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Analytical Methodology (analytical + methodology)
Selected AbstractsAnalytical methodologies for quantification of ferulic acid and its oligomersJOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE, Issue 9 2008Hélène Barberousse Abstract Ferulic acid (4-hydroxy-3-methoxycinnamic acid) is the most widespread hydroxycinnamic acid in the plant world, where it is a key molecule in cell wall architecture. Owing to its high antioxidant properties, ferulic acid shows large potential applications in food industry as well as in the health and cosmetic markets. There is thus a high interest in extracting this high-value compound from waste materials of the agricultural industry, which requires the selection of an appropriate quantification method. This paper therefore gives an overview of analytical methodologies developed over past decades for quantification of ferulic acid and its oligomers. Copyright © 2008 Society of Chemical Industry [source] Recent advances in the analysis of antibiotics by CE and CECELECTROPHORESIS, Issue 1 2010María Castro-Puyana Abstract This article reviews the latest advances in the development of analytical methodologies by CE and CEC for the analysis of different groups of antibiotics. CZE and MEKC have been the most employed CE modes. Analytical information on experimental conditions, detection mode, and LOD are provided to the readers. In addition, the main applications performed in the pharmaceutical, biological, food, and environmental fields have been reviewed emphasizing the sample preparation requirements. The publications reviewed cover the period of time from June 2007 to May 2009. [source] Cover Picture: Electrophoresis 15'09ELECTROPHORESIS, Issue 15 2009Article first published online: 7 AUG 200 Issue no. 15 is a regular issue consisting of 20 research papers distributed over 7 different parts dealing with various fundamental studies, analytical methodologies, various aspects of proteins and protein biomarkers, affinity studies, genetics, pathogens and toxins, and enantioseparations. [source] Variable carbon recovery of Walkley-Black analysis and implications for national soil organic carbon accountingEUROPEAN JOURNAL OF SOIL SCIENCE, Issue 6 2007S. Lettens Summary There is considerable interest in the computation of national and regional soil carbon stocks, largely as the result of the provisions of the Kyoto Protocol. Such stocks are often calculated and compared without proper reference to the uncertainties induced by different analytical methodologies. We illustrate the nature and magnitude of these uncertainties with the present soil organic carbon (SOC) study in Belgium. The SOC recovery of the Walkley-Black method was investigated based on a database of 475 samples of silt loam and sandy soils, which cover different soil depths and vegetation types in northern Belgium. The organic carbon content of the soil samples was measured by the original Walkley-Black method and by a total organic carbon analyser. The recovery was computed as the ratio of these two results per soil sample. Land use, texture and soil sampling depth had a significant influence on the recovery as well as their three-way interaction term (land use × texture × sampling depth). The impact of a land use, texture and sampling depth dependent Walkley-Black correction on the year 2000 SOC inventory of Belgium was determined by regression analysis. Based on new correction factors, the national SOC stocks increased by 22% for the whole country, ranging from 18% for cropland to 31% for mixed forest relative to the standard corrected SOC inventory. The new recovery values influenced therefore not only C stocks in the year 2000, but also the expected SOC change following land use change. Adequate correction of Walkley-Black measurements is therefore crucial for the absolute and comparative SOC assessments that are required for Kyoto reporting and must be computed to take into account the regional status of soil and land use. ,Universal' corrections are probably an unrealistic expectation. [source] Monitoring neuropeptide-specific proteases: processing of the proopiomelanocortin peptides adrenocorticotropin and , -melanocyte-stimulating hormone in the skinEXPERIMENTAL DERMATOLOGY, Issue 10 2006Simone König Abstract:, The neuroendocrine precursor protein proopiomelanocortin (POMC) and its derived neuropeptides are involved in a number of important regulatory processes in the central nervous system as well as in peripheral tissues. Despite its important role in controlling the local activation of melanocortin (MC) receptors, the extracellular proteolytic processing of POMC peptides has received little attention. The mechanisms relevant for controlling the bioavailability of adrenocorticotropin and melanocyte-stimulating hormones for the corresponding MC receptors in the skin by specific peptidases such as neprilysin (neutral endopeptidase; NEP) or angiotensin-converting