Current trends and challenges in sample preparation for metallic nanoparticles analysis in daily products and environmental samples: A review

NASA Astrophysics Data System (ADS)

De la Calle, Inmaculada; Menta, Mathieu; Séby, Fabienne

2016-11-01

Due to the increasing use of nanoparticles (NPs) in consumer products, it becomes necessary to develop different strategies for their detection, identification, characterization and quantification in a wide variety of samples. Since the analysis of NPs in consumer products and environmental samples is particularly troublesome, a detailed description of challenges and limitations is given here. This review mainly focuses on sample preparation procedures applied for the mostly used techniques for metallic and metal oxide NPs characterization in consumer products and most outstanding publications of biological and environmental samples (from 2006 to 2015). We summarize the procedures applied for total metal content, extraction/separation and/or preconcentration of NPs from the matrix, separation of metallic NPs from their ions or from larger particles and NPs' size fractionation. Sample preparation procedures specifically for microscopy are also described. Selected applications in cosmetics, food, other consumer products, biological tissues and environmental samples are presented. Advantages and inconveniences of those procedures are considered. Moreover, selected simplified schemes for NPs sample preparation, as well as usual techniques applied are included. Finally, promising directions for further investigations are discussed.

Semiautomated Device for Batch Extraction of Metabolites from Tissue Samples

PubMed Central

2012-01-01

Metabolomics has become a mainstream analytical strategy for investigating metabolism. The quality of data derived from these studies is proportional to the consistency of the sample preparation. Although considerable research has been devoted to finding optimal extraction protocols, most of the established methods require extensive sample handling. Manual sample preparation can be highly effective in the hands of skilled technicians, but an automated tool for purifying metabolites from complex biological tissues would be of obvious utility to the field. Here, we introduce the semiautomated metabolite batch extraction device (SAMBED), a new tool designed to simplify metabolomics sample preparation. We discuss SAMBED’s design and show that SAMBED-based extractions are of comparable quality to extracts produced through traditional methods (13% mean coefficient of variation from SAMBED versus 16% from manual extractions). Moreover, we show that aqueous SAMBED-based methods can be completed in less than a quarter of the time required for manual extractions. PMID:22292466

Variable Memory Strategy Use in Children's Adaptive Intratask Learning Behavior: Developmental Changes and Working Memory Influences in Free Recall

ERIC Educational Resources Information Center

Lehmann, Martin; Hasselhorn, Marcus

2007-01-01

Variability in strategy use within single trials in free recall was analyzed longitudinally from second to fourth grades (ages 8-10 years). To control for practice effects another sample of fourth graders was included (age 10 years). Video analyses revealed that children employed different strategies when preparing for free recall. A gradual shift…

Nursing faculty preparedness for clinical teaching.

PubMed

Suplee, Patricia Dunphy; Gardner, Marcia; Jerome-D'Emilia, Bonnie

2014-03-01

Nursing faculty who teach in clinical settings face complex situations requiring evidence-based educational and evaluative strategies, yet many have had limited preparation for these tasks. A convenience sample of 74 nursing faculty participated in a survey about clinical teaching in prelicensure nursing programs. Most faculty developed teaching skills through conferences (57%), orientation at their educational institution (53%), or exposure in graduate school (38%). Thirty-one percent reported having no preparation for clinical teaching. Faculty felt least prepared to manage students with learning, physical, or emotional disabilities and incivility. Twenty-six percent had no preparation for evaluating students in the clinical setting, and only 17% had worked with a faculty mentor. Few evidence-based teaching strategies were used by the faculty. These findings indicate gaps exist in the preparation of clinical faculty. Graduate education, comprehensive orientation programs, and continuing professional development may help to ensure faculty are effective in managing and evaluating student learning. Copyright 2014, SLACK Incorporated.

Adaptive Insecure Attachment and Resource Control Strategies during Middle Childhood

ERIC Educational Resources Information Center

Chen, Bin-Bin; Chang, Lei

2012-01-01

By integrating the life history theory of attachment with resource control theory, the current study examines the hypothesis that insecure attachment styles reorganized in middle childhood are alternative adaptive strategies used to prepare for upcoming competition with the peer group. A sample of 654 children in the second through seventh grades…

Mesoporous structured MIPs@CDs fluorescence sensor for highly sensitive detection of TNT.

PubMed

Xu, Shoufang; Lu, Hongzhi

2016-11-15

A facile strategy was developed to prepare mesoporous structured molecularly imprinted polymers capped carbon dots (M-MIPs@CDs) fluorescence sensor for highly sensitive and selective determination of TNT. The strategy using amino-CDs directly as "functional monomer" for imprinting simplify the imprinting process and provide well recognition sites accessibility. The as-prepared M-MIPs@CDs sensor, using periodic mesoporous silica as imprinting matrix, and amino-CDs directly as "functional monomer", exhibited excellent selectivity and sensitivity toward TNT with detection limit of 17nM. The recycling process was sustainable for 10 times without obvious efficiency decrease. The feasibility of the developed method in real samples was successfully evaluated through the analysis of TNT in soil and water samples with satisfactory recoveries of 88.6-95.7%. The method proposed in this work was proved to be a convenient and practical way to prepare high sensitive and selective fluorescence MIPs@CDs sensors. Copyright © 2016 Elsevier B.V. All rights reserved.

Study of sample preparation for quantitative analysis of amino acids in human sweat by liquid chromatography-tandem mass spectrometry.

PubMed

Delgado-Povedano, M M; Calderón-Santiago, M; Priego-Capote, F; Luque de Castro, M D

2016-01-01

The determination of physiological levels of amino acids is important to aid in the diagnosis and treatment of several diseases and nutritional status of individuals. Amino acids are frequently determined in biofluids such as blood (serum or plasma) and urine; however, there are less common biofluids with different concentration profiles of amino acids that could be of interest. One of these biofluids is sweat that can be obtained in a non-invasive manner and is characterized by low complex composition. The analysis of amino acids in human sweat requires the development of sample preparation strategies according to the sample matrix and small collected volume. The influence of sample preparation on the quantitative analysis of amino acids in sweat by LC-MS/MS has been assessed through a comparison between two strategies: dilution of sweat and centrifugal microsolid-phase extraction (c-μSPE). In both cases, several dilution factors were assayed for in-depth knowledge of the matrix effects, and the use of c-μSPE provided the best results in terms of accuracy. The behavior of the target analytes was a function of the dilution factor, thus providing a pattern for sample preparation that depended on the amino acid to be determined. The concentration of amino acids in sweat ranges between 6.20 ng mL(-1) (for homocysteine) and 259.77 µg mL(-1) (for serine) with precision, expressed as relative standard deviation, within 1.1-21.4%. Copyright © 2015 Elsevier B.V. All rights reserved.

Transportation Demand Management Planning At Multi-Tenant Buildings, An Example Of Tdm Planning During Project

DOT National Transportation Integrated Search

1988-09-01

THIS GUIDE FOR DEVELOPERS, BUILDING OWNERS AND BUILDING MANAGERS IS ONE IN A SERIES OF SAMPLES OF TDM PLANS THAT ILLUSTRATE THE DESIGN AND PROPOSED APPLICATION OF TDM STRATEGIES. THIS SAMPLE PLAN WAS PREPARED FOR A FICTITIOUS BUILDING MANAGER NEAR DO...

Work conditions and the food choice coping strategies of employed parents.

PubMed

Devine, Carol M; Farrell, Tracy J; Blake, Christine E; Jastran, Margaret; Wethington, Elaine; Bisogni, Carole A

2009-01-01

How work conditions relate to parents' food choice coping strategies. Pilot telephone survey. City in the northeastern United States (US). Black, white, and Hispanic employed mothers (25) and fathers (25) randomly recruited from low-/moderate-income zip codes; 78% of those reached and eligible participated. Sociodemographic characteristics; work conditions (hours, shift, job schedule, security, satisfaction, food access); food choice coping strategies (22 behavioral items for managing food in response to work and family demands (ie, food prepared at/away from home, missing meals, individualizing meals, speeding up, planning). Two-tailed chi-square and Fisher exact tests (P < or = .05, unless noted). Half or more of respondents often/sometimes used 12 of 22 food choice coping strategies. Long hours and nonstandard hours and schedules were positively associated among fathers with take-out meals, missed family meals, prepared entrees, and eating while working; and among mothers with restaurant meals, missed breakfast, and prepared entrees. Job security, satisfaction, and food access were also associated with gender-specific strategies. Structural work conditions among parents such as job hours, schedule, satisfaction, and food access are associated with food choice coping strategies with importance for dietary quality. Findings have implications for worksite interventions but need examination in a larger sample.

Quantitative Ultrasound-Assisted Extraction for Trace-Metal Determination: An Experiment for Analytical Chemistry

ERIC Educational Resources Information Center

Lavilla, Isela; Costas, Marta; Pena-Pereira, Francisco; Gil, Sandra; Bendicho, Carlos

2011-01-01

Ultrasound-assisted extraction (UAE) is introduced to upper-level analytical chemistry students as a simple strategy focused on sample preparation for trace-metal determination in biological tissues. Nickel extraction in seafood samples and quantification by electrothermal atomic absorption spectrometry (ETAAS) are carried out by a team of four…

Magnetic nanoparticles: preparation, physical properties, and applications in biomedicine

PubMed Central

2012-01-01

Finally, we have addressed some relevant findings on the importance of having well-defined synthetic strategies developed for the generation of MNPs, with a focus on particle formation mechanism and recent modifications made on the preparation of monodisperse samples of relatively large quantities not only with similar physical features, but also with similar crystallochemical characteristics. Then, different methodologies for the functionalization of the prepared MNPs together with the characterization techniques are explained. Theorical views on the magnetism of nanoparticles are considered. PMID:22348683

Review of sample preparation strategies for MS-based metabolomic studies in industrial biotechnology.

