961 resultados para Complex sample analysis


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A capillary electrophoresis with electrochemical detection(CE-ED) method was developed for the quality analysis of herbal medicine products prepared from the same herb of Herba Sarcandrae: Fufang Caoshanhu tablets, Qingrexiaoyanning capsules, and Xuekang oral liquids. Under the optimal analysis conditions, the low detection limit[1.0x10(-7) mol/L(S/N=3)] and the wide linear range(1.0x10(-7)-1.0x10(-4) mol/L) were obtained for quality standard compound of isofraxidin. The precisions of the peak current and the migration time(as RSDs) for the real sample analysis were 2.0%-2.6%, and 1.2%-1.8% for isofraxidin, respectively.

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There is an urgent need for thorough analysis of Radix astragali, a widely used Chinese herb, for quality control purposes. This paper describes the development of a total analytical method for Radix astragali extract, a multi-component complex mixture. Twenty-four components were separated step by step from the extract using a series of isocratic isopropanol-methanol elutions, and then 42 components were separated similarly using methanol-water elutions. Based on the log k(w) and -S of the 66 components obtained from the above procedure and the optimization software developed in our laboratory, an optimum elution program consisting of seven methanol-water segments and four isopropanol-methanol segments was developed to finish the task of analyzing the total components in a single run. Under optimized gradient conditions, the sample of Radix astragali extract was analyzed. As expected, most of the components were well separated and the experimental chromatogram was in a good agreement with the predicted one.

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Urinary 8-hydroxydeoxyguanosine (80HdG) has been considered as an excellent marker of individuals at high risk of developing cancer. Until now, urinary 80HdG has largely been measured by high-performance liquid chromatography with electrochemical detection. A new method for the analysis of urinary 80HdG by high-performance capillary electrophoresis has been developed and optimized in our laboratory. A single step solid-phase extraction procedure was optimized and used for extracting 80HdG from human urine. Separations were performed in an uncoated silica capillary (50 cm x 50 tm i.d.) using a P/ACE MDQ system with UV detection. The separation of 80HdG from interfering urinary matrix components is optimized with regard to pH, applied voltage, pressure injection time and concentration of SDS in running buffer. The detection limit of this method is 0.4 mug/ml, the linear range is 0.8-500 mug/ml, the correlation coefficients levels is better than 0.999. The developed method is simple, fast and good reproducibility, furthermore, it requires a very small injection volumes and low costs of analysis, which makes it possible to provide a new noninvasive assay for an indirect measurement of oxidative DNA damage.

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The use of matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) for environmental analysis has been mainly focused on qualitative analysis of high-mass molecules, such as toxins, humic acid, and microorganisms. Herein,we describe a novel MALDI-TOF-MS method with a matrix of oxidized carbon nanotubes for analysis of low-mass compounds in environmental samples. A number of chemicals in the environment were qualitatively analyzed by the present method, and it was found that most of them, especially the highly polar chemicals, were measurable with high sensitivity. With the intrinsic ability to measure high-mass chemicals, this method can compensate for the current shortage of methods for environmental analysis for the measurement of highly polar or high-mass chemicals. For sample analysis, arsenic speciation in Chinese traditional medicines was qualified and diphenylolpropane in water samples was quantified. With the relatively high tolerance of the method to interfering molecules, a simple pretreatment or even no pretreatment could be employed before MS detection. Furthermore, this method can be employed in a high-throughput format.

