the contribution of other factors. We provide a worked example of this approach based on a theoretical predator,prey interaction [Abrams, P. & Matsuda, H. (1997). Evolution, 51, 1740], and find that in this system the impact of prey evolution on predator per capita growth rate is 63% that of internal ecological dynamics. We then propose analytical methods for measuring these contributions in field situations, and apply them to two long-term data sets for which suitable ecological and evolutionary data exist. For both data sets relatively high rates of evolutionary change have been found when measured as character change in standard deviations per generation (haldanes). For Darwin's finches evolving in response to fluctuating rainfall [Grant, P.R. & Grant, B.R. (2002). Science, 296, 707], we estimate that evolutionary change has been more rapid than ecological change by a factor of 2.2. For a population of freshwater copepods whose life history evolves in response to fluctuating fish predation [Hairston, N.G. Jr & Dillon, T.A. (1990). Evolution, 44, 1796], we find that evolutionary change has been about one quarter the rate of ecological change , less than in the finch example, but nevertheless substantial. These analyses support the view that in order to understand temporal dynamics in ecological processes it is critical to consider the extent to which the attributes of the system under investigation are simultaneously changing as a result of rapid evolution. [source] Stochastic matrix models for conservation and management: a comparative review of methodsECOLOGY LETTERS, Issue 3 2001John Fieberg Stochastic matrix models are frequently used by conservation biologists to measure the viability of species and to explore various management actions. Models are typically parameterized using two or more sets of estimated transition rates between age/size/stage classes. While standard methods exist for analyzing a single set of transition rates, a variety of methods have been employed to analyze multiple sets of transition rates. We review applications of stochastic matrix models to problems in conservation and use simulation studies to compare the performance of different analytic methods currently in use. We find that model conclusions are likely to be robust to the choice of parametric distribution used to model vital rate fluctuations over time. However, conclusions can be highly sensitive to the within-year correlation structure among vital rates, and therefore we suggest using analytical methods that provide a means of conducting a sensitivity analysis with respect to correlation parameters. Our simulation results also suggest that the precision of population viability estimates can be improved by using matrix models that incorporate environmental covariates in conjunction with experiments to estimate transition rates under a range of environmental conditions. [source] Green Approaches to Field Nitrate Analysis: An Electroanalytical PerspectiveELECTROANALYSIS, Issue 7 2009Radha Desai Abstract The different approaches that have been taken in the development of analytical methods for the determination of nitrate within the field are reviewed. The emphasis has been placed on providing a critical appraisal of the chemistry that underpins current commercial systems and the need to remove the dependence on heavy metal and concentrated acid components. The search for more environmentally acceptable and user friendly systems has long been pursued and the present communication seeks to explore the recent development in portable testing technologies and how they might evolve in the future. In particular, the role of electrochemical techniques in the latter are investigated and their potential application compared and contrasted with the more traditional wet chemical detection strategies. [source] Electroactivity of Nonconjugated Proteins and Peptides.ELECTROANALYSIS, Issue 23 2007Towards Electroanalysis of All Proteins Abstract Present proteomics and biomedicine require sensitive analytical methods for all proteins. Recent progress in electrochemical analysis of peptides and proteins based on their intrinsic electroactivity is reviewed. Tyrosine and/or tryptophan-containing proteins are oxidizable at carbon electrodes. At mercury electrodes all peptides and proteins (about 13 peptides and >25 proteins were tested) produce chronopotentiometric peak H at nanomolar concentrations. This peak is sensitive to changes in protein structure. Microliter sample volumes are sufficient for the analysis. Electrochemical methods can be used in studies of nucleic acid-protein interactions and can be applied in biomedicine. Examples of such applications in neurogenerative diseases and cancer are presented. [source] Decomposition and reconstruction of signal in real-time spectral analysisELECTRONICS & COMMUNICATIONS IN JAPAN, Issue 11 2008Hideto Nakatsuji Abstract In recent years, wavelet transform which gives expression in the time,frequency domain has been adopted for a nonstationary process. The authors have proposed a new spectral analytical method in the time,frequency domain. In the conventional spectral analytical methods, the decomposition and the reconstruction of signals have been obtained analytically. The proposed method consists of two approaches. We call these approaches Approach 1 and Approach 2. In this paper, we show the decomposition and reconstruction of signals based on Approach 1. First, we