PubMed

Causon, Tim J; Hann, Stephan

2016-09-28

Fermentation and cell culture biotechnology in the form of so-called "cell factories" now play an increasingly significant role in production of both large (e.g. proteins, biopharmaceuticals) and small organic molecules for a wide variety of applications. However, associated metabolic engineering optimisation processes relying on genetic modification of organisms used in cell factories, or alteration of production conditions remain a challenging undertaking for improving the final yield and quality of cell factory products. In addition to genomic, transcriptomic and proteomic workflows, analytical metabolomics continues to play a critical role in studying detailed aspects of critical pathways (e.g. via targeted quantification of metabolites), identification of biosynthetic intermediates, and also for phenotype differentiation and the elucidation of previously unknown pathways (e.g. via non-targeted strategies). However, the diversity of primary and secondary metabolites and the broad concentration ranges encompassed during typical biotechnological processes means that simultaneous extraction and robust analytical determination of all parts of interest of the metabolome is effectively impossible. As the integration of metabolome data with transcriptome and proteome data is an essential goal of both targeted and non-targeted methods addressing production optimisation goals, additional sample preparation steps beyond necessary sampling, quenching and extraction protocols including clean-up, analyte enrichment, and derivatisation are important considerations for some classes of metabolites, especially those present in low concentrations or exhibiting poor stability. This contribution critically assesses the potential of current sample preparation strategies applied in metabolomic studies of industrially-relevant cell factory organisms using mass spectrometry-based platforms primarily coupled to liquid-phase sample introduction (i.e. flow injection, liquid chromatography, or capillary electrophoresis). Particular focus is placed on the selectivity and degree of enrichment attainable, as well as demands of speed, absolute quantification, robustness and, ultimately, consideration of fully-integrated bioanalytical solutions to optimise sample handling and throughput. Copyright © 2016 Elsevier B.V. All rights reserved.

Understanding Procurement for Sampling and Analytical Services Under a Triad Approach

EPA Pesticide Factsheets

The EPA Brownfields and Land Revitalization Technology Support Center (BTSC) has prepared this document to highlight methods and strategies that have been successfully used to procure services under a Triad framework.

Senior Leaders' Views on Leadership Preparation and Succession Strategies in New Zealand: Time for a Career-Related Professionalization Policy and Provisions

ERIC Educational Resources Information Center

Macpherson, Reynold

2014-01-01

This research note reports the views of members of a branch of a professional association about their career paths and the appropriateness of preparatory and succession strategies for leaders in New Zealand schools. This sample of 12 "seniors" was unusual for its relative professional seniority, span of responsibilities and postgraduate…

Crystallization of PTP Domains.

PubMed

Levy, Colin; Adams, James; Tabernero, Lydia

2016-01-01

Protein crystallography is the most powerful method to obtain atomic resolution information on the three-dimensional structure of proteins. An essential step towards determining the crystallographic structure of a protein is to produce good quality crystals from a concentrated sample of purified protein. These crystals are then used to obtain X-ray diffraction data necessary to determine the 3D structure by direct phasing or molecular replacement if the model of a homologous protein is available. Here, we describe the main approaches and techniques to obtain suitable crystals for X-ray diffraction. We include tools and guidance on how to evaluate and design the protein construct, how to prepare Se-methionine derivatized protein, how to assess the stability and quality of the sample, and how to crystallize and prepare crystals for diffraction experiments. While general strategies for protein crystallization are summarized, specific examples of the application of these strategies to the crystallization of PTP domains are discussed.

Sampling designs for contaminant temporal trend analyses using sedentary species exemplified by the snails Bellamya aeruginosa and Viviparus viviparus.

PubMed

Yin, Ge; Danielsson, Sara; Dahlberg, Anna-Karin; Zhou, Yihui; Qiu, Yanling; Nyberg, Elisabeth; Bignert, Anders

2017-10-01

Environmental monitoring typically assumes samples and sampling activities to be representative of the population being studied. Given a limited budget, an appropriate sampling strategy is essential to support detecting temporal trends of contaminants. In the present study, based on real chemical analysis data on polybrominated diphenyl ethers in snails collected from five subsites in Tianmu Lake, computer simulation is performed to evaluate three sampling strategies by the estimation of required sample size, to reach a detection of an annual change of 5% with a statistical power of 80% and 90% with a significant level of 5%. The results showed that sampling from an arbitrarily selected sampling spot is the worst strategy, requiring much more individual analyses to achieve the above mentioned criteria compared with the other two approaches. A fixed sampling site requires the lowest sample size but may not be representative for the intended study object e.g. a lake and is also sensitive to changes of that particular sampling site. In contrast, sampling at multiple sites along the shore each year, and using pooled samples when the cost to collect and prepare individual specimens are much lower than the cost for chemical analysis, would be the most robust and cost efficient strategy in the long run. Using statistical power as criterion, the results demonstrated quantitatively the consequences of various sampling strategies, and could guide users with respect of required sample sizes depending on sampling design for long term monitoring programs. Copyright © 2017 Elsevier Ltd. All rights reserved.

Results and analysis of saltstone cores taken from saltstone disposal unit cell 2A

DOE Office of Scientific and Technical Information (OSTI.GOV)

Reigel, M. M.; Hill, K. A.

2016-03-01

As part of an ongoing Performance Assessment (PA) Maintenance Plan, Savannah River Remediation (SRR) has developed a sampling and analyses strategy to facilitate the comparison of field-emplaced samples (i.e., saltstone placed and cured in a Saltstone Disposal Unit (SDU)) with samples prepared and cured in the laboratory. The primary objectives of the Sampling and Analyses Plan (SAP) are; (1) to demonstrate a correlation between the measured properties of laboratory-prepared, simulant samples (termed Sample Set 3), and the field-emplaced saltstone samples (termed Sample Set 9), and (2) to validate property values assumed for the Saltstone Disposal Facility (SDF) PA modeling. Themore » analysis and property data for Sample Set 9 (i.e. six core samples extracted from SDU Cell 2A (SDU2A)) are documented in this report, and where applicable, the results are compared to the results for Sample Set 3. Relevant properties to demonstrate the aforementioned objectives include bulk density, porosity, saturated hydraulic conductivity (SHC), and radionuclide leaching behavior.« less

Comparison of Dilution, Filtration, and Microwave Digestion Sample Pretreatments in Elemental Profiling of Wine by ICP-MS.

PubMed

Godshaw, Joshua; Hopfer, Helene; Nelson, Jenny; Ebeler, Susan E

2017-09-25

Wine elemental composition varies by cultivar, geographic origin, viticultural and enological practices, and is often used for authenticity validation. Elemental analysis of wine by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is challenging due to the potential for non-spectral interferences and plasma instability arising from organic matrix components. Sample preparation mitigates these interferences, however, conflicting recommendations of best practices in ICP-MS analysis of wine have been reported. This study compared direct dilution, microwave-assisted acid digestion, and two filtration sample pretreatments, acidification prior to filtration and filtration followed by acidification, in elemental profiling of one white and three red table wines by ICP-MS. Of 43 monitored isotopes, 37 varied by sample preparation method, with significantly higher results of 17 isotopes in the microwave-digested samples. Both filtration treatments resulted in lower results for 11 isotopes compared to the other methods. Finally, isotope dilution determination of copper based on natural abundances and the 63 Cu: 65 Cu instrument response ratio agreed with external calibration and confirmed a significant sample preparation effect. Overall, microwave digestion did not compare favorably, and direct dilution was found to provide the best compromise between ease of use and result accuracy and precision, although all preparation strategies were able to differentiate the wines.

Determination of trace metals in spirits by total reflection X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Siviero, G.; Cinosi, A.; Monticelli, D.; Seralessandri, L.

2018-06-01

Eight spirituous samples were analyzed for trace metal content with Horizon Total Reflection X-Ray Fluorescence (TXRF) Spectrometer. The expected single metal amount is at the ng/g level in a mixed aqueous/organic matrix, thus requiring a sample preparation method capable of achieving suitable limits of detection. On-site enrichment and Atmospheric Pressure-Vapor Phase Decomposition allowed to detect Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Sr and Pb with detection limits ranging from 0.1 ng/g to 4.6 ng/g. These results highlight how the synergy between instrument and sample preparation strategy may foster the use of TXRF as a fast and reliable technique for the determination of trace elements in spirituous samples, either for quality control or risk assessment purposes.

Sludge batch 9 (SB9) acceptance evaluation. Radionuclide concentrations in tank 51 SB9 qualification sample prepared at SRNL

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C. J.; Diprete, D. P.; Pareizs, J. M.

Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tankmore » 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a composition expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.« less

Sludge batch 9 (SB9) accepance evaluation: Radionuclide concentrations in tank 51 SB9 qualification sample prepared at SRNL

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C.; Diprete, D.; Pareizs, J.

Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tankmore » 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a compositioniv expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.« less

Academic achievement in first-year Portuguese college students: the role of academic preparation and learning strategies.

PubMed

Soares, Ana Paula; Guisande, Adelina M; Almeida, Leandro S; Páramo, Fernanda M

2009-06-01

This paper analyses the role of academic preparation and learning strategies in the prediction of first-year Portuguese college students' academic achievement, considering students' sex and academic field attended. A sample of 445 first-year college students (68.5% female) from the University of Minho (25.8% enrolled in economics, 35.3% in science/technology, and 38.9% in humanities degrees) participated in the study. Students answered a questionnaire on learning strategies in the classroom at the end of the first semester, which consisted of 44 items organized in five dimensions: comprehensive approach, surface approach, personal competency perceptions, intrinsic motivation, and organization of study activities. Academic achievement (grade point average at the end of first year) and academic preparation (students' higher education access mark) were obtained through the academic records of the university. Results showed that academic preparation was the strongest predictor of first-year academic achievement, and only marginal additional variance was explained by learning strategies as assessed by the self-reported questionnaire. There were sex and academic field differences, but these variables do not seem strong enough to affect the results, although the different percentages of variance captured by each model and the different weights associated to higher education access mark, stimulate the use of these and/or other personal and contextual variables when analysing the phenomenon.

Quantitative evaluation of the CEEM soil sampling intercomparison.