enzyme (ACE) have been addressed in a number of recent investigations. This review summarizes the current body of knowledge concerning the qualitative and quantitative POMC peptide processing with respect to the action and specificity of NEP and ACE and discusses relevant recent analytical methodologies. [source] Solid-state glycation of ,-lactoglobulin by lactose and galactose: localization of the modified amino acids using mass spectrometric techniquesJOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 1 2004François Fenaille Abstract The Maillard reaction is commonly encountered during food processing or storage, and also in human nutrition, hence there is a need for analytical methodologies to identify and characterize the modified proteins. This paper reports specific methods using mass spectrometric techniques to localize protein modifications induced by lactose and galactose on ,-lactoglobulin (,-Lg) under solid-state glycation conditions. The extent of glycation was first determined by liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS). The specific identification of lactose-modified amino acid residues was realized using both NanoESI-MS, NanoESI-MS/MS (neutral loss scanning modes) and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) (with and without guanidination of lysine residues) on unfractionated digests. The results indicated that, after 8.25 h of incubation, the lysine residues were the main targets of lactose-induced modification. In addition to the 15 lysine residues, Leu1 (NH2 terminal) and the Arg124 were also found to be modified, thus leading to a total of 17 different modified amino acid residues (versus 15 found by LC/ESI-MS measurement). In a second set of experiments, different strategies consisting of constant neutral loss and precursor ion scanning were compared to characterize galactose-induced modifications. Owing to the high level of ,-Lg glycation, the combined use of these different strategies appeared to be necessary for determining the galactose-modified sites after 8.25 h of incubation. Thus, among the 22 galactose adducts deduced from the LC/ESI-MS measurement, apart from the N-terminal and classical lysine residues, we also observed a few arginine residues (Arg40, Arg124 and Arg148) that were modified, and also dialkylations on specific lysine residues (Lys47, Lys75). Copyright © 2003 John Wiley & Sons, Ltd. [source] Modified headspace-SPME-GC device for sampling volatile compounds in acidic mediumJOURNAL OF SEPARATION SCIENCE, JSS, Issue 6-7 2003W. A. Araújo Abstract Most of the existing analytical methods for determining dithiocarbamate pesticide residues utilize an acid decomposition step, which promotes the release of carbon disulfide from the pesticide molecule. After release, the CS2 is sampled by static headspace techniques using gas-tight syringes and analyzed by gas chromatography with flame photometric detection (GC-FPD). In our search for faster analytical methodologies for sampling of volatile compounds we have used solid phase microextraction (SPME). However, evaluation of the commercially available SPME system for the analysis of CS2 obtained by decomposing dithiocarbamates showed it to be unsuitable for analysis in an acidic environment. The present communication reports the development of an appropriate device for sampling volatile compounds in an acidic environment by static headspace-SPME followed by GC-FPD. On examining the limitations of using a standard metal needle in HS-SPME sampling of analytes in acidic medium, a corrosion process was observed in both needle and fiber. A new double-needle device which avoids such corrosion problems was developed and built. The successful application of this device to the analysis of mancozeb in water samples is described. [source] Analytical methodologies for quantification of ferulic acid and its oligomersJOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE, Issue 9 2008Hélène Barberousse Abstract Ferulic acid (4-hydroxy-3-methoxycinnamic acid) is the most widespread hydroxycinnamic acid in the plant world, where it is a key molecule in cell wall architecture. Owing to its high antioxidant properties, ferulic acid shows large potential applications in food industry as well as in the health and cosmetic markets. There is thus a high interest in extracting this high-value compound from waste materials of the agricultural industry, which requires the selection of an appropriate quantification method. This paper therefore gives an overview of analytical methodologies developed over past decades for quantification of ferulic acid and its oligomers. Copyright © 2008 Society of Chemical Industry [source] Application of mass spectrometry in the analysis of polybrominated diphenyl ethersMASS SPECTROMETRY REVIEWS, Issue 5 2010Dongli Wang Abstract This review summarized the applications of mass spectrometric techniques for the analysis of the important flame retardants polybrominated diphenyl ethers (PBDEs) to