show that the signal is decomposed to the signal elements. They are called the decomposition waves, and all of these decomposed waves are added to obtain the reconstructed wave. Next, we show the magnitude characteristic and the phase characteristic between the original signal and the reconstructed wave. Then the conditions between the signal and the reconstructed wave are derived to realize a sufficiently approximated wave. By a numeric calculation example, we show the approximation ability by the proposed method. © 2009 Wiley Periodicals, Inc. Electron Comm Jpn, 91(11): 37,45, 2008; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/ecj.10182 [source] Recent developments in peptide stereoisomer separations by capillary electromigration techniquesELECTROPHORESIS, Issue S1 2009Gerhard K. E. Scriba Abstract The stereochemistry of peptides determines their physicochemical and biological activities. Thus, analytical methods that are able to discriminate between peptide stereoisomers are important. As peptides are typically hydrophilic compounds, many methods for the separation of peptide diastereomers and enantiomers have been developed by capillary electromigration techniques. Moreover, peptide enantiomers displayed unique migration behavior such as a pH-dependent change of the enantiomer migration order in CD-mediated enantioseparations in CE making them ideal compounds to study mechanistic effects of enantioseparations. The present short review summarizes recent developments in the separation of stereoisomers of peptide and peptidomimetics by capillary electromigration techniques. Moreover, recent NMR and molecular modeling studies as well as investigation on the effect of buffer additives on complex formation will be discussed as attempts to understand mechanistic aspects of peptide enantioseparations and to analyze the structure of peptide-CD complexes. [source] IEF in microfluidic devicesELECTROPHORESIS, Issue 5 2009Greg J. Sommer Abstract IEF is one of the most powerful and prevalent techniques used in separation sciences. The power of IEF comes from the fact that it not only separates analytes based on their pI but also focuses them into highly resolved bands. In line with the miniaturization trend spurring the analytical community, the past decade has yielded a wealth of research focused on implementing IEF in microfluidic chip-based formats (,IEF). Scaling down the separation technique provides several advantages such as reduced sample sizes, assay automation, and significant improvements in assay speed without sacrificing separation performance. Besides presenting microscale adaptations of standard schemes, researchers have also developed improved detection techniques, demonstrated novel ,IEF assays, and incorporated ,IEF with other analytical methods for achieving on-chip multidimensional separations. This review provides a brief historical outline of IEF's beginnings, theoretical incentives driving miniaturization of the methodology, a thorough synopsis of ,IEF publications to date, and an outlook to the future. [source] Electrical field-assisted solid-phase extraction coupled on-line to capillary electrophoresis-mass spectrometryELECTROPHORESIS, Issue 10 2008Gabriel Morales-Cid Abstract A substantial demand currently exists for analytical methods affording the determination of very low concentrations of analytes in complex matrices, such as those of environmental and biological samples, as simply as possible. However, the pretreatment of complex samples, which is unavoidable prior to CE-MS analysis, is usually complicated and time-consuming. In this work, we used voltage-assisted SPE for the first time as an alternative to conventional treatments for preconcentrating and purifying analytes. To this end, we used a simple flow system coupled on-line to CE-MS equipment. The system is quite robust and provides reproducible peak areas (the precision ranges from 2.5 to 3.8%). Also, it provides increased sensitivity affording the determination of trace amounts (nanogram per liter levels) of analytes in only a few milliliters of sample. The proposed system was applied to the determination of members of two compound families (viz. tetracyclines and amines). [source] Microchip-based small, dense low-density lipoproteins assay for coronary heart disease risk assessmentELECTROPHORESIS, Issue 9 2008Hua Wang Abstract Small, dense low-density lipoprotein (sdLDL) has been accepted as an emerging cardiovascular risk factor, and there has been an increasing interest in analytical methods for sdLDL profiling for diagnosis. Serum sdLDL may be measured by different laboratory techniques, but all these methods are laborious, time-consuming, and costly. Recently, we have demonstrated that a low-temperature bonding of quartz microfluidic chips for serum lipoproteins analysis (Zhuang, G., Jin, Q., Liu, J., Cong, H. et al., Biomed. Microdevices 2006, 8, 255,261). In contrast to this previous study, we chose SDS as anionic surfactant to modify both lipoproteins and the channel surface to minimize lipoprotein adsorption and improve the resolution of lipoprotein separation. Two major LDL subclass patterns including large, buoyant LDL (lLDL), sdLDL, and high-density lipoprotein (HDL) were effectively separated with high reproducibility. RSD values of the migration time (min) and peak areas of standard LDL and HDL were 6.28, 4.02, 5.02, and 2.5%, respectively. Serum lipoproteins of 15 healthy