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An approach for the separation and identification of components in a traditional Chinese medicine Psoralea corylifolia was developed. Ion-exchange chromatography (IEC) was applied for the fractionation of P corylifolia extract, and then followed by concentration of all the fractions with rotary vacuum evaporator. Each of the enriched fractions was then further separated on an ODS column with detection of UV absorbance and atmospheric pressure chemical ionization mass spectrometer (APCI/MS), respectively, and also analyzed by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF/MS) with matrix of oxidized carbon nanotubes. Totally more than 188 components in P. corylifolia extract were detected with this integrated approach, and 12 of them were preliminary identified according to their UV spectra and mass spectra performed by APCI/MS and MALDI-TOF/MS. The obtained analytical results not only demonstrated the powerful resolution of integration IEC fractionation with reversed-phase liquid chromatography (RPLC)-APCI/MS and MALDI-TOF/MS for analysis of compounds in a complex sample, but also exhibited the superiority of APCI/MS and MALDI-TOF/MS for identification of low-mass compounds, such as for study of traditional Chinese medicines (TCMs) and metabolome. (c) 2005 Published by Elsevier B.V.

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A rapid and sensitive immuno-based screening method was developed to detect domoic acid (DA) present in extracts of shellfish species using a surface plasmon resonance-based optical biosensor. A rabbit polyclonal antibody raised against DA was mixed with standard or sample extracts and allowed to interact with DA immobilized onto a sensor chip surface. The characterization of the antibody strongly suggested high cross-reactivity with DA and important isomers of the toxin. The binding of this antibody to the sensor chip surface was inhibited in the presence of DA in either standard solutions or sample extracts. The DA chip surface proved to be highly stable, achieving approximately 800 analyses per chip without any loss of surface activity. A single analytical cycle (sample injection, chip regeneration, and system wash) took 10 min to complete. Sample analysis (scallops, mussels, cockles, oysters) was achieved by simple extraction with methanol. These extracts were then filtered and diluted before analysis. Detection limits in the ng/g range were achieved by the assay; however, the assay parameters chosen allowed the test to be performed most accurately at the European Union's official action limit for DA of 20 mu g/g. At this concentration, intra- and interassay variations were measured for a range of shellfish species and ranged from 4.5 to 7.4% and 2.3 to 9.7%, respectively.

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Biosensors are used for a large number of applications within biotechnology, including the pharmaceutical industry and life sciences. Since the production of Biacore surface-plasmon resonance instruments in the early 1990s, there has been steadily growing use of this technology for the detection of food contaminants (e.g., veterinary drugs, mycotoxins, marine toxins, food dyes and processing contaminants). Other biosensing technologies (e.g., electrochemical and piezoelectric) have also been employed for the analysis of small-molecule contaminants. This review concentrates on recent advances made in detection and quantification of antimicrobial compounds with different types of biosensors and on the emergence of multiplexing, which is highly desirable as it increases sample analysis at lower cost and in less time. (C) 2010 Elsevier Ltd. All rights reserved.

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Requirements analysis focuses on stakeholders concerns and their influence towards e-government systems. Some characteristics of stakeholders concerns clearly show the complexity and conflicts. This imposes a number of questions in the requirements analysis, such as how are they relevant to stakeholders? What are their needs? How conflicts among the different stakeholders can be resolved? And what coherent requirements can be methodologically produced? This paper describes the problem articulation method in organizational semiotics which can be used to conduct such complex requirements analysis. The outcomes of the analysis enable e-government systems development and management to meet userspsila needs. A case study of Yantai Citizen Card is chosen to illustrate a process of analysing stakeholders in the lifecycle of requirements analysis.

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Mandibular prognathism typically shows familial aggregation. Various genetic models have been described and it is assumed to be a multifactorial and polygenic trait, with a threshold for expression. Our goal was to examine specific genetic models of the familial transmission of this trait. The study sample comprised of 2,562 individuals from 55 families. Complete family histories for each proband were ascertained and the affection status of relatives were confirmed by lateral cephalograms, photographs, and dental models. Pedigrees were drawn using PELICAN and complex segregation analysis was performed using POINTER. Parts of some pedigrees were excluded to create one founder pedigrees, so the total N was 2,050. Analysis showed more affected females than males (P = 0.030). The majority of the pedigrees suggest autosomal dominant inheritance. Incomplete penetrance was demonstrated by the ratio of affected/unaffected parents and siblings. The heritability of mandibular prognathism was estimated to be 0.316. We conclude that there is a major gene that influences the expression of mandibular prognathism with clear signs of Mendelian inheritance and a multifactorial component. (C) 2007 Wiley-Liss, Inc.