understand the environmental sources, fate and toxicity of PBDEs that were briefly discussed to give a general idea for the need of analytical methodologies. Specific performance of various mass spectrometers hyphenated with, for example, gas chromatograph, liquid chromatograph, and inductively coupled plasma (GC/MS, LC/MS, and ICP/MS, respectively) for the analysis of PBDEs was compared with an objective to present the information on the evolution of MS techniques for determining PBDEs in environmental and human samples. GC/electron capture negative ionization quadrupole MS (GC/NCI qMS), GC/high resolution MS (GC/HRMS) and GC ion trap MS (GC/ITMS) are most commonly used MS techniques for the determination of PBDEs. New analytical technologies such as fast tandem GC/MS and LC/MS become available to improve analyses of higher PBDEs. The development and application of the tandem MS techniques have helped to understand environmental fate and transformations of PBDEs of which abiotic and biotic degradation of decaBDE is thought to be one major source of Br1-9BDEs present in the environment in addition to direct loading from commercial mixtures. MS-based proteomics will offer an insight into the molecular mechanisms of toxicity and potential developmental and neurotoxicity of PBDEs. © 2009 Wiley Periodicals, Inc., Mass Spec Rev 29:737,775, 2010 [source] The problem with "the Paleoptera Problem:" sense and sensitivityCLADISTICS, Issue 5 2003T.Heath Ogden While the monophyly of winged insects (Pterygota) is well supported, phylogenetic relationships among the most basal extant pterygote lineages are problematic. Ephemeroptera (mayflies) and Odonata (dragonflies) represent the two most basal extant lineages of winged insects, and determining their relationship with regard to Neoptera (remaining winged insects) is a critical step toward understanding insect diversification. A recent molecular analysis concluded that Paleoptera (Odonata Ephemeroptera) is monophyletic. However, we demonstrate that this result is supported only under a narrow range of alignment parameters. We have further tested the monophyly of Paleoptera using additional sequence data from 18SrDNA, 28S rDNA, and Histone 3 for a broader selection of taxa and a wider range of analytical methodologies. Our results suggest that the current suite of molecular data ambiguously resolve the three basal winged insect lineages and do not provide independent confirmation of Odonata + Neoptera as supported via morphological data. [source] A new evaluation technique for the detection of impurities in purified proteins via CE with native UV-LIFELECTROPHORESIS, Issue 2 2010Audrey Rodat Abstract An analytical methodology for quality control analyses of IgG and their impurities is presented using a new UV-LIF (266,nm) detector inside the cassette of a CE instrument and its performance was evaluated. The observed sensitivity was very close to that obtained by silver staining of slab gels (LOD of 25,ng/mL), while the sensitivity of the analysis is 80 times better than with CE/UV absorption (214,nm). Examples of the analysis of pharmaceutical and other commercial IgGs are provided and the kinetics of the reduction of IgG by ,-mercaptoethanol is reported, demonstrating the ease of performing the analysis. [source] Impact of changes in analytical techniques for the measurement of polychlorinated biphenyls and organochlorine pesticides on temporal trends in herring gull eggsENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 7 2010Shane R. de Solla Abstract Changes in analytical approaches during the tenure of monitoring programs for organochlorine (OC) pesticides and polychlorinated biphenyls (PCBs) may affect estimates of temporal trends. We used an in-house reference material to create multiplication factors to adjust the estimates of OC pesticides and PCBs (Aroclor equivalents) in Great Lake herring gull eggs analyzed using electron capture detection (1987,1997) to be more equivalent to estimates using mass spectrometric detection (1998,2005) as well as accompanying differences in analytical procedures. We examined temporal trends in contaminant concentrations in herring gull eggs using change point regressions, to determine whether significant changes in long-term trends were associated with analytical methodology. The highest frequency of change point occurrences shifted from 1997 (when analytical methodology was altered) to 2003 after data adjustment. The explanatory power (r2) of the regressions was lower after adjustment, although only marginally so (mean r2 difference,=,0.04). The initial rates of decline before change points in contaminant concentrations were generally slower after the data adjustment, but after any change points the declines were not significantly different. The regression models did not change for 83.3% of the cases. The effects on the interpretation of long-term temporal trends in herring gull eggs, although not negligible, were minor relative to