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Analytical Conditions (analytical + condition)
Selected AbstractsQuantitation of talinolol and other ,-blockers by capillary electrophoresis for in vitro drug absorption studiesELECTROPHORESIS, Issue 15 2003Bilal Awadallah Abstract A capillary zone electrophoresis method is described for the enantioseparation of talinolol using heptakis(2,3-diacetyl-6-sulfo)-,-cyclodextrin (HDAS-,-CD) as a chiral selector. After liquid-liquid extraction of talinolol from physiological solution, electrokinetic injection was employed to improve the sensitivity. The use of a coated capillary was necessary to achieve stable and reproducible enantioseparations. A baseline separation of the talinolol enantiomers was achieved in less than 10 min using 100 mM phosphate solution as background electrolyte and pH 3.5, at the presence of 3.0 mM HDAS-,-CD and at 20°C. In addition, this analytical condition proved to be useful for the enantioseparation of a number of other ,-blocking agents such as alprenolol, atenolol, bisoprolol, celiprolol, metipranolol, oxprenolol, and sotalol. For determing talinolol, the method could be validated in terms of precision, accuracy and linearity, and was found to be suitable in determination of talinolol enantiomers in highly diluted samples obtained from in vitro experiments. [source] A unified model incorporating yield, burn-in, and reliabilityNAVAL RESEARCH LOGISTICS: AN INTERNATIONAL JOURNAL, Issue 5 2004Kyungmee O. Kim Abstract The correlated improvement in yield and reliability has been observed in the case studies on integrated circuits and electronic assemblies. This paper presents a model that incorporates yield and reliability with the addition of a burn-in step to explain their correlated improvement. The proposed model includes as special cases several yield and reliability models that have been previously published and thus provides a unifying framework. The model is used to derive a condition for which yield functions can be multiplied to obtain the overall yield. Yield and reliability are compared as a function of operation time, and an analytical condition for burn-in to be effective is also obtained. Finally, Poisson and negative binomial defects models are further considered to investigate how reliability is based on yield. © 2004 Wiley Periodicals, Inc. Naval Research Logistics, 2004. [source] A simple procedure to approximate slip displacement of freestanding rigid body subjected to earthquake motionsEARTHQUAKE ENGINEERING AND STRUCTURAL DYNAMICS, Issue 4 2007Tomoyo Taniguchi Abstract A simple calculation procedure for estimating absolute maximum slip displacement of a freestanding rigid body placed on the ground or floor of linear/nonlinear multi-storey building during an earthquake is developed. The proposed procedure uses the displacement induced by the horizontal sinusoidal acceleration to approximate the absolute maximum slip displacement, i.e. the basic slip displacement. The amplitude of this horizontal sinusoidal acceleration is identical to either the peak horizontal ground acceleration or peak horizontal floor response acceleration. Its period meets the predominant period of the horizontal acceleration employed. The effects of vertical acceleration are considered to reduce the friction force monotonously. The root mean square value of the vertical acceleration at the peak horizontal acceleration is used. A mathematical solution of the basic slip displacement is presented. Employing over one hundred accelerograms, the absolute maximum slip displacements are computed and compared with the corresponding basic slip displacements. Their discrepancies are modelled by the logarithmic normal distribution regardless of the analytical conditions. The modification factor to the basic slip displacement is quantified based on the probability of the non-exceedence of a certain threshold. Therefore, the product of the modification factor and the basic slip displacement gives the design slip displacement of the body as the maximum expected value. Since the place of the body and linear/nonlinear state of building make the modification factor slightly vary, ensuring it to suit the problem is essential to secure prediction accuracy. Copyright © 2006 John Wiley & Sons, Ltd. [source] Simultaneous Determination of Nickel and Cadmium by Adsorptive Stripping VoltammetryELECTROANALYSIS, Issue 12 2008B. Gholivand Abstract A sensitive and fast method for the simultaneous determination of trace amounts of nickel and cadmium in real samples has been described using differential pulse adsorptive stripping voltammetry (DPASV) by adsorptive accumulation of the N,N,-bis(salicylaldehydo)4-carboxyphenylenediamine (BSCPDA),complex on the hanging mercury drop electrode (HMDE). As supporting electrolyte 0.02,mol