PubMed

Wagner, G; Lischer, P; Theocharopoulos, S; Muntau, H; Desaules, A; Quevauviller, P

2001-01-08

The aim of the CEEM soil project was to compare and to test the soil sampling and sample preparation guidelines used in the member states of the European Union and Switzerland for investigations of background and large-scale contamination of soils, soil monitoring and environmental risk assessments. The results of the comparative evaluation of the sampling guidelines demonstrated that, in soil contamination studies carried out with different sampling strategies and methods, comparable results can hardly be expected. Therefore, a reference database (RDB) was established by the organisers, which acted as a basis for the quantitative comparison of the participants' results. The detected deviations were related to the methodological details of the individual strategies. The comparative evaluation concept consisted of three steps: The first step was a comparison of the participants' samples (which were both centrally and individually analysed) between each other, as well as with the reference data base (RDB) and some given soil quality standards on the level of concentrations present. The comparison was made using the example of the metals cadmium, copper, lead and zinc. As a second step, the absolute and relative deviations between the reference database and the participants' results (both centrally analysed under repeatability conditions) were calculated. The comparability of the samples with the RDB was categorised on four levels. Methods of exploratory statistical analysis were applied to estimate the differential method bias among the participants. The levels of error caused by sampling and sample preparation were compared with those caused by the analytical procedures. As a third step, the methodological profiles of the participants were compiled to concisely describe the different procedures used. They were related to the results to find out the main factors leading to their incomparability. The outcome of this evaluation process was a list of strategies and methods, which are problematic with respect to comparability, and should be standardised and/or specified in order to arrive at representative and comparable results in soil contamination studies throughout Europe. Pre-normative recommendations for harmonising European soil sampling guidelines and standard operating procedures have been outlined in Wagner G, Desules A, Muntau H, Theocharopoulos S. Comparative Evaluation of European Methods for Sampling and Sample Preparation of Soils for Inorganic Analysis (CEEM Soil). Final Report of the Contract SMT4-CT96-2085, Sci Total Environ 2001;264:181-186. Wagner G, Desaules A, Munatu H. Theocharopolous S, Quevauvaller Ph. Suggestions for harmonising sampling and sample pre-treatment procedures and improving quality assurance in pre-analytical steps of soil contamination studies. Paper 1.7 Sci Total Environ 2001b;264:103-118.

Impact of metal-induced degradation on the determination of pharmaceutical compound purity and a strategy for mitigation.

PubMed

Dotterer, Sally K; Forbes, Robert A; Hammill, Cynthia L

2011-04-05

Case studies are presented demonstrating how exposure to traces of transition metals such as copper and/or iron during sample preparation or analysis can impact the accuracy of purity analysis of pharmaceuticals. Some compounds, such as phenols and indoles, react with metals in the presence of oxygen to produce metal-induced oxidative decomposition products. Compounds susceptible to metal-induced decomposition can degrade following preparation for purity analysis leading to falsely high impurity results. Our work has shown even metals at levels below 0.1 ppm can negatively impact susceptible compounds. Falsely low results are also possible when the impurities themselves react with metals and degrade prior to analysis. Traces of metals in the HPLC mobile phase can lead to chromatographic artifacts, affecting the reproducibility of purity results. To understand and mitigate the impact of metal induced decomposition, a proactive strategy is presented. The pharmaceutical would first be tested for reactivity with specific transition metals in the sample solvent/diluents and in the HPLC mobile phase. If found to be reactive, alternative sample diluents and/or mobile phases with less reactive solvents or addition of a metal chelator would be explored. If unsuccessful, glassware cleaning or sample solution refrigeration could be investigated. By employing this strategy during method development, robust purity methods would be delivered to the quality control laboratories, preventing future problems from potential sporadic contamination of glassware with metals. Copyright © 2010 Elsevier B.V. All rights reserved.

Manual for Preparing Individualized Education Programs.

ERIC Educational Resources Information Center

Baylor, Terrill D.

Presented are guidelines for developing an individualized program and services plan, an individual implementation plan, and daily activity and strategy plans for handicapped students. Instructions are outlined for utilizing forms related to planning and implementation of individualized education programs. Appended are sample forms. (SBH)

Improving FTIR imaging speciation of organic compound residues or their degradation products in wall painting samples, by introducing a new thin section preparation strategy based on cyclododecane pre-treatment.

PubMed

Papliaka, Zoi Eirini; Vaccari, Lisa; Zanini, Franco; Sotiropoulou, Sophia

2015-07-01

Fourier transform infrared (FTIR) imaging in transmission mode, employing a bidimensional focal plane array (FPA) detector, was applied for the detection and spatially resolved chemical characterisation of organic compounds or their degradation products within the stratigraphy of a critical group of fragments, originating from prehistoric and roman wall paintings, containing a very low concentration of subsisted organic matter or its alteration products. Past analyses using attenuated total reflection (ATR) or reflection FTIR on polished cross sections failed to provide any evidence of any organic material assignable as binding medium of the original painting. In order to improve the method's performance, in the present study, a new method of sample preparation in thin section was developed. The procedure is based on the use of cyclododecane C12H24 as embedding material and a subsequent double-side polishing of the specimen. Such procedure provides samples to be studied in FTIR transmission mode without losing the information on the spatial distribution of the detected materials in the paint stratigraphy. For comparison purposes, the same samples were also studied after opening their stratigraphy with a diamond anvil cell. Both preparation techniques offered high-quality chemical imaging of the decay products of an organic substance, giving clues to the painting technique. In addition, the thin sections resulting from the cyclododecane pre-treatment offered more layer-specific data, as the layer thickness and order remained unaffected, whereas the samples resulting from compression within the diamond cell were slightly deformed; however, since thinner and more homogenous, they provided higher spectral quality in terms of S/N ratio. In summary, the present study illustrates the appropriateness of FTIR imaging in transmission mode associated with a new thin section preparation strategy to detect and localise very low-concentrated organic matter subjected to deterioration processes, when the application of FTIR in reflection mode or FTIR-ATR fails to give any relevant information.

Direct and long-term detection of gene doping in conventional blood samples.

PubMed

Beiter, T; Zimmermann, M; Fragasso, A; Hudemann, J; Niess, A M; Bitzer, M; Lauer, U M; Simon, P

2011-03-01

The misuse of somatic gene therapy for the purpose of enhancing athletic performance is perceived as a coming threat to the world of sports and categorized as 'gene doping'. This article describes a direct detection approach for gene doping that gives a clear yes-or-no answer based on the presence or absence of transgenic DNA in peripheral blood samples. By exploiting a priming strategy to specifically amplify intronless DNA sequences, we developed PCR protocols allowing the detection of very small amounts of transgenic DNA in genomic DNA samples to screen for six prime candidate genes. Our detection strategy was verified in a mouse model, giving positive signals from minute amounts (20 μl) of blood samples for up to 56 days following intramuscular adeno-associated virus-mediated gene transfer, one of the most likely candidate vector systems to be misused for gene doping. To make our detection strategy amenable for routine testing, we implemented a robust sample preparation and processing protocol that allows cost-efficient analysis of small human blood volumes (200 μl) with high specificity and reproducibility. The practicability and reliability of our detection strategy was validated by a screening approach including 327 blood samples taken from professional and recreational athletes under field conditions.

Lesson Planning the Kodaly Way.

ERIC Educational Resources Information Center

Boshkoff, Ruth

1991-01-01

Discusses the contribution of Zoltan Kodaly to music lesson planning. Emphasizes preparation, presentation, and practice as the three important strategies in teaching concepts and skills to be included in a lesson plan. Includes a sample lesson plan covering a semester and advice on choosing song material. (DK)

A Preview of Coming Attractions: Classroom Teacher's Idea Notebook.

ERIC Educational Resources Information Center

Morin, Joy Ann

1995-01-01

Contends that it is important for students to be motivated and well prepared for class units and activities. Describes a "previews of coming attractions" instructional strategy that uses advance organizers to increase information processing efficiency. Includes a sample unit outline illustrating this approach. (CFR)

Optimization of sample preparation variables for wedelolactone from Eclipta alba using Box-Behnken experimental design followed by HPLC identification.

PubMed

Patil, A A; Sachin, B S; Shinde, D B; Wakte, P S

2013-07-01

Coumestan wedelolactone is an important phytocomponent from Eclipta alba (L.) Hassk. It possesses diverse pharmacological activities, which have prompted the development of various extraction techniques and strategies for its better utilization. The aim of the present study is to develop and optimize supercritical carbon dioxide assisted sample preparation and HPLC identification of wedelolactone from E. alba (L.) Hassk. The response surface methodology was employed to study the optimization of sample preparation using supercritical carbon dioxide for wedelolactone from E. alba (L.) Hassk. The optimized sample preparation involves the investigation of quantitative effects of sample preparation parameters viz. operating pressure, temperature, modifier concentration and time on yield of wedelolactone using Box-Behnken design. The wedelolactone content was determined using validated HPLC methodology. The experimental data were fitted to second-order polynomial equation using multiple regression analysis and analyzed using the appropriate statistical method. By solving the regression equation and analyzing 3D plots, the optimum extraction conditions were found to be: extraction pressure, 25 MPa; temperature, 56 °C; modifier concentration, 9.44% and extraction time, 60 min. Optimum extraction conditions demonstrated wedelolactone yield of 15.37 ± 0.63 mg/100 g E. alba (L.) Hassk, which was in good agreement with the predicted values. Temperature and modifier concentration showed significant effect on the wedelolactone yield. The supercritical carbon dioxide extraction showed higher selectivity than the conventional Soxhlet assisted extraction method. Copyright © 2013 Elsevier Masson SAS. All rights reserved.

Synthesis, characterization and application of ion imprinted polymeric nanobeads for highly selective preconcentration and spectrophotometric determination of Ni2 + ion in water samples

NASA Astrophysics Data System (ADS)

Rajabi, Hamid Reza; Razmpour, Saham

2016-01-01

Here, the researchers report on the synthesis of ion imprinted polymeric (IIP) nanoparticles using a thermal polymerization strategy, and their usage for the separation of Ni2 + ion from water samples. The prepared Ni-IIP was characterized by colorimetry, FT-IR spectroscopy, and scanning electron microscopy. It was found that the particle size of the prepared particle to be 50-70 nm in diameter with the highly selective binding capability for Ni2 + ion, with reasonable adsorption and desorption process. After preconcentration, bound ions can be eluted with an aqueous solution of hydrochloric acid, after their complexation with dimethylglyoxime, these ions can be quantified by UV-Vis absorption spectrophotometry. The effect of various parameters on the extraction efficiency including pH of sample solution, adsorption and leaching times, initial sample volume, concentration and volume of eluent were investigated. In selectivity study, it was found that imprinting causes increased affinity of the prepared IIP toward Ni2 + ion over other ions such as Na+, K+, Ag+, Co2 +, Cu2 +, Cd2 +, Hg2 +, Pb2 +, Zn2 +, Mn2 +, Mg2 +, Cr3 +, and Fe3 +. The prepared IIP can be used and regenerated for at least eight times without any significant decrease in binding affinities. The prepared IIP is considered to be promising and selective sorbent for solid-phase extraction and preconcentration of Ni2 + ion from different water samples.