the magnitude of the temporal changes. Environ. Toxicol. Chem. 2010;29:1476,1483. © 2010 SETAC [source] Emissions of greenhouse gases attributable to the activities of the land transport: modelling and analysis using I-CIR stochastic diffusion,the case of SpainENVIRONMETRICS, Issue 2 2008R. Gutiérrez Abstract In this study, carried out on the basis of the conclusions and methodological recommendations of the Fourth Assessment Report (2007) of the International Panel on Climate Change (IPCC), we consider the emissions of greenhouse gases (GHG), and particularly those of CO2, attributable to the activities of land transport, for all sectors of the economy, as these constitute a significant proportion of total GHG emissions. In particular, the case of Spain is an example of a worrying situation in this respect, both in itself and in the context of the European Union. To analyse the evolution, in this case, of such emissions, to enable medium-term forecasts to be made and to obtain a model that will enable us to analyse the effects of possible corrector mechanisms, we have statistically fitted a inverse Cox-Ingersoll-Ross (I-CIR) type nonlinear stochastic diffusion process, on the basis of the real data measured for the period 1990,2004, during which the Kyoto protocol has been applicable. We have studied the evolution of the trend of these emissions using estimated trend functions, for which purpose probabilistic complements such as trend functions and stationary distribution are incorporated, and a statistical methodology (estimation and asymptotic inference) for this diffusion, these tools being necessary for the application of the analytical methodology proposed. Copyright © 2007 John Wiley & Sons, Ltd. [source] Elemental Analysis of Human Cremains Using ICP-OES to Classify Legitimate and Contaminated Cremains,JOURNAL OF FORENSIC SCIENCES, Issue 5 2006Timothy R. Brooks ABSTRACT: The Tri-State Crematory Incident in Nobel, GA (February 2001) revealed limitations in traditional human cremated remains (cremains) analytical methodology. The goal of this study was to develop a method for effectively classifying questionable sets of cremains as legitimate or contaminated. Eighty-eight samples of known human cremains, concrete, mixtures of the two, and questionable sets of cremains were acid digested and analyzed for 21 elements by Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). Variable cluster and principle component analyses identified the seven elements (Sb, B, Li, Mn, Sr, Tl, and V) used to develop discriminant functions to classify questionable sets into two groups: cremains and concrete. The discriminant analysis shows that at the 0.90 probability level, mixtures of 50% or less human content were classified as concrete. Mixtures with 90% human content classified as cremains. Sixty percent and 75% human content mixtures remained in the questionable classification, but as the concentration of human increased in the mixture, the probability of assignment to the known cremains group increased. Most of the questionable human samples classified as cremains. This is a pilot study and cannot yet satisfy Daubert standards for courtroom admissibility, but it indicates that it is possible to determine the legitimacy of cremains using elemental analysis by ICP-OES coupled with multivariate statistical analysis. [source] Solid,liquid equilibrium of substrates and products of the enzymatic synthesis of ampicillinAICHE JOURNAL, Issue 6 2010Mônica Santana Abstract The solid,liquid equilibrium of precursors and products of the enzymatic synthesis of ampicillin (AMP) [6-aminopencillanic acid (6-APA) and D(,)phenylglycine (PG)] was investigated at different temperatures (283,298 K) and pHs (5.5,7.5). Solubility data were obtained using an analytical methodology. Equilibrium dissociation constants were experimentally measured at several temperatures for AMP, 6-APA, PG, and D(,)phenylglycine methyl ester. A model based on the simplified perturbed hard sphere theory proposed by Khoshkbarchi and Vera (Ind Eng Chem Res. 1996;35:4319-4327) was fitted against solubility data. The model could describe the water solubility behavior for AMP and PG as function of pH and temperature, but a bias was observed when fitting the model to the solubility of 6-APA. © 2009 American Institute of Chemical Engineers AIChE J, 2010 [source] Investigating the presence of pesticide transformation products in water by using liquid chromatography-mass spectrometry with different mass analyzers,JOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 2 2008Félix Hernández Abstract Many pesticide transformation products (TPs) can reach environmental waters as a consequence of their normally having a higher polarity than their parent pesticides. This makes the development of analytical methodology for reliable identification and subsequent quantification at the sub-microgram per liter levels necessary, as required under current legislation. In this paper we report