L,1 ammonia buffers containing ligand has been used. Optimal analytical conditions were found to be: BSCPDA concentration of 42,,M, pH,9.6 and adsorption potential at ,50,mV versus Ag/AgCl. With an accumulation time of 20,s, the peaks current are proportional to the concentration of nickel and cadmium over the 1,180, and 0.5,200,ng mL,1 with detection limits of 0.06 and 0.03,ng mL,1 respectively. The sensitivity of method for determination of nickel and cadmium were obtained 0.54 and 0.98,nA mL ng,1, respectively. The procedure was applied to simultaneous determination of nickel and cadmium in some real and synthetic artificial samples with satisfactory results. [source] Simple method for determination of five terpenoids from different parts of Tripterygium wilfordii and its preparations by HPLC coupled with evaporative light scattering detectionJOURNAL OF SEPARATION SCIENCE, JSS, Issue 9 2007Xiao-Ling Luo Abstract By optimizing the extraction, separation, and analytical conditions, a reliable and accurate high-performance liquid chromatography method coupled with evaporative light scattering detection (ELSD) was developed for simultaneous determination of five terpenoids, i. e., triptolide, tripchlorolide, demethylzelastral, wilforlide B, and wilforlide A, in root, stem, leaves, root bark, twig, and root without bark of Tripterygium wilfordii Hook. f and six of its herbal preparations. This approach would thus provide a more accurate and general method for evaluating the quality of the herb and its preparations. Separation of these five terpenoids was achieved on a ZORBAX Eclipse XDB-C8 column with gradient elution using water and acetonitrile as solvents, both containing 0.05% formic acid, at a temperature of 30°C and a flow rate of 0.8 mL/min. The drift tube temperature of ELSD was set at 100°C, and the nitrogen flow rate at 1.5 L/min. Good linear relationships were obtained with correlation coefficients for the analytes exceeding 0.992, and the LOD and LOQ were less than 0.149 ,g and 0.297 ,g on column, respectively. Intra-day and inter-day precision of the analytes were less than 1.25% and 5.97%, respectively, and the average recovery rates obtained were in the range of 95.9 ± 3.7% to 100.4 ± 5.0% for all terpenoids with RSDs below 4.99%. Quantitative analysis of the five terpenoids in different parts of Tripterygium wilfordii and its six preparations showed that the contents of the terpenoids varied significantly. The tender root contained higher concentrations of triptolide, tripchlorolide, demethylzelastral, and wilforlide B than any other part of the herb. Correspondingly, the root bark contained the greatest concentration of wilforlide A, and the stem and twig came in second and third. This suggested that we could infer whether the medicinal materials were absolute roots without bark or not from the comparative contents of these terpenoids in the tablets in view of the fact that only the roots without bark are the valid officinal part of the plant. This method and the quantitation results obtained can provide a scientific and general as well as simple and convenient approach for the product manufacturers to set up quality control standards and for informing the public about the quality and safety of the preparations. [source] Fast GC analysis with a 50 ,m ID column: theory, practical aspects, and application to a highly complex sampleJOURNAL OF SEPARATION SCIENCE, JSS, Issue 14 2004Luigi Mondello Abstract This research focuses on the minimization of GC analysis times through the use of a 5 m×0.05 mm ID×0.05 ,m (film thickness) column. Experimental minimum plate height (Hmin) and optimum linear velocity values were derived from standard compound applications, under various analytical conditions, and then related to classical chromatographic theory. Deviations from the latter are measured and discussed. Practical aspects linked to the use of such capillaries, such as column sample capacity and detector acquisition rates, are also considered. Furthermore, a fast, and what can be considered a very fast method, were applied to the separation of a fuel sample. Coefficients of variation of elution times and relative peak areas were calculated in the very fast application. All analytical results are compared with those obtained by conventional 0.25 mm ID column applications. [source] Critical assessment of the applicability of gas chromatography-combustion-isotope ratio mass spectrometry to determine amino sugar dynamics in soilRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 8 2009Charlotte Decock Amino sugars in soils have been used as markers of microbial necromass and to determine the relative contribution of bacterial and fungal residues to soil organic matter. However, little is known about the dynamics of amino sugars in soil. This is partly