subjects and 15 patients with coronary heart disease (CHD) were separated by microchip CE. No peaks of sdLDL were detected in serum samples of healthy subjects while sdLDL fractional peaks were observed in patients' entire serum samples. These results suggested that the microchip-based sdLDLs assay was a simple, rapid, and highly efficient technique and significantly improved the analysis of CHD risk factors. [source] Evaluation of different warping methods for the analysis of CE profiles of urinary nucleosidesELECTROPHORESIS, Issue 16 2007Ewa Szyma Abstract Nowadays, numerous metabolite concentrations can readily be determined in a given biological sample by high-throughput analytical methods. However, such raw analytical data comprise noninformative components due to many disturbances normally occurring in the analyses of biological material. To eliminate those unwanted original analytical data components, advanced chemometric data preprocessing methods might be of help. Here, such methods are applied to electrophoretic nucleoside profiles in urine samples of cancer patients and healthy volunteers. In this study, three warping methods: dynamic time warping (DTW), correlation optimized warping (COW), and parametric time warping (PTW) were examined on two sets of electrophoretic data by means of quality of peaks alignment, time of preprocessing, and way of customization. The application of warping methods helped to limit shifting of peaks and enabled differentiation between whole electropherograms of healthy and cancer patients objectively by a principal component analysis (PCA). The evaluation of preprocessed data and raw data by PC analysis confirms differences between the applied warping tools and proves their suitability in metabonomic data interpretation. [source] Computer-assisted 2-D agarose electrophoresis of Haemophilus influenzae type B meningitis vaccines and analysis of polydisperse particle populations in the size range of viruses: A reviewELECTROPHORESIS, Issue 4 2007Dietmar Tietz Dr. Abstract When protein,polysaccharide conjugated vaccines were first developed for the immunization of small children against meningitis caused by infection with Haemophilus influenzae type b (Hib), the vaccine preparations varied in immunogenicity. Testing for immunogenicity was time-consuming and alternative analytical procedures for determining vaccine quality were unsatisfactory. For example, due to the very high molecular weight of the vaccine particles, immunogens could only be physically characterized as a fraction in the void volume of Sepharose gel filtration. In search of better analytical methods, a computer-assisted electrophoretic technique for analyzing such vaccines was developed in the period from 1983 to 1995. This new approach made it possible to analyze highly negatively charged particles as large as or larger than intact viruses. 2-D gel patterns were generated that varied depending on the conditions of the particular vaccine preparation and were therefore characteristic of each vaccine sample. Thus, vaccine particle populations with a continuous size variation over a wide range (polydisperse) could be characterized according to size and free mobility (related to particle surface net charge density). These advances are reviewed in this article, since the developed methods are still a promising tool for vaccine quality control and for predicting immunogen effectiveness in the production of vaccines. The technique is potentially beneficial for Hib immunogens and other high-molecular-mass vaccines. Additional biomedical applications for this nondenaturing electrophoretic technique are briefly discussed and detailed information about computational and mathematical procedures and theoretical aspects is provided in the Appendices. [source] Advances in the enantioseparation of second-generation antidepressant drugs by electrodriven methodsELECTROPHORESIS, Issue 1 2006Roberto Mandrioli Abstract Stereochemistry is steadily increasing in importance in the development of new drugs, and the availability of pure enantiomer drugs can make therapy safer and more efficacious. In particular, almost all second-generation antidepressant drugs possess one or more chiral centres; however, only some of them are administered as single enantiomers. A fundamental part of the quality control of pharmaceutical formulations is the determination of enantiomeric excess and enantiomeric purity; this is also important for the therapeutic drug monitoring of depressed patients. For this purpose, efficient and reliable analytical methods are needed and electrodriven techniques (most of all CE, CEC and MEKC) are very efficient and inexpensive candidates for the role. In this review, the enantioselective electrodriven methods available for the analysis of second-generation antidepressant are presented and discussed. In particular, the following pharmacological classes of antidepressants will be considered: selective serotonin reuptake inhibitors (fluoxetine, citalopram, paroxetine, sertraline); norepinephrine reuptake inhibitors (reboxetine); serotonin and norepinephrine reuptake inhibitors (venlafaxine, milnacipran, duloxetine); and noradrenergic and specific serotonergic antidepressants (mirtazapine). [source] Tests for the toxicity assessment of cyanobacterial bloom samplesENVIRONMENTAL TOXICOLOGY, Issue 5 2001gorzata Tarczynska Abstract Cyanobacterial (blue,green algal) blooms are one of the common