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Phelan (2000) has produced a complex bibliometric analysis of the international contribution of Australian educational research based upon publications and citations reported in the journals indexed by the Institute for Scientific Information - the Standards & Poors of the academic world. This paper examins Phelan's analysis, showing its strengths and weaknesses, as well as examining his proposal for the establishment of an Australian database along the lines of the ISI's index.

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The need to monitor biogenic amines levels is essential for many areas of the food industry for two main reasons: the caustic nature and potential toxicity of these amines, and the potential to use amine levels as markers for freshness and quality in foodstuffs. Optimised analysis conditions used for the determination of biogenic amines derivatised with 2-napthyloxycarbonyl chloride has been applied to different pet food samples to assess the effectiveness of this method for complex sample matrices. Further to this, the use of high-resolution mass spectrometry has enabled the previously unconfirmed derivatised form of seven biogenic amines to be established. The derivatised forms identified include as mono substituted (tryptamine and histamine), bisubstituted (putrescine, cadaverine and tyramine), trisubstituted (spermidine) and tetrasubstituted (spermine). The methodology of biogenic amine determination was performed successfully to a range of pet food products highlighting the applicability to a variety of complex sample matrices.

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A presente tese engloba três artigos sobre diferencial de salários e estimação de demanda no Brasil. O primeiro artigo investiga o diferencial de salários entre os trabalhadores dos setores público e privado. A principal contribuição deste estudo é a estimação de um modelo de regressão com mudança endógena (endogenous switching regression model), que corrige o viés de seleção no processo de escolha setorial realizada pelos trabalhadores e permite a identificação de fatores determinantes na entrada do trabalhador no mercado de trabalho do setor público. O objetivo do segundo trabalho é calcular a elasticidade-preço e a elasticidade-despesa de 25 produtos alimentares das famílias residentes nas áreas rurais e urbanas do Brasil. Para tanto, foram estimados dois sistemas de equações de demanda por alimentos, um referente às famílias residentes nas áreas rurais do país e o outro sistema associado às famílias residentes nas áreas urbanas. O terceiro artigo busca testar a validade do modelo unitário para solteiros(as) e a validade do modelo de racionalidade coletiva de Browning e Chiappori (1998) para casais no Brasil. Para tanto, foi estimado um sistema de demanda do consumo brasileiro com base no modelo QUAIDS, que apresenta uma estrutura de preferências flexível o suficiente para permitir curvas de Engel quadráticas.

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In this work, the objective in study was the development of a biossensor potencyometric for urea detection, starting from the extracted urease of soy grains. Initially, was made a chemometrics study, through a planning factorial 24, objectified to find great conditions for the extraction of the urease without its properties were affected. Starting from this study, the best conditions were determined for the obtaining of rich extracts in urease, allowing the biossensors making with good characteristics. These were made using a platinum electrode as transducer with the dispersed urease in chitosan head office and reticulated in glutaraldehyde vapor. The biossensors obtained presented a limit of urea detection the same to 0,33 mM and lineal strip between 0,33 and 3 mM of the substratum. The time of answer was considered loud, mainly, in low concentrations of the substratum, where it was taken about 5 minutes by analysis. For high concentrations that time was reduced for not more than one minute. The time of life was limited by the adherence of the enzymatic membrane to the transducer, but it was possible to maintain the biossensor with operation for one month with about 50 accomplished measures. Application of the biossensor for analyses of fertilizers to the urea base presented excellent result for a sample with few interfering, but it was different when the used fertilizer was originating from of a complex sample. Even so the label was not expressed the text of nitrogen it was totally coming of the urea. An evaluation of the kinetic parameters of the catalytic reaction of the biossensor showed coherence with the results exposed in the literature