because of a lack of adequate techniques to determine ,turnover rates' of amino sugars in soil. We conducted an incubation experiment where 13C-labeled organic substrates of different quality were added to a sandy soil. The objectives were to evaluate the applicability of compound-specific stable isotope analysis via gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) for the determination of 13C amino sugars and to demonstrate amino sugar dynamics in soil. We found total analytical errors between 0.8 and 2.6, for the ,13C-values of the soil amino sugars as a result of the required ,13C-corrections for isotopic alterations due to derivatization, isotopic fractionation and analytical conditions. Furthermore, the ,13C-values of internal standards in samples determined via GC-C-IRMS deviated considerably from the ,13C-values of the pure compounds determined via elemental analyzer IRMS (with a variation of 9 to 10, between the first and third quartile among all samples). This questions the applicability of GC-C-IRMS for soil amino sugar analysis. Liquid chromatography-combustion-IRMS (LC-C-IRMS) might be a promising alternative since derivatization, one of the main sources of error when using GC-C-IRMS, is eliminated from the procedure. The high 13C-enrichment of the substrate allowed for the detection of very high 13C-labels in soil amino sugars after 1 week of incubation, while no significant differences in amino sugar concentrations over time and across treatments were observed. This suggests steady-state conditions upon substrate addition, i.e. amino sugar formation equalled amino sugar decomposition. Furthermore, higher quality substrates seemed to favor the production of fungal-derived amino sugars. Copyright © 2009 John Wiley & Sons, Ltd. [source] Inter-laboratory comparison of elemental analysis and gas chromatography/combustion/isotope ratio mass spectrometry.RAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 7 200915N measurements of selected compounds for the development of an isotopic Grob test An inter-laboratory exercise was carried out by a consortium of five European laboratories to establish a set of compounds, suitable for calibrating gas chromatography/combustion/isotope ratio mass spectrometry (GC-C-IRMS) devices, to be used as isotopic reference materials for hydrogen, carbon, nitrogen and oxygen stable isotope measurements. The set of compounds was chosen with the aim of developing a mixture of reference materials to be used in analytical protocols to check for food and beverage authentication. The exercise was organized in several steps to achieve the certification level: the first step consisted of the a priori selection of chemical compounds on the basis of the scientific literature and successive GC tests to set the analytical conditions for each single compound and the mixture. After elimination of the compounds that turned out to be unsuitable in a multi-compound mixture, some additional oxygen- and nitrogen-containing substances were added to complete the range of calibration isotopes. The results of ,13C determinations for the entire set of reference compounds have previously been published, while the ,D and ,18O determinations were unsuccessful and after statistical analysis of the data the results did not reach the level required for certification. In the present paper we present the results of an inter-laboratory exercise to identify and test the set of nitrogen-containing compounds present in the mixture developed for use as reference materials for the validation of GC-C-IRMS analyses in individual laboratories. Copyright © 2009 John Wiley & Sons, Ltd. [source] Classification of Static Behavior of a Class of Unstructured Models of Continuous BioprocessesBIOTECHNOLOGY PROGRESS, Issue 4 2001A. Ajbar The stability characteristics of a class of unstructured models of continuous bioreactors are analyzed using elementary concepts of singularity theory and continuation techniques. The class consists of models for which the non-biomass product formation rate is linearly proportional to the utilization rate of limiting substrate. The kinetics expressions of cell growth and product synthesis are allowed to assume general forms of substrate and product. Global analytical conditions are derived that allow the construction of a practical picture in the multidimensional parameter space delineating the different static behavior these models can predict, including unique steady states, coexistence of non-trivial steady states with wash-out conditions, and multistability resulting from hysteresis. These general results are applied to specific examples of bioprocesses and allow the study of the effect of kinetic and operating parameters on the stability characteristics of these models. [source] Variables influencing Platelet Function