State of the art of environmentally friendly sample preparation approaches for determination of PBDEs and metabolites in environmental and biological samples: A critical review.

PubMed

Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C

2016-01-28

Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

Gradient Material Strategies for Hydrogel Optimization in Tissue Engineering Applications

PubMed Central

2018-01-01

Although a number of combinatorial/high-throughput approaches have been developed for biomaterial hydrogel optimization, a gradient sample approach is particularly well suited to identify hydrogel property thresholds that alter cellular behavior in response to interacting with the hydrogel due to reduced variation in material preparation and the ability to screen biological response over a range instead of discrete samples each containing only one condition. This review highlights recent work on cell–hydrogel interactions using a gradient material sample approach. Fabrication strategies for composition, material and mechanical property, and bioactive signaling gradient hydrogels that can be used to examine cell–hydrogel interactions will be discussed. The effects of gradients in hydrogel samples on cellular adhesion, migration, proliferation, and differentiation will then be examined, providing an assessment of the current state of the field and the potential of wider use of the gradient sample approach to accelerate our understanding of matrices on cellular behavior. PMID:29485612

Ultra-high performance liquid chromatography coupled with quadrupole/time of flight mass spectrometry based chemical profiling approach for the holistic quality control of complex Kang-Jing formula preparations.

PubMed

Yang, Xiao-Huan; Cheng, Xiao-Lan; Qin, Bing; Cai, Zhuo-Ya; Cai, Xiong; Liu, Shao; Wang, Qi; Qin, Yong

2016-05-30

The Kang-Jing (KJ) formula is a compound preparation made from 12 kinds of herbs. So far, four different methods (M1-M4) have been documented for KJ preparation, but the influence of preparation methods on the holistic quality of KJ have remained unknown. In this study, a strategy was proposed to investigate the influence of different preparation methods on the holistic quality of KJ using ultra-high performance liquid chromatography coupled with quadrupole/time of flight mass spectrometry (UHPLC-QTOF-MS/MS) based chemical profiling. A total of 101 compounds mainly belonging to flavonoids, tanshinones, monoterpene glycosides, triterpenoid saponins, alkaloids, phenolic acids and volatile oils, were identified. Among these compounds, glaucine was detected only in M3/M4 samples, while two dehydrocorydaline isomers merely detected in M2/M3/M4 samples. Tetrahydrocolumbamine, ethylic lithospermic acid, salvianolic acid E and rosmarimic acid were only detected in M1/M3/M4 samples. In the subsequent quantitative analysis, 12 major compounds were determined by UHPLC-MS/MS. The proposed method was validated with respect to linearity, accuracy, precision and recovery. It was found that the contents of marker compounds varied significantly in samples prepared by different methods. These results demonstrated that preparation method does significantly affect the holistic quality of KJ. UHPLC-QTOF-MS/MS based chemical profiling approach is efficient and reliable for comprehensive quality evaluation of KJ. Collectively, this study provide the chemical evidence for revealing the material basis of KJ, and establish a simple and accurate chemical profiling method for its quality control. Copyright © 2016 Elsevier B.V. All rights reserved.

Electrical field-induced extraction and separation techniques: promising trends in analytical chemistry--a review.

PubMed

Yamini, Yadollah; Seidi, Shahram; Rezazadeh, Maryam

2014-03-03

Sample preparation is an important issue in analytical chemistry, and is often a bottleneck in chemical analysis. So, the major incentive for the recent research has been to attain faster, simpler, less expensive, and more environmentally friendly sample preparation methods. The use of auxiliary energies, such as heat, ultrasound, and microwave, is one of the strategies that have been employed in sample preparation to reach the above purposes. Application of electrical driving force is the current state-of-the-art, which presents new possibilities for simplifying and shortening the sample preparation process as well as enhancing its selectivity. The electrical driving force has scarcely been utilized in comparison with other auxiliary energies. In this review, the different roles of electrical driving force (as a powerful auxiliary energy) in various extraction techniques, including liquid-, solid-, and membrane-based methods, have been taken into consideration. Also, the references have been made available, relevant to the developments in separation techniques and Lab-on-a-Chip (LOC) systems. All aspects of electrical driving force in extraction and separation methods are too specific to be treated in this contribution. However, the main aim of this review is to provide a brief knowledge about the different fields of analytical chemistry, with an emphasis on the latest efforts put into the electrically assisted membrane-based sample preparation systems. The advantages and disadvantages of these approaches as well as the new achievements in these areas have been discussed, which might be helpful for further progress in the future. Copyright © 2013 Elsevier B.V. All rights reserved.

Improved Identification of Membrane Proteins by MALDI-TOF MS/MS Using Vacuum Sublimated Matrix Spots on an Ultraphobic Chip Surface

PubMed Central

Poetsch, Ansgar; Schlüsener, Daniela; Florizone, Christine; Eltis, Lindsay; Menzel, Christoph; Rögner, Matthias; Steinert, Kerstin; Roth, Udo

2008-01-01

Integral membrane proteins are notoriously difficult to identify and analyze by mass spectrometry because of their low abundance and limited number of trypsin cleavage sites. Our strategy to address this problem is based on a novel technology for MALDI-MS peptide sample preparation that increases the success rate of membrane protein identification by increasing the sensitivity of the MALDI-TOF system. For this, we used sample plates with predeposited matrix spots of CHCA crystals prepared by vacuum sublimation onto an extremely low wettable (ultraphobic) surface. In experiments using standard peptides, an up to 10-fold gain of sensitivity was found for on-chip preparations compared with classical dried-droplet preparations on a steel target. In order to assess the performance of the chips with membrane proteins, three model proteins (bacteriorhodopsin, subunit IV(a) of ATP synthase, and the cp47 subunit from photosystem II) were analyzed. To mimic realistic analysis conditions, purified proteins were separated by SDS-PAGE and digested with trypsin. The digest MALDI samples were prepared either by dried-droplet technique on steel plates using CHCA as matrix, or applied directly onto the matrix spots of the chip surface. Significantly higher signal-to-noise ratios were observed for all of the spectra resulting from on-chip preparations of different peptides. In a second series of experiments, the membrane proteome of Rhodococcus jostii RHA1 was investigated by AIEC/SDS-PAGE in combination with MALDI-TOF MS/MS. As in the first experiments, Coomassie-stained SDS-PAGE bands were digested and the two different preparation methods were compared. For preparations on the Mass·Spec·Turbo Chip, 43 of 60 proteins were identified, whereas only 30 proteins were reliably identified after classical sample preparation. Comparison of the obtained Mascot scores, which reflect the confidence level of the protein identifications, revealed that for 70% of the identified proteins, higher scores were obtained by on-chip sample preparation. Typically, this gain was a consequence of higher sequence coverage due to increased sensitivity. PMID:19137096

Chemical Ligation of Folded Recombinant Proteins: Segmental Isotopic Labeling of Domains for NMR Studies

NASA Astrophysics Data System (ADS)

Xu, Rong; Ayers, Brenda; Cowburn, David; Muir, Tom W.

1999-01-01

A convenient in vitro chemical ligation strategy has been developed that allows folded recombinant proteins to be joined together. This strategy permits segmental, selective isotopic labeling of the product. The src homology type 3 and 2 domains (SH3 and SH2) of Abelson protein tyrosine kinase, which constitute the regulatory apparatus of the protein, were individually prepared in reactive forms that can be ligated together under normal protein-folding conditions to form a normal peptide bond at the ligation junction. This strategy was used to prepare NMR sample quantities of the Abelson protein tyrosine kinase-SH(32) domain pair, in which only one of the domains was labeled with 15N Mass spectrometry and NMR analyses were used to confirm the structure of the ligated protein, which was also shown to have appropriate ligand-binding properties. The ability to prepare recombinant proteins with selectively labeled segments having a single-site mutation, by using a combination of expression of fusion proteins and chemical ligation in vitro, will increase the size limits for protein structural determination in solution with NMR methods. In vitro chemical ligation of expressed protein domains will also provide a combinatorial approach to the synthesis of linked protein domains.

Universal Solid-phase Reversible Sample-Prep for Concurrent Proteome and N-glycome Characterization

PubMed Central

Zhou, Hui; Morley, Samantha; Kostel, Stephen; Freeman, Michael R.; Joshi, Vivek; Brewster, David; Lee, Richard S.

2017-01-01

SUMMARY We describe a novel Solid-phase Reversible Sample-Prep (SRS) platform, which enables rapid sample preparation for concurrent proteome and N-glycome characterization by mass spectrometry. SRS utilizes a uniquely functionalized, silica-based bead that has strong affinity toward proteins with minimal-to-no affinity for peptides and other small molecules. By leveraging the inherent size difference between, SRS permits high-capacity binding of proteins, rapid removal of small molecules (detergents, metabolites, salts, etc.), extensive manipulation including enzymatic and chemical treatments on beads-bound proteins, and easy recovery of N-glycans and peptides. The efficacy of SRS was evaluated in a wide range of biological samples including single glycoprotein, whole cell lysate, murine tissues, and human urine. To further demonstrate the SRS platform, we coupled a quantitative strategy to SRS to investigate the differences between DU145 prostate cancer cells and its DIAPH3-silenced counterpart. Our previous studies suggested that DIAPH3 silencing in DU145 prostate cancer cells induced transition to an amoeboid phenotype that correlated with tumor progression and metastasis. In this analysis we identified distinct proteomic and N-glycomic alterations between the two cells. Intriguingly, a metastasis-associated tyrosine kinase receptor ephrin-type-A receptor (EPHA2) was highly upregulated in DIAPH3-silenced cells, indicating underling connection between EPHA2 and DIAPH3. Moreover, distinct alterations in the N-glycome were identified, suggesting a cross-link between DIAPH3 and glycosyltransferase networks. Overall, SRS is an enabling universal sample preparation strategy that is not size limited and has the capability to efficiently prepare and clean peptides and N-glycans concurrently from nearly all sample types. Conceptually, SRS can be utilized for the analysis of other posttranslational modifications, and the unique surface chemistry can be further transformed for high-throughput automation. The technical simplicity, robustness, and modularity of SRS make it a highly promising technology with great potential in proteomic-based research. PMID:26791391

A new strategy for preparation of hair slurries using cryogenic grinding and water-soluble tertiary-amines medium

NASA Astrophysics Data System (ADS)

Kamogawa, Marcos Y.; Nogueira, Ana Rita A.; Costa, Letícia M.; Garcia, Edivaldo E.; Nóbrega, Joaquim A.