the photodegradation of several pesticides frequently detected in environmental waters from the Spanish Mediterranean region using the high-resolution and exact-mass capabilities of hybrid quadrupole time-of-flight mass spectrometry (QTOF MS) hyphenated to liquid chromatography (LC). Once the main photodegradation/hydrolysis products formed in aqueous media were identified, analytical methodology for their simultaneous quantification and reliable identification in real water samples was developed using on-line solid-phase extraction (SPE)-LC-tandem MS with a triple-quadrupole (QqQ) analyzer. The methodology was validated in both ground and surface water samples spiked at the limit of quantification (LOQ) and 10 × LOQ levels, i.e. 50 and 500 ng/l, obtaining satisfactory recoveries and precision for all compounds. Subsequent analysis of ground and surface water samples resulted in the detection of a number of TPs higher than parent pesticides. Additionally, several soil-interstitial water samples collected from the unsaturated zone were analyzed to explore the degradation/transformation of some pesticides in the field using experimental plots equipped with lisimeters. Several TPs were found in these samples, with most of them having also been detected in ground and surface water from the same area. This paper illustrates the extraordinary potential of LC-MS(/MS) with QTOF and QqQ analyzers for qualitative/structural and quantitative analysis, respectively, offering analytical chemists one of the most powerful tools available at present to investigate the presence of pesticide TPs in water. Copyright © 2007 John Wiley & Sons, Ltd. [source] On the electrostatic equilibrium of granular flow in pneumatic conveying systemsAICHE JOURNAL, Issue 11 2006Jun Yao Abstract An analytical methodology involving the concept of "electrostatic equilibrium" is developed for granular flow in pneumatic conveying systems. The methodology can be used for estimation of the electrostatic field distribution at various sections of the system and explanation of the mechanisms involved for various electrostatic phenomena observed. For all cases conducted in the conveying system, there was a "charging time" required for the system to reach the state of "electrostatic equilibrium." Experiments conducted at different sections of the system showed that the time required increased in the order: horizontal pipe, vertical pipe, and pipe bend. Through a physical analysis, it is deduced that electrostatic equilibrium is related to the granules' behavior and local flow characteristics. In general, a longer time duration taken to reach equilibrium corresponds to a process with more complicated granular flow patterns. In the electrostatic equilibrium state, the field distribution shows the highest electrostatic field strength near the pipe wall, and this field strength degrades from the pipe wall to the pipe center. At various pipe sections, the highest strength occurs at the bend, in accord with observations that electric sparking first occurs at that location within the entire pneumatic conveying system. In the vertical pipe, granular distribution was measured using electrical capacitance tomography (ECT), and granular velocities were cross-referenced with those using particle image velocimetry (PIV). The electrostatic force at low air flow rates is found to be the primary cause for granules sticking to the pipe wall and results in the formation of the half-ring or ring structure. The state of electrostatic equilibrium is physically influenced by several elements in conveying systems. In a cyclic conveying system, a new pipe (or low humidity or no antistatic agent) tends to expedite the process to reach electrostatic equilibrium and attain high magnitude of electrostatic current at the state. In a non-cyclic horizontal conveying system, a thin film (pipe) is found to prolong the process duration to reach equilibrium, while the case with charged film (pipe) takes shorter duration to do so. © 2006 American Institute of Chemical Engineers AIChE J, 2006 [source] A liquid chromatographic method optimization for the assessment of low and high molar mass carbonyl compounds in winesJOURNAL OF SEPARATION SCIENCE, JSS, Issue 20 2009Luciana C. de Azevedo Abstract Carbonyl compounds (CC) play an important role in beverage aroma since they may affect flavor of wines, brandies, and beers, among others. For this reason, it is necessary to identify and quantify CC through adequate analytical techniques. This study is a proposal of both developing and optimization of a new analytical methodology that allows investigate C1,C8 CC in wines simultaneously by quantifying even those ones that are predominantly present in the adduct form hydroxylalkylsulfonic acids (HASA). The HASA dissociation is undertaken by specific alkaline media (pH 11). The developed methodology employed the LC with UV/VIS detection (, = 365 nm) technique under gradient elution in the way to reach both free-CC and bound-CC quantification. Results showed that binary gradient system using eluent A (MeOH/ACN/H2O 74.5:0.5:25% v/v/v) and eluent B (MeOH) reached the best separation condition of both lower and higher molecular mass CC. This proposed method allowed simultaneous quantification of formaldehyde, acetaldehyde, propanone, furfuraldehyde, butyraldehyde, benzaldehyde, hexanaldehyde, 2-ethyl-hexanaldehyde, E-pent-2-en-1-al, and cyclohexanone , all of them were found in white wine (Moscato Canelli) and red wine (Shiraz) produced in the São Francisco Valley, in the Northeastern Region of Brazil , although this optimized method may probably be suitable for quantification of propionaldehyde, isobutyraldehyde, heptanaldehyde, octanaldehyde, benzaldehyde, and E-hex-2-en-1-al as well. We could not prove if this method is also able to determine the latter CC group since we have not found these substances present in detectable levels in our real samples considered in this study. [source] Applying Human Systems Integration to the Rapid Acquisition ProcessNAVAL ENGINEERS JOURNAL, Issue 1 2007DEMETRIUS D. MACK The rapidly changing complexity of the Global War on Terrorism has changed the approach to equipping forward-deployed military forces. Combatant Commanders conducting operations now require timely materiel solutions to enhance mission capabilities and reduce the risk for individual soldiers. To address this challenge, the US Army established the Rapid Equipping Force to assess emerging requirements, to propose solutions to those requirements, and to implement those solutions in an expedient time frame. Unfortunately, the REF lacks a consistent analytical methodology for assessing alternative materiel solutions. To address the need for a human systems integration (HSI) analysis method, the authors developed an Assessment-Based Rapid Acquisition HSI Analysis Method (ABRAHAM) capable of generating tailored surveys and evaluating these surveys for unacceptable risks to soldiers. To validate ABRAHAM's concept and content, ABRAHAM was showcased in three Department of Defense settings: the Human Factors Engineering Technical Advisory Group, the REF, and the US Marine Corps' Operational Test and Evaluation Activity. The ABRAHAM appears to fill a gap in the current library of HSI tools. Based on the feedback provided during the product showcases, there is sufficient interest and technological maturity to further develop ABRAHAM to serve both the traditional and rapid acquisition processes. [source] Analysis of carbohydrates and amino acids in vegetable waste waters by ion chromatographyPHYTOCHEMICAL ANALYSIS, Issue 2 2003Michele Arienzo Abstract High-performance anion exchange chromatography coupled with pulsed amperometric detection was used for the quantitative determination of total and free sugars in olive oil mill waste waters (OMWW). Automated amino acid ion chromatography was employed to analyse total and free amino acids in the same OMWW. Sugars were analysed in samples pre-purified by means of a three-step purification procedure involving: (i) methanol precipitation of OMWW; (ii) dialysis of the obtained solid and liquid fractions; and (iii) chromatographic purification on RP18 phase followed by Amberlite resin. The amino acids were determined directly in samples obtained from the first two steps performed for sugar analysis. The analysis carried out with the reported methodologies allowed the quantitative determination of total sugars and amino acids and the differentiation between their free and bound forms. The sugars determined were arabinose, fructose, galactose, glucose, rhamnose, xylose, galacturonic and glucuronic acids, and the amino acids were Asp, Glu, Thr, Ser, Pro, Gly, Ala, Val, Met, Ile, Leu, Tyr, Phe, Lys, His, Arg and Cys. Asn, Gln, and Trp were not detected. The technological, biotechnological and environmental advantages arising from this analytical methodology applied to OMWW are briefly discussed. Copyright © 2003 John Wiley & Sons, Ltd. [source] Towards harmonized approaches for mycotoxin analyses: an assessmentQUALITY ASSURANCE & SAFETY OF CROPS & FOOD, Issue 2 2009Anton J. Alldrick Abstract Mycotoxins (the poisonous metabolites of certain filamentous fungi) are potential contaminants of staple food commodities and, if uncontrolled, may present a significant public health hazard. In many jurisdictions, questions relating to mycotoxin contamination are addressed at both generic and specific levels by food-safety legislation. Key to the successful management of the mycotoxin question, both in terms of verifying food-safety measures by the agri-food businesses and ensuring compliance with statutory limits by enforcement agencies, is the use of reliable sampling and analytical methodology. Evidence from European Union Rapid Alert System for Food and Feed data suggest that harmonization of methodologies used to determine the mycotoxin content of foods would contribute to improved compliance at both regulatory and commercial levels. [source] High-performance liquid chromatography/mass spectrometric and proton nuclear magnetic resonance spectroscopic studies of the transacylation and hydrolysis of the acyl glucuronides of a series of phenylacetic acids in buffer and human plasmaRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 20 2010Elin S. Karlsson The use of high-performance liquid chromatography/mass spectrometry (HPLC/MS) and proton nuclear magnetic resonance (1H NMR) spectroscopy for the kinetic analysis of acyl glucuronide (AG) isomerisation and hydrolysis of the 1-,- O -acyl glucuronides (1-,- O -AG) of phenylacetic acid, (R)- and (S)-,-methylphenylacetic acid and ,,,-dimethylphenylacetic acid is described and compared. Each AG was incubated in both aqueous buffer, at pH 7.4, and control human plasma at 37°C. Aliquots of these incubations, taken throughout the reaction time-course, were analysed by HPLC/MS and 1H NMR spectroscopy. In buffer, transacylation reactions predominated, with relatively little hydrolysis to the free aglycone observed. In human plasma incubations the calculated rates of reaction were much faster than for buffer and, in contrast to the observations in buffer, hydrolysis to the free aglycone was a significant contributor to the overall reaction. A diagnostic analytical methodology based on differential mass spectrometric fragmentation of 1-, -O- AGs compared to the 2-, 3- and 4-positional isomers, which enables selective determination of the former, was confirmed and applied. These findings show that HPLC/MS offers a viable alternative to the more commonly used NMR spectroscopic approach for the determination of the transacylation and hydrolysis reactions of these AGs, with the major advantage of having the capability to do so in a complex biological matrix such as plasma. Copyright © 2010 John Wiley & Sons, Ltd. [source] Field-Flow Fractionation as Analytical Technique for the Characterization of Dry Yeast: Correlation with Wine Fermentation ActivityBIOTECHNOLOGY PROGRESS, Issue 6 2003Ramsés Sanz Important oenological properties of wine depend on the winemaking yeast used in the fermentation process. There is considerable controversy about the quality of yeast, and a simple and cheap analytical methodology for quality control of yeast is needed. Gravitational field flow fractionation (GFFF) was used to characterize several commercial active dry wine yeasts from Saccharomycescerevisiae and Saccharomyces bayanus and to assess the quality of the raw material before use. Laboratory-scale fermentations were performed using two different S. cerevisiae strains as inocula, and GFFF was used to follow the behavior of yeast cells during alcoholic fermentation. The viable/nonviable cell ratio was obtained by flow cytometry (FC) using propidium iodide as fluorescent dye. In each experiment, the amount of dry wine yeast to be used was calculated in order to provide the same quantity of viable cells. Kinetic studies of the fermentation process were performed controlling the density of the must, from 1.071 to 0.989 (20/20 density), and the total residual sugars, from 170 to 3 g/L. During the wine fermentation process, differences in the peak profiles obtained by GFFF between the two types of commercial yeasts that can be related with the unlike cell growth were observed. Moreover, the strains showed different fermentation kinetic profiles that could be correlated with the corresponding fractograms monitored by GFFF. These results allow optimism that sedimentation FFF techniques could be successfully used for quality assessment of the raw material and to predict yeast behavior during yeast-based bioprocesses such as wine production. [source] Through Neural Stimulation to Behavior Manipulation: A Novel Method for Analyzing Dynamical Cognitive ModelsCOGNITIVE SCIENCE - A MULTIDISCIPLINARY JOURNAL, Issue 3 2010Thomas Hope Abstract The dynamical systems' approach to cognition (Dynamicism) promises computational models that effectively embed cognitive processing within its more natural behavioral context. Dynamical cognitive models also pose difficult, analytical challenges, which motivate the development of new analytical methodology. We start by illustrating the challenge by applying two conventional analytical methods to a well-known Dynamicist model of categorical perception. We then introduce our own analysis, which works by analogy with neural stimulation methods, and which yields some novel insights into the way the model works. We then extend and apply the method to a second Dynamicist model, which captures the key psychophysical trends that emerge when humans and animals compare two numbers. The results of the analysis,which reveals units with tuning functions that are monotonically related to the magnitudes of the numbers that the agents must compare,offer a clear contribution to the contentious debate concerning the way number information is encoded in the brain. [source] | |||||||||||||||||||