Analyzer-100TM closure times in healthy individualsBRITISH JOURNAL OF HAEMATOLOGY, Issue 5 2005Hannelore Haubelt Summary We investigated the relationship between platelet function analyzer (PFA-100TM) closure times (CT) and bleeding time (BT), platelet aggregation (PA) induced by ADP, arachidonic acid, and collagen, blood cell counts, and von Willebrand factor (VWF) in 120 well-characterised healthy individuals. Pre-analytical and analytical conditions were standardised comprehensively. In a substantial number of cases the differences between duplicate measurements exceeded 15%. The reference range (5th and 95th percentiles) for CT with the collagen/epinephrine (CEPI) and the collagen/ADP (CADP) cartridge was 93,223 s and 64,117 s respectively. Re-examination of 11 individuals with CEPI-CT above the 95th percentile revealed considerable batch-to-batch variation of CEPI-CT. Males had significantly longer CADP than females (P = 0·002). CEPI and CADP-CT measured pm were significantly longer than corresponding values determined am (P = 0·003 and P < 0·0001 respectively). Blood group O was associated with greater CEPI and CADP-CT and lower VWF levels compared with non-O blood groups (P = 0·008, P = 0·0003 and P < 0·0001 respectively). Linear regression analysis revealed association between CEPI-CT, CADP-CT and VWF (P < 0·0001), but no relationship was found between CT and BT or between CT and PA. We conclude that VWF plasma levels modulate PFA-100TM CT to a greater extent than platelet function. Establishment of reliable reference ranges and careful standardisation of pre-analytical and analytical conditions is a prerequisite for obtaining reliable PFA-100TM results. Duplicate measurements are necessary. [source] Development of a Method for the Quantification of the Molar Gold Concentration in Tumour Cells Exposed to Gold-Containing DrugsCHEMMEDCHEM, Issue 5 2007Ingo Ott Dr. Abstract The knowledge of the cellular molar concentration of a drug is an extremely important parameter for the discussion and interpretation of its efficacy and bioavailability. Concerning metal complexes, electrothermal atomic absorption spectroscopy (ETAAS) offers a valuable analytical tool. However, matrix effects often hamper proper quantification of the metal concentration in biological tissues. This paper describes the development of an ETAAS method for the quantification of the molar gold concentration in HT-29 colon carcinoma cells. ETAAS analytical conditions were optimised and a factor was developed which allows the calculation of the molar cellular gold concentration from the measured gold per cellular biomass value. The method was used to quantify the gold content in HT-29 cells after exposure to the gold drug auranofin. Results indicated a strong cellular uptake of auranofin (compared to other metal anticancer drugs), which significantly correlated with the antiproliferative effects triggered by this agent. [source] Interlaboratory reproducibility of a microsatellite-based typing assay for Aspergillus fumigatus through the use of allelic ladders: proof of conceptCLINICAL MICROBIOLOGY AND INFECTION, Issue 2 2009H. A. De Valk Abstract An interlaboratory study was performed with the aim of investigating the reproducibility of a multiplex microbial microsatellite-based typing assay for Aspergillus fumigatus in different settings using a variety of experimental and analytical conditions and with teams having variable prior microsatellite typing experience. In order to circumvent problems with exchange of sizing data, allelic ladders are introduced as a straightforward and universally applicable concept for standardization of such typing assays. Allelic ladders consist of mixtures of well-characterized reference fragments to act as reference points for the position in an electrophoretic trace of fragments with established repeat numbers. Five laboratories independently analysed six microsatellite markers in 18 samples that were provided either as DNA or as A. fumigatus conidia. Allelic data were reported as repeat numbers and as sizes in nucleotides. Without the use of allelic ladders, size differences of up to 6.7 nucleotides were observed, resulting in interpretation errors of up to two repeat units. Difficulties in interpretation were related to non-specific amplification products (which were resolved with explanation) and bleed-through of the different fluorescent labels. In contrast, after resolution of technical or interpretive problems, standardization of sizing data by using allelic ladders enabled all participants to produce identical typing data. The use of allelic ladders as a routine part of molecular typing using microsatellite markers provides robust results suitable for interlaboratory comparisons and for deposition in a global typing database. [source] | ||||||||||||||||