consequences of the increasing eutrophication of surface waters. The production of cyanobacterial toxins and their presence in drinking and recreational waters represents a growing danger to human and animal health. Due to a lack of toxin standards and to resource limitations on the wide-scale use of analytical methods (e.g., high-performance liquid chromatography, enzyme-linked immunosorbent assay (ELISA)) in cyanobacterial toxin monitoring, it is necessary to assess and to develop additional methods for their detection and estimation. Microbiotests using invertebrates offer a possible approach for the inexpensive and straightforward detection and assessment of cyanobacterial bloom toxicity. Three microbiotests with: Thamnocephalus platyurus, Daphnia magna, and Spirostomum ambiguum were examined with bloom samples containing hepatotoxic microcystin-LR and up to five additional microcystin variants. Two kinds of cyanobacterial bloom sample preparations were tested: crude extracts (CE) and purified extracts (PE). The highest toxicity was found when CE was used for microbiotests. The sensitivity of microorganisms decreased from S. ambiguum to T. platyurus and to D. magna. A statistically significant correlation was found between microcystin concentration and T. platyurus biotest, and between mouse bioassay and S. ambiguum results. Addition of Me2SO (1%, v/v) is a possible method to increase the sensitivity of the microorganisms for microcystin-LR. © 2001 John Wiley & Sons, Inc. Environ Toxicol 16: 383,390, 2001 [source] Exposure assessment of 17,-ethinylestradiol in surface waters of the United States and Europe,ENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 12 2009Robert Hannah Abstract An evaluation of measured and predicted concentrations of 17,-ethinylestradiol in surface waters of the United States and Europe was conducted to develop expected long-term exposure concentrations for this compound. Measured environmental concentrations (MECs) in surface waters were identified from the literature. Predicted environmental concentrations (PECs) were generated for European and U.S. watersheds using the GREAT-ER and PhATEÔ models, respectively. The majority of MECs are nondetect and generally consistent with model PECs and conservative mass balance calculations. However, the highest MECs are not consistent with concentrations derived from conservative (worst-case) mass balance estimates or model PECs. A review of analytical methods suggests that tandem or high-resolution mass spectrometry methods with extract cleanup result in lower detection limits and lower reported concentrations consistent with model predictions and bounding estimates. Based on model results using PhATE and GREAT-ER, the 90th-percentile low-flow PECs in surface water are approximately 0.2 and 0.3 ng/L for the United States and Europe, respectively. These levels represent conservative estimates of long-term exposure that can be used for risk assessment purposes. Our analysis also indicates that average concentrations are one to two orders of magnitude lower than these 90th-percentile estimates. Higher reported concentrations (e.g., greater than the 99th-percentile PEC of ,1 ng/L) could result from methodological problems or unusual environmental circumstances; however, such concentrations are not representative of levels generally found in the environment, warrant special scrutiny, and are not appropriate for use in risk assessments of long-term exposures. [source] InN@SiO2 Nanomaterials as New Blue Light EmittersEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 23 2008Prabhakaran Munusamy Abstract In this article we report blue photoluminescence (, 450 nm) from InN@SiO2 nanomaterials. The InN@SiO2 nanomaterials were prepared by a simple precipitation reaction followed by a solid-state reaction. Various control experiments demonstrate that the interface between the InN and SiO2 seems to play a crucial role in the origin of the blue emission from the InN@SiO2 nanomaterial. The InN@SiO2 nanomaterial was characterized by using analytical methods such as TEM, XRD, Raman, XPS, and photoluminescence spectroscopy, which confirmed the existence of InN on SiO2 with a small excess of nitrogen relative to indium.(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008) [source] Comparative analysis of triacylglycerols from Olea europaea L. fruits using HPLC and MALDI-TOFMSEUROPEAN JOURNAL OF LIPID SCIENCE AND TECHNOLOGY, Issue 5 2010Faouzi Sakouhi Abstract MALDI-TOFMS and HPLC are two analytical methods that were used to characterize triacylglycerols (TAG) of the Meski, Sayali, and Picholine Tunisian olive varieties. The HPLC chromatograms of the oils showed the presence of 15 TAG species, among which triolein (OOO) was the most abundant (21,48%). In the Sayali cultivar, OOO was the predominant TAG species followed by POO and LOO. However, the minor TAG molecules were represented by LnLO and LnLP. MALDI mass spectra produced sodiated ([M,+,Na]+) and potassiated ([M,+,K]+) TAG molecules; only the major TAG were potassiated [OOO,+,K] ([OOO,+,K]+, [POO,+,K]+, and [LOO,+,K]+). In contrast to the HPLC chromatograms, the MALDI mass spectra showed 13 peaks of TAG. The major peak was detected at m/z,907, which corresponds to OOO with an Na+ adduct. The results from both HPLC and MALDI techniques predict the fatty acid composition and their percentages for each olive variety. Practical applications: TAG are the main components in vegetable oils. These biomolecules determine the physical, chemical, and nutritional properties of the oils. The nutritional benefits of TAG are related to DAG (moderate plasma lipid level) and esterified FA, which are intermediate biosynthetic molecules of TAG. TAG analysis is necessary to discriminate between oils of different origin, since some oils have similar FA profiles. Olive products, oils, and table olives, are the main diet sources of TAG in the Mediterranean countries. In this work, chromatographic and spectrometric methods were used for TAG analysis and characterization of Tunisian olive varieties. [source] Stepwise geographical traceability of virgin olive oils by chemical profiles using artificial neural network modelsEUROPEAN JOURNAL OF LIPID SCIENCE AND TECHNOLOGY, Issue 10 2009Diego L. García-González Abstract The geographical traceability of virgin olive oils implies the use of analytical methods that allow the identification of the origin of the oil and the authentication of the information boasted on the labels. In this work, the geographical identification of the virgin olive oils has been addressed by complete chemical characterisation of samples (64 compounds analysed by GC and HPLC) and the design of artificial neural network (ANN) models for each one of the levels of a proposed classification scheme. A high number of samples (687) from Spain, Italy and Portugal served as training and test sets for the ANN models. The highest classification level, focused on the grouping of samples by country, was achieved through analysis of fatty acids, with 99.9% of samples classified. Other levels (region, province, Protected Designations of Origin or PDO) were focused on Spanish oils and required additional series of compounds (sterols, alcohols, hydrocarbons) as well as the fatty acids to obtain classification rates higher than 90%. The classification of oils into different PDOs , the last and most difficult level of classification , showed the highest root mean square errors. The classification percentages, however, were still higher than 90% in the test set, which proves the application of the traceability methodology for a chemical verification of PDO claims. [source] Temperature-Dependent Solid-State Reactions With and Without Kirkendall Effect in Al2O3/ZnO, Fe2O3/ZnO, and CoXOY/ZnO Oxide Thin Film Systems,ADVANCED ENGINEERING MATERIALS, Issue 6 2010Andriy Zolotaryov Temperature-dependent solid-state reactions and the occurrence of the Kirkendall effect are studied in thin film oxide systems applying optical reflection microscopy, X-ray reflectivity, (scanning) transmission electron microscopy, grazing-incidence X-ray diffraction measurements, and SQUID magnetometry. The efficiency of the simultaneous application of different analytical methods for the precise selection and investigation of the most interesting samples is demonstrated first on the example of the Al2O3/ZnO system, for which the spinel formation after a solid-state reaction and the formation of Kirkendall voids were already reported. The demonstrated methodology is then applied to study Fe2O3/ZnO and CoXOY/ZnO film pairs. The investigations clearly demonstrate the temperature-driven formation of a ferromagnetic spinel by a solid state reaction involving the Kirkendall effect in the Fe2O3/ZnO system, already after an annealing at 600,°C for 1,h. We also report on the solid state reaction in the CoXOY/ZnO system after annealing at 700,°C for 1,h, however without the Kirkendall effect and without any evidence of ferromagnetism of the final state. [source] Comparison of Cyclodextrin-Dipeptide Inclusion Complexes in the Absence and Presence of Urea by Means of Capillary Electrophoresis, Nuclear Magnetic Resonance and Molecular ModelingEUROPEAN JOURNAL OF ORGANIC CHEMISTRY, Issue 18 2007Benjamin Waibel Abstract The use of capillary electrophoresis (CE) modified with cyclodextrin (CD) for the separation of stereoisomers of peptides is well established. To increase the solubility of ,-CD, urea is often added to the buffer which may influence the complexation of a CD with a guest molecule. The aim of the present study was to investigate the influence of urea on the complexation between dipeptides and ,-CD using Ala-Phe and Ala-Tyr as model compounds. For this purpose three different analytical methods were employed: capillary electrophoresis (CE), 1H-NMR spectroscopy and molecular dynamics simulations (MD). Electropherograms of the peptide enantiomers were different in the presence and absence of urea. For example, at pH,2.5 in the absence of urea the enantiomers of Ala-Tyr are not separated in contrast to the use of buffers containing urea. Applying "complexation-induced chemical shift (CICS)" in NMR spectroscopy and rotating frame Overhauser enhancement spectroscopy (ROESY) revealed differences in the complexation of the peptide enantiomers by ,-CD in the absence and presence of urea suggesting the stabilization of the complex through the phenolic hydroxyl group of tyrosine. MD simulations for different complexes were carried out with consideration of both water and urea molecules in solution. Simulations were performed for 1 ns. In conclusion, NMR spectroscopy and MD methods help to understand the structure of peptide-CD complexes and the separation and migration behavior in CE. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007) [source] | ||||||||||||||||||||||||||||||||||||||||||||||