2001-10-01

The investigation of trace metal contents in hair can be used as an index of exposure to potentially toxic elements. Direct determination of Cd, Cu and Pb in slurries of hair samples was investigated using an atomic absorption spectrometer with Zeeman-effect background correction. The samples were pulverized in a freezer/mill for 13 min, and hair slurries with 1.0 g l -1 for the determination of Cu and Pb, and 5.0 g l -1 for the determination of Cd, respectively, were prepared in three different media: 0.1% v/v Triton X-100, 0.14 mol l -1 HNO 3, and 0.1% v/v of CFA-C, a mixture of tertiary amines. The easiest way to manipulate the hair samples was in CFA-C medium. The optimum pyrolysis and atomization temperatures were established with hair sample slurries spiked with 10 μg l -1 Cd 2+, 30 μg l -1 Pb 2+, and 10 μg l -1 Cu 2+. For Cd and Pb, Pd was used as a chemical modifier, and for Cu no modifier was needed. The analyte addition technique was used for quantification of Cd, Cu, and Pb in hair sample slurries. A reference material (GBW076901) was analyzed, and a paired t-test showed that the results for all elements obtained with the proposed slurry sampling procedure were in agreement at a 95% confidence level with the certified values. The cryogenic grinding was an effective strategy to efficiently pulverize hair samples.

Visualizing BPA by molecularly imprinted ratiometric fluorescence sensor based on dual emission nanoparticles.

PubMed

Lu, Hongzhi; Xu, Shoufang

2017-06-15

Construction of ratiometric fluorescent probe often involved in tedious multistep preparation or complicated coupling or chemical modification process. The emergence of dual emission fluorescent nanoparticles would simplify the construction process and avoids the tedious chemical coupling. Herein, we reported a facile strategy to prepare ratiometric fluorescence molecularly imprinted sensor based on dual emission nanoparticles (d-NPs) which comprised of carbon dots and gold nanoclusters for detection of Bisphenol A (BPA). D-NPs emission at 460nm and 580nm were first prepared by seed growth co-microwave method using gold nanoparticles as seeds and glucose as precursor for carbon dots. When they were applied to propose ratiometric fluorescence molecularly imprinted sensor, the preparation process was simplified, and the sensitivity of sensor was improved with detection limit of 29nM, and visualizing BPA was feasible based on the distinguish fluorescence color change. The feasibility of the developed method in real samples was successfully evaluated through the analysis of BPA in water samples with satisfactory recoveries of 95.9-98.9% and recoveries ranging from 92.6% to 98.6% in canned food samples. When detection BPA in positive feeding bottles, the results agree well with those obtained by accredited method. The developed method proposed in this work to prepare ratiometric fluorescence molecularly imprinted sensor based on dual emission nanoparticles proved to be a convenient, reliable and practical way to prepared high sensitive and selective fluorescence sensors. Copyright © 2017 Elsevier B.V. All rights reserved.

Systems analysis of singly and multiply O-glycosylated peptides in the human serum glycoproteome via EThcD and HCD mass spectrometry.

PubMed

Zhang, Yong; Xie, Xinfang; Zhao, Xinyuan; Tian, Fang; Lv, Jicheng; Ying, Wantao; Qian, Xiaohong

2018-01-06

Human serum has been intensively studied to identify biomarkers via global proteomic analysis. The altered O-glycoproteome is associated with human pathological state including cancer, inflammatory and degenerative diseases and is an attractive source of disease biomarkers. Because of the microheterogeneity and macroheterogeneity of O-glycosylation, site-specific O-glycosylation analysis in human serum is still challenging. Here, we developed a systematic strategy that combined multiple enzyme digestion, multidimensional separation for sample preparation and high-resolution tandem MS with Byonic software for intact O-glycopeptide characterization. We demonstrated that multiple enzyme digestion or multidimensional separation can make sample preparation more efficient and that EThcD is not only suitable for the identification of singly O-glycosylated peptides (50.3%) but also doubly (21.2%) and triply (28.5%) O-glycosylated peptides. Totally, with the strict scoring criteria, 499 non-redundant intact O-glycopeptides, 173 O-glycosylation sites and 6 types of O-glycans originating from 49 O-glycoprotein groups were identified in human serum, including 121 novel O-glycosylation sites. Currently, this is the largest data set of site-specific native O-glycoproteome from human serum samples. We expect that the strategies developed by this study will facilitate in-depth analyses of native O-glycoproteomes in human serum and provide opportunities to understand the functional roles of protein O-glycosylation in human health and diseases. The altered O-glycoproteome is associated with human pathological state and is an attractive source of disease biomarkers. However, site-specific O-glycosylation analysis is challenging because of the microheterogeneity (different glycoforms attached to one glycosylation site) and macroheterogeneity (site occupancy) of O-glycosylation. In this work, we developed a systematic strategy for intact O-glycopeptide characterization. This study took advantage of the inherent properties of the new fragmentation method called EThcD, which provides more complete fragmentation information about O-glycosylated peptides and a more confident site localization of O-glycans than collision-induced dissociation (HCD). We demonstrated that multiple enzyme digestion or multidimensional separation can make sample preparation more efficient and that EThcD was not only suitable for the identification of singly O-glycosylated peptides (50.3%) but also doubly (21.2%) and triply (28.5%) O-glycosylated peptides. Finally, we got a largest data set of site-specific native O-glycoproteome from human serum samples. Furthermore, quantitative analysis of intact O-glycopeptides from the serum samples of IgA nephropathy (IgAN) patients and healthy donors was performed, and the results showed the potential of the strategy to discover O-glycosylation biomarkers. We expect that the strategies developed by this study will facilitate in-depth analyses of native O-glycoproteomes in human serum and lead to exciting opportunities to understand the functional roles of protein O-glycosylation in human health and diseases. Copyright © 2017. Published by Elsevier B.V.

Quality assurance in the determination of metals in clinical chemistry and toxicology: the METOS project. Metalli Tossici.

PubMed

Patriarca, M; Menditto, A; Morisi, G

1995-01-01

National external quality assessment schemes (EQAS) for the determination of trace elements in blood (Al, Cd, Cu, Pb, Zn) have been promoted in Italy since 1983. They were organized by a working group of the Istituto Superiore di Sanità and known as "METOS (Metalli Tossici, toxic metals) project". The organization of the schemes included the preparation of suitable control materials by the promoting centre and the elaboration of valuable strategies of sample distribution, treatment of data and evaluation of results, that could be applied even to a small number of participants. The procedures used and the results obtained in ten years of activity of the METOS project are reported. Within the framework of the programme some information has been obtained, confirming the validity of the procedures used for sample preparation, sample distribution and evaluation of laboratories performance.

Database extraction strategies for low-template evidence.

PubMed

Bleka, Øyvind; Dørum, Guro; Haned, Hinda; Gill, Peter

2014-03-01

Often in forensic cases, the profile of at least one of the contributors to a DNA evidence sample is unknown and a database search is needed to discover possible perpetrators. In this article we consider two types of search strategies to extract suspects from a database using methods based on probability arguments. The performance of the proposed match scores is demonstrated by carrying out a study of each match score relative to the level of allele drop-out in the crime sample, simulating low-template DNA. The efficiency was measured by random man simulation and we compared the performance using the SGM Plus kit and the ESX 17 kit for the Norwegian population, demonstrating that the latter has greatly enhanced power to discover perpetrators of crime in large national DNA databases. The code for the database extraction strategies will be prepared for release in the R-package forensim. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

Methodological considerations for implementation of lymphocyte subset analysis in a clinical reference laboratory.

PubMed

Muirhead, K A; Wallace, P K; Schmitt, T C; Frescatore, R L; Franco, J A; Horan, P K

1986-01-01

As the diagnostic utility of lymphocyte subset analysis has been recognized in the clinical research laboratory, a wide variety of reagents and cell preparation, staining and analysis methods have also been described. Methods that are perfectly suitable for analysis of smaller sample numbers in the biological or clinical research setting are not always appropriate and/or applicable in the setting of a high volume clinical reference laboratory. We describe here some of the specific considerations involved in choosing a method for flow cytometric analysis which minimizes sample preparation and data analysis time while maximizing sample stability, viability, and reproducibility. Monoclonal T- and B-cell reagents from three manufacturers were found to give equivalent results for a reference population of healthy individuals. This was true whether direct or indirect immunofluorescence staining was used and whether cells were prepared by Ficoll-Hypaque fractionation (FH) or by lysis of whole blood. When B cells were enumerated using a polyclonal anti-immunoglobulin reagent, less cytophilic immunoglobulin staining was present after lysis than after FH preparation. However, both preparation methods required additional incubation at 37 degrees C to obtain results concordant with monoclonal B-cell reagents. Standard reagents were chosen on the basis of maximum positive/negative separation and the availability of appropriate negative controls. The effects of collection medium and storage conditions on sample stability and reproducibility of subset analysis were also assessed. Specimens collected in heparin and stored at room temperature in buffered medium gave reproducible results for 3 days after specimen collection, using either FH or lysis as the preparation method. General strategies for instrument optimization, quality control, and biohazard containment are also discussed.

Automation of dimethylation after guanidination labeling chemistry and its compatibility with common buffers and surfactants for mass spectrometry-based shotgun quantitative proteome analysis.

PubMed

Lo, Andy; Tang, Yanan; Chen, Lu; Li, Liang

2013-07-25

Isotope labeling liquid chromatography-mass spectrometry (LC-MS) is a major analytical platform for quantitative proteome analysis. Incorporation of isotopes used to distinguish samples plays a critical role in the success of this strategy. In this work, we optimized and automated a chemical derivatization protocol (dimethylation after guanidination, 2MEGA) to increase the labeling reproducibility and reduce human intervention. We also evaluated the reagent compatibility of this protocol to handle biological samples in different types of buffers and surfactants. A commercially available liquid handler was used for reagent dispensation to minimize analyst intervention and at least twenty protein digest samples could be prepared in a single run. Different front-end sample preparation methods for protein solubilization (SDS, urea, Rapigest™, and ProteaseMAX™) and two commercially available cell lysis buffers were evaluated for compatibility with the automated protocol. It was found that better than 94% desired labeling could be obtained in all conditions studied except urea, where the rate was reduced to about 92% due to carbamylation on the peptide amines. This work illustrates the automated 2MEGA labeling process can be used to handle a wide range of protein samples containing various reagents that are often encountered in protein sample preparation for quantitative proteome analysis. Copyright © 2013 Elsevier B.V. All rights reserved.

Identification of (antioxidative) plants in herbal pharmaceutical preparations and dietary supplements.

PubMed

Deconinck, Eric; Custers, Deborah; De Beer, Jacques Omer

2015-01-01

The standard procedures for the identification, authentication, and quality control of medicinal plants and herbs are nowadays limited to pure herbal products. No guidelines or procedures, describing the detection or identification of a targeted plant or herb in pharmaceutical preparations or dietary supplements, can be found. In these products the targeted plant is often present together with other components of herbal or synthetic origin. This chapter describes a strategy for the fast development of a chromatographic fingerprint approach that allows the identification of a targeted plant in herbal preparations and dietary supplements. The strategy consists of a standard chromatographic gradient that is tested for the targeted plant with different extraction solvents and different mobile phases. From the results obtained, the optimal fingerprint is selected. Subsequently the samples are analyzed according to the selected methodological parameters, and the obtained fingerprints can be compared with the one obtained for the pure herbal product or a standard preparation. Calculation of the dissimilarity between these fingerprints will result in a probability of presence of the targeted plant. Optionally mass spectrometry can be used to improve specificity, to confirm identification, or to identify molecules with a potential medicinal or antioxidant activity.

Testing the implementation and sustainment facilitation (ISF) strategy as an effective adjunct to the Addiction Technology Transfer Center (ATTC) strategy: study protocol for a cluster randomized trial.

PubMed

Garner, Bryan R; Zehner, Mark; Roosa, Mathew R; Martino, Steve; Gotham, Heather J; Ball, Elizabeth L; Stilen, Patricia; Speck, Kathryn; Vandersloot, Denna; Rieckmann, Traci R; Chaple, Michael; Martin, Erika G; Kaiser, David; Ford, James H

2017-11-17

Improving the extent to which evidence-based practices (EBPs)-treatments that have been empirically shown to be efficacious or effective-are integrated within routine practice is a well-documented challenge across numerous areas of health. In 2014, the National Institute on Drug Abuse funded a type 2 effectiveness-implementation hybrid trial titled the substance abuse treatment to HIV Care (SAT2HIV) Project. Aim 1 of the SAT2HIV Project tests the effectiveness of a motivational interviewing-based brief intervention (MIBI) for substance use as an adjunct to usual care within AIDS service organizations (ASOs) as part of its MIBI Experiment. Aim 2 of the SAT2HIV Project tests the effectiveness of implementation and sustainment facilitation (ISF) as an adjunct to the Addiction Technology Transfer Center (ATTC) model for training staff in motivational interviewing as part of its ISF Experiment. The current paper describes the study protocol for the ISF Experiment. Using a cluster randomized design, case management and leadership staff from 39 ASOs across the United States were randomized to receive either the ATTC strategy (control condition) or the ATTC + ISF strategy (experimental condition). The ATTC strategy is staff-focused and includes 10 discrete strategies (e.g., provide centralized technical assistance, conduct educational meetings, provide ongoing consultation). The ISF strategy is organization-focused and includes seven discrete strategies (e.g., use an implementation advisor, organize implementation team meetings, conduct cyclical small tests of change). Building upon the exploration-preparation-implementation-sustainment (EPIS) framework, the effectiveness of the ISF strategy is examined via three staff-level measures: (1) time-to-proficiency (i.e., preparation phase outcome), (2) implementation effectiveness (i.e., implementation phase outcome), and (3) level of sustainment (i.e., sustainment phase outcome). Although not without limitations, the ISF experiment has several strengths: a highly rigorous design (randomized, hypothesis-driven), high-need setting (ASOs), large sample size (39 ASOs), large geographic representation (23 states and the District of Columbia), and testing along multiple phases of the EPIS continuum (preparation, implementation, and sustainment). Thus, study findings will significantly improve generalizable knowledge regarding the best preparation, implementation, and sustainment strategies for advancing EBPs along the EPIS continuum. Moreover, increasing ASO's capacity to address substance use may improve the HIV Care Continuum. Trial registration ClinicalTrials.gov: NCT03120598.

Large-Scale Low-Cost NGS Library Preparation Using a Robust Tn5 Purification and Tagmentation Protocol

PubMed Central

Hennig, Bianca P.; Velten, Lars; Racke, Ines; Tu, Chelsea Szu; Thoms, Matthias; Rybin, Vladimir; Besir, Hüseyin; Remans, Kim; Steinmetz, Lars M.

2017-01-01

Efficient preparation of high-quality sequencing libraries that well represent the biological sample is a key step for using next-generation sequencing in research. Tn5 enables fast, robust, and highly efficient processing of limited input material while scaling to the parallel processing of hundreds of samples. Here, we present a robust Tn5 transposase purification strategy based on an N-terminal His6-Sumo3 tag. We demonstrate that libraries prepared with our in-house Tn5 are of the same quality as those processed with a commercially available kit (Nextera XT), while they dramatically reduce the cost of large-scale experiments. We introduce improved purification strategies for two versions of the Tn5 enzyme. The first version carries the previously reported point mutations E54K and L372P, and stably produces libraries of constant fragment size distribution, even if the Tn5-to-input molecule ratio varies. The second Tn5 construct carries an additional point mutation (R27S) in the DNA-binding domain. This construct allows for adjustment of the fragment size distribution based on enzyme concentration during tagmentation, a feature that opens new opportunities for use of Tn5 in customized experimental designs. We demonstrate the versatility of our Tn5 enzymes in different experimental settings, including a novel single-cell polyadenylation site mapping protocol as well as ultralow input DNA sequencing. PMID:29118030

Variable memory strategy use in children's adaptive intratask learning behavior: developmental changes and working memory influences in free recall.

PubMed

Lehmann, Martin; Hasselhorn, Marcus

2007-01-01

Variability in strategy use within single trials in free recall was analyzed longitudinally from second to fourth grades (ages 8-10 years). To control for practice effects another sample of fourth graders was included (age 10 years). Video analyses revealed that children employed different strategies when preparing for free recall. A gradual shift from labeling to cumulative rehearsal was present both with increasing age and across different list positions. Whereas cumulative rehearsal was frequent at early list positions, labeling was dominant at later list portions. Working memory capacity predicted the extent of cumulative rehearsal usage, which became more efficient with increasing age. Results are discussed in the context of the adaptive strategy choice model.

Design Considerations of a Compounded Sterile Preparations Course

PubMed Central

Petraglia, Christine; Mattison, Melissa J.

2016-01-01

Objective. To design a comprehensive learning and assessment environment for the practical application of compounded sterile preparations using a constructivist approach. Design. Compounded Sterile Preparations Laboratory is a required 1-credit course that builds upon the themes of training aseptic technique typically used in health system settings and threads application of concepts from other courses in the curriculum. Students used critical-thinking skills to devise appropriate strategies to compound sterile preparations. Assessment. Aseptic technique skills were assessed with objective, structured, checklist-based rubrics. Most students successfully completed practical assessments using appropriate technique (mean assessment grade=83.2%). Almost all students passed the practical media fill (98%) and gloved fingertip sampling (86%) tests on the first attempt; all passed on the second attempt. Conclusion. Employing a constructivist scaffold approach to teaching proper hygiene and aseptic technique prepared students to pass media fill and gloved fingertip tests and to perform well on practical compounding assessments. PMID:26941438

INTERIM REPORT, DEVELOP A SAMPLING STRATEGY: PREPARE TO IMPLEMENT A COHORT STUDY OF CHILDREN'S ENVIRONMENTAL HEALTH

EPA Science Inventory

Overview

The goal of the National Children's Study (NCS) is to collect information on environmental and

social factors in the lives of children, starting before birth and continuing until age 21, to inform

researchers about their effects on the health and dev...

Interaction between tungsten monocarbide and an iron-based metallic melt

NASA Astrophysics Data System (ADS)

Chumanov, I. V.; Anikeev, A. N.

2015-12-01

A technique and results of investigation of compacted tungsten carbide substrates by scanning microscopy are reported. Samples are prepared in the course of studies of the wettability of tungsten carbide substrates with the iron melt, which are performed in accordance with the sessile drop method using two different heating strategies, namely, contact and noncontact heating of metal.

Perceptions of Memo Quality: A Case Study of Engineering Practitioners, Professors, and Students

ERIC Educational Resources Information Center

Amare, Nicole; Brammer, Charlotte

2005-01-01

One goal of college technical writing courses is to prepare students for real-world writing situations. Business writing textbooks function similarly, using guidelines, sample assignments, and model documents to help students develop rhetorical strategies to use in the workplace. Students attend class, or read and perform exercises in a textbook,…

An X-ray transparent microfluidic platform for screening of the phase behavior of lipidic mesophases

PubMed Central

Khvostichenko, Daria S.; Kondrashkina, Elena; Perry, Sarah L.; Pawate, Ashtamurthy S.; Brister, Keith

2013-01-01

Lipidic mesophases are a class of highly ordered soft materials that form when certain lipids are mixed with water. Understanding the relationship between the composition and the microstructure of mesophases is necessary for fundamental studies of self-assembly in amphiphilic systems and for applications, such as crystallization of membrane proteins. However, the laborious formulation protocol for highly viscous mesophases and the large amounts of material required for sample formulation are significant obstacles in such studies. Here we report a microfluidic platform that facilitates investigations of the phase behavior of mesophases by reducing sample consumption, and automating and parallelizing sample formulation. The mesophases were formulated on-chip using less than 40 nL of material per sample and their microstructure was analyzed in situ using small-angle X-ray scattering (SAXS). The 220 μm-thick X-ray compatible platform was comprised of thin polydimethylsiloxane (PDMS) layers sandwiched between cyclic olefin copolymer (COC) sheets. Uniform mesophases were prepared using an active on-chip mixing strategy coupled with periodic cooling of the sample to reduce the viscosity. We validated the platform by preparing and analyzing mesophases of lipid monoolein (MO) mixed with aqueous solutions of different concentrations of β-octylglucoside (βOG), a detergent frequently used in membrane protein crystallization. Four samples were prepared in parallel on chip, by first metering and automatically diluting βOG to obtain detergent solutions of different concentration, then metering MO, and finally mixing by actuation of pneumatic valves. Integration of detergent dilution and subsequent mixing significantly reduced the number of manual steps needed for sample preparation. Three different types of mesophases typical for monoolein were successfully identified in SAXS data from on-chip samples. Microstructural parameters of identical samples formulated in different chips showed excellent agreement. Phase behavior observed on-chip corresponded well with that of samples prepared via the traditional coupled-syringe method (“off-chip”) using 300-fold larger amount of material, further validating the utility of the microfluidic platform for on-chip characterization of mesophase behavior. PMID:23882463

Substrate preparation for reliable imaging of DNA molecules with the scanning force microscope.

PubMed

Vesenka, J; Guthold, M; Tang, C L; Keller, D; Delaine, E; Bustamante, C

1992-07-01

A simple method of substrate preparation for imaging circular DNA molecules with the scanning force microscope (SFM) is presented. These biomolecules are adsorbed onto mica that has been soaked in magnesium acetate, sonicated and glow-discharged. The stylus-sample forces that may be endured before sample damage occurs depends on the ambient relative humidity. Images of circular DNA molecules have been obtained routinely using tips specially modified by an electron beam with a radius of curvature, Rc, of about 10 nm [D. Keller and C. Chih-Chung, Surf. Sci. 268 (1992) 333]. The resolution of these adsorbed biomolecules is determined by the Rc. At higher forces individual circular DNA molecules can be manipulated with the SFM stylus. Strategies to develop still sharper probes will be discussed.

Geospatial database for regional environmental assessment of central Colorado.

USGS Publications Warehouse

Church, Stan E.; San Juan, Carma A.; Fey, David L.; Schmidt, Travis S.; Klein, Terry L.; DeWitt, Ed H.; Wanty, Richard B.; Verplanck, Philip L.; Mitchell, Katharine A.; Adams, Monique G.; Choate, LaDonna M.; Todorov, Todor I.; Rockwell, Barnaby W.; McEachron, Luke; Anthony, Michael W.

2012-01-01

In conjunction with the future planning needs of the U.S. Department of Agriculture, Forest Service, the U.S. Geological Survey conducted a detailed environmental assessment of the effects of historical mining on Forest Service lands in central Colorado. Stream sediment, macroinvertebrate, and various filtered and unfiltered water quality samples were collected during low-flow over a four-year period from 2004–2007. This report summarizes the sampling strategy, data collection, and analyses performed on these samples. The data are presented in Geographic Information System, Microsoft Excel, and comma-delimited formats. Reports on data interpretation are being prepared separately.

Accelerating root system phenotyping of seedlings through a computer-assisted processing pipeline.

PubMed

Dupuy, Lionel X; Wright, Gladys; Thompson, Jacqueline A; Taylor, Anna; Dekeyser, Sebastien; White, Christopher P; Thomas, William T B; Nightingale, Mark; Hammond, John P; Graham, Neil S; Thomas, Catherine L; Broadley, Martin R; White, Philip J

2017-01-01

There are numerous systems and techniques to measure the growth of plant roots. However, phenotyping large numbers of plant roots for breeding and genetic analyses remains challenging. One major difficulty is to achieve high throughput and resolution at a reasonable cost per plant sample. Here we describe a cost-effective root phenotyping pipeline, on which we perform time and accuracy benchmarking to identify bottlenecks in such pipelines and strategies for their acceleration. Our root phenotyping pipeline was assembled with custom software and low cost material and equipment. Results show that sample preparation and handling of samples during screening are the most time consuming task in root phenotyping. Algorithms can be used to speed up the extraction of root traits from image data, but when applied to large numbers of images, there is a trade-off between time of processing the data and errors contained in the database. Scaling-up root phenotyping to large numbers of genotypes will require not only automation of sample preparation and sample handling, but also efficient algorithms for error detection for more reliable replacement of manual interventions.

Coupling detergent lysis/clean-up methodology with intact protein fractionation for enhanced proteome characterization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Ritin; Dill, Brian; Chourey, Karuna

2012-01-01

The expanding use of surfactants for proteome sample preparations has prompted the need to systematically optimize the application and removal of these MS-deleterious agents prior to proteome measurements. Here we compare four different detergent clean-up methods (Trichloroacetic acid (TCA) precipitation, Chloroform/Methanol/Water (CMW) extraction, commercial detergent removal spin column method (DRS) and filter-aided sample preparation(FASP)) with respect to varying amounts of protein biomass in the samples, and provide efficiency benchmarks with respect to protein, peptide, and spectral identifications for each method. Our results show that for protein limited samples, FASP outperforms the other three clean-up methods, while at high protein amountmore » all the methods are comparable. This information was used in a dual strategy of comparing molecular weight based fractionated and unfractionated lysates from three increasingly complex samples (Escherichia coli, a five microbial isolate mixture, and a natural microbial community groundwater sample), which were all lysed with SDS and cleaned up using FASP. The two approaches complemented each other by enhancing the number of protein identifications by 8%-25% across the three samples and provided broad pathway coverage.« less

Healthier home food preparation methods and youth and caregiver psychosocial factors are associated with lower BMI in African American youth.

PubMed

Kramer, Rebecca F; Coutinho, Anastasia J; Vaeth, Elisabeth; Christiansen, Karina; Suratkar, Sonali; Gittelsohn, Joel

2012-05-01

Obesity disproportionately affects African American (AA) children and adolescents and leads to an increased risk of adult chronic diseases. Eating few meals at home has been implicated as a cause of obesity among youth, but to our knowledge, previous studies have not specifically investigated this relationship in AA adolescents or looked at both the healthfulness and frequency of home meals in AA households. The objective of the present study was to investigate the relationship between home food preparation and adolescent BMI in a sample of 240 AA adolescents aged 10-15 y and their caregivers. Multiple linear regressions were used to model psychosocial characteristics, household factors, and adolescent and caregiver food preparation behaviors as predictors of adolescent BMI, and psychosocial and household factors as predictors of food preparation behavior. Adolescents in the sample had a mean BMI-for-age percentile of 70.4, and >90% of the sample families received at least one form of food assistance. Adolescent children of caregivers who used healthier cooking methods were more likely to use healthy cooking methods themselves (P = 0.02). Having more meals prepared by a caregiver was predictive of higher BMI-for-age percentile in adolescents (P = 0.02), but healthier cooking methods used by the caregiver was associated with reduced risk of adolescent overweight or obesity (P < 0.01). Meals prepared at home in AA households do not necessarily promote healthy BMI in youth. Family meals are a promising adolescent obesity prevention strategy, but it is important to target both frequency and healthfulness of meals prepared at home for effective health promotion in AA families.

Clinical nurses' perceptions and expectations of the role of doctorally-prepared nurses: a qualitative study in Iran.

PubMed

Cheraghi, Mohammad-Ali; Jasper, Melanie; Vaismoradi, Mojtaba

2014-01-01

Nurses with doctorates are increasing in number throughout the world, yet the multitude of roles they play following graduation is unclear. The purpose of this study was to explore and describe clinical nurses' perceptions and expectations of the role of doctorally-prepared nurses in Iran. A qualitative study, using a content analysis approach was conducted with 43 clinical nurses chosen using a purposive sampling strategy. Oral, semi-structured and written interviews were used to generate data. During data analysis, three main themes emerged; "advantages of the doctoral degree", "clarification of doctorally-prepared nurses' role in clinical practice", and "unmet expectations of doctorally-prepared nurses". An understanding of the expectations of nurses on the role of doctorally-prepared nurses is needed to improve the collaboration between clinical nurses and doctorally-prepared nurses; remove misunderstandings on the abilities and skills of doctorally-prepared nurses; incorporate the expectations into doctoral education in order to facilitate their collaboration; and also remove the theory and practice gap through the utilisation of doctorally-prepared nurses' knowledge and skills in practice. Copyright © 2013 Elsevier Ltd. All rights reserved.

Microfluidic devices for sample preparation and rapid detection of foodborne pathogens.

PubMed

Kant, Krishna; Shahbazi, Mohammad-Ali; Dave, Vivek Priy; Ngo, Tien Anh; Chidambara, Vinayaka Aaydha; Than, Linh Quyen; Bang, Dang Duong; Wolff, Anders

2018-03-10

Rapid detection of foodborne pathogens at an early stage is imperative for preventing the outbreak of foodborne diseases, known as serious threats to human health. Conventional bacterial culturing methods for foodborne pathogen detection are time consuming, laborious, and with poor pathogen diagnosis competences. This has prompted researchers to call the current status of detection approaches into question and leverage new technologies for superior pathogen sensing outcomes. Novel strategies mainly rely on incorporating all the steps from sample preparation to detection in miniaturized devices for online monitoring of pathogens with high accuracy and sensitivity in a time-saving and cost effective manner. Lab on chip is a blooming area in diagnosis, which exploits different mechanical and biological techniques to detect very low concentrations of pathogens in food samples. This is achieved through streamlining the sample handling and concentrating procedures, which will subsequently reduce human errors and enhance the accuracy of the sensing methods. Integration of sample preparation techniques into these devices can effectively minimize the impact of complex food matrix on pathogen diagnosis and improve the limit of detections. Integration of pathogen capturing bio-receptors on microfluidic devices is a crucial step, which can facilitate recognition abilities in harsh chemical and physical conditions, offering a great commercial benefit to the food-manufacturing sector. This article reviews recent advances in current state-of-the-art of sample preparation and concentration from food matrices with focus on bacterial capturing methods and sensing technologies, along with their advantages and limitations when integrated into microfluidic devices for online rapid detection of pathogens in foods and food production line. Copyright © 2018. Published by Elsevier Inc.

Tracing origins of complex pharmaceutical preparations using surface desorption atmospheric pressure chemical ionization mass spectrometry.

PubMed

Zhang, Xinglei; Jia, Bin; Huang, Keke; Hu, Bin; Chen, Rong; Chen, Huanwen

2010-10-01

A novel strategy to trace the origins of commercial pharmaceutical products has been developed based on the direct chemical profiling of the pharmaceutical products by surface desorption atmospheric pressure chemical ionization mass spectrometry (DAPCI-MS). Besides the unambiguous identification of active drug components, various compounds present in the matrixes are simultaneously detected without sample pretreatment, providing valuable information for drug quality control and origin differentiation. Four sources of commercial amoxicillin products made by different manufacturers have been successfully differentiated. This strategy has been extended to secerning six sources of Liuwei Dihuang Teapills, which are herbal medicine preparations with extremely complex matrixes. The photolysis status of chemical drug products and the inferior natural herd medicine products prepared with different processes (e.g., extra heating) were also screened using the method reported here. The limit of detection achieved in the MS/MS experiments was estimated to be 1 ng/g for amoxicillin inside the capsule product. Our experimental data demonstrate that DAPCI-MS is a useful tool for rapid pharmaceutical analysis, showing promising perspectives for tracking the entire pharmaceutical supply chain to prevent counterfeit intrusions.

Study of sample preparation for determination of endocannabinoids and analogous compounds in human serum by LC-MS/MS in MRM mode.

PubMed

Luque-Córdoba, D; Calderón-Santiago, M; Luque de Castro, M D; Priego-Capote, F

2018-08-01

Endocannabinoids are lipids with a key role in physiological processes such as the immune response or the metabolism. This involvement explains their association to pathologies such as cancer, obesity or multiple sclerosis. The determination of endocannabinoids constitutes a challenge for clinical laboratories due to the variety of biological matrices and the wide range of concentrations at which they can be found. This research deals with the comparison of three sample preparation strategies (viz., on-line SPE, off-line SPE for interferents removal, and protein precipitation) for subsequent LC-MS/MS analysis of 14 endocannabinoids and analogous compounds in serum. As a result, the on-line coupling between SPE and LC-MS/MS is proposed as the best approach for this determination. The proposed method allows full automation of the overall process, shortening of the analysis time, and avoidance of errors associated with sample preparation steps. The improvement in sensitivity and selectivity thus achieved allows obtaining quantification limits at the pg mL -1 level, which makes possible the application of the method for clinical studies. Copyright © 2018 Elsevier B.V. All rights reserved.

Identifying tips for intramolecular NC-AFM imaging via in situ fingerprinting

NASA Astrophysics Data System (ADS)

Sang, Hongqian; Jarvis, Samuel P.; Zhou, Zhichao; Sharp, Peter; Moriarty, Philip; Wang, Jianbo; Wang, Yu; Kantorovich, Lev

2014-10-01

A practical experimental strategy is proposed that could potentially enable greater control of the tip apex in non-contact atomic force microscopy experiments. It is based on a preparation of a structure of interest alongside a reference surface reconstruction on the same sample. Our proposed strategy is as follows. Spectroscopy measurements are first performed on the reference surface to identify the tip apex structure using a previously collected database of responses of different tips to this surface. Next, immediately following the tip identification protocol, the surface of interest is studied (imaging, manipulation and/or spectroscopy). The prototype system we choose is the mixed Si(111)-7×7 and surface which can be prepared on the same sample with a controlled ratio of reactive and passivated regions. Using an ``in silico'' approach based on ab initio density functional calculations and a set of tips with varying chemical reactivities, we show how one can perform tip fingerprinting using the Si(111)-7×7 reference surface. Then it is found by examining the imaging of a naphthalene tetracarboxylic diimide (NTCDI) molecule adsorbed on surface that negatively charged tips produce the best intramolecular contrast attributed to the enhancement of repulsive interactions.

Absolute Quantification of Middle- to High-Abundant Plasma Proteins via Targeted Proteomics.

PubMed

Dittrich, Julia; Ceglarek, Uta

2017-01-01

The increasing number of peptide and protein biomarker candidates requires expeditious and reliable quantification strategies. The utilization of liquid chromatography coupled to quadrupole tandem mass spectrometry (LC-MS/MS) for the absolute quantitation of plasma proteins and peptides facilitates the multiplexed verification of tens to hundreds of biomarkers from smallest sample quantities. Targeted proteomics assays derived from bottom-up proteomics principles rely on the identification and analysis of proteotypic peptides formed in an enzymatic digestion of the target protein. This protocol proposes a procedure for the establishment of a targeted absolute quantitation method for middle- to high-abundant plasma proteins waiving depletion or enrichment steps. Essential topics as proteotypic peptide identification and LC-MS/MS method development as well as sample preparation and calibration strategies are described in detail.

An Internal Standard for Assessing Phosphopeptide Recovery from Metal Ion/Oxide Enrichment Strategies

NASA Astrophysics Data System (ADS)

Paulo, Joao A.; Navarrete-Perea, Jose; Erickson, Alison R.; Knott, Jeffrey; Gygi, Steven P.

2018-04-01

Phosphorylation-mediated signaling pathways have major implications in cellular regulation and disease. However, proteins with roles in these pathways are frequently less abundant and phosphorylation is often sub-stoichiometric. As such, the efficient enrichment, and subsequent recovery of phosphorylated peptides, is vital. Mass spectrometry-based proteomics is a well-established approach for quantifying thousands of phosphorylation events in a single experiment. We designed a peptide internal standard-based assay directed toward sample preparation strategies for mass spectrometry analysis to understand better phosphopeptide recovery from enrichment strategies. We coupled mass-differential tandem mass tag (mTMT) reagents (specifically, TMTzero and TMTsuper-heavy), nine mass spectrometry-amenable phosphopeptides (phos9), and peak area measurements from extracted ion chromatograms to determine phosphopeptide recovery. We showcase this mTMT/phos9 recovery assay by evaluating three phosphopeptide enrichment workflows. Our assay provides data on the recovery of phosphopeptides, which complement other metrics, namely the number of identified phosphopeptides and enrichment specificity. Our mTMT/phos9 assay is applicable to any enrichment protocol in a typical experimental workflow irrespective of sample origin or labeling strategy. [Figure not available: see fulltext.

Synthesis of amino-functionalized silica nanoparticles for preparation of new laboratory standards

NASA Astrophysics Data System (ADS)

Alvarez-Toral, Aitor; Fernández, Beatriz; Malherbe, Julien; Claverie, Fanny; Pecheyran, Christophe; Pereiro, Rosario

2017-12-01

Platinum group elements (PGEs) are particularly interesting analytes in different fields, including environmental samples as well as high cost materials that contain them, such as for example automotive catalysts. This type of solid samples could be analysed by laser ablation (LA) coupled to ICP-MS, which allow to significantly reducing the analysis time since the time-consuming processes for sample preparation are not required. There is a considerable demand of standards with high PGEs concentration for quantification purposes, which cannot be carried out easily using LA-ICP-MS because the available standards (i.e. NIST SRM 61 × series) do not have such analytes in the same concentration range. In this paper, a new strategy is proposed for the synthesis of homogeneous laboratory standards with Pt, Pd and Rh concentrations that range from 77 μg/g of Pd up to 2035 μg/g of Rh. The proposed strategy is based on the synthesis of monodisperse amino-functionalized amorphous silica nanoparticles, which can retain metal ions. In addition to Pt, Pd and Rh, three lanthanides were also added to the nanoparticles (La, Ce, Nd). Sturdy pressed pellets can be made from the resulting nanopowder without the use of any binder. Elemental composition of standards made of nanoparticles was analysed by conventional nebulization ICP-MS and their homogeneity was successfully evaluated by LA-ICP-MS.

Detection of bacteria in platelet concentrates prepared from spiked single donations using cultural and molecular genetic methods.

PubMed

Störmer, M; Cassens, U; Kleesiek, K; Dreier, J

2007-02-01

Bacteria show differences in their growth kinetics depending on the type of blood component. On to storage at 22 degrees C, platelet concentrates (PCs) seem to be more prone to bacterial multiplication than red cell concentrates. Knowledge of the potential for bacterial proliferation in blood components, which are stored at a range of temperatures, is essential before considering implementation of a detection strategy. The efficacy of bacterial detection was determined, using real-time reverse transcriptase-polymerase chain reaction (RT-PCR), following bacterial growth in blood components obtained from a deliberately contaminated whole-blood (WB) unit. Cultivation was used as the reference method. WB was spiked with 2 colony-forming units mL(-1)Staphylococcus epidermidis or Klebsiella pneumoniae, kept for 15 h at room temperature and component preparation was processed. Samples were drawn, at intervals throughout the whole separation process, from each blood component. Nucleic acids were extracted using an automated high-volume extraction method. The 15-h storage revealed an insignificant increase in bacterial titre. No bacterial growth was detected in red blood cell or plasma units. K. pneumoniae showed rapid growth in the pooled PC and could be detected immediately after preparation using RT-PCR. S. epidermidis grew slowly and was detected 24 h after separation. These experiments show that sampling is indicative at 24 h after preparation of PCs at the earliest to minimize the sampling error.

Biochemical Fractionation and Stable Isotope Dilution Liquid Chromatography-mass Spectrometry for Targeted and Microdomain-specific Protein Quantification in Human Postmortem Brain Tissue*

PubMed Central

MacDonald, Matthew L.; Ciccimaro, Eugene; Prakash, Amol; Banerjee, Anamika; Seeholzer, Steven H.; Blair, Ian A.; Hahn, Chang-Gyu

2012-01-01

Synaptic architecture and its adaptive changes require numerous molecular events that are both highly ordered and complex. A majority of neuropsychiatric illnesses are complex trait disorders, in which multiple etiologic factors converge at the synapse via many signaling pathways. Investigating the protein composition of synaptic microdomains from human patient brain tissues will yield valuable insights into the interactions of risk genes in many disorders. These types of studies in postmortem tissues have been limited by the lack of proper study paradigms. Thus, it is necessary not only to develop strategies to quantify protein and post-translational modifications at the synapse, but also to rigorously validate them for use in postmortem human brain tissues. In this study we describe the development of a liquid chromatography-selected reaction monitoring method, using a stable isotope-labeled neuronal proteome standard prepared from the brain tissue of a stable isotope-labeled mouse, for the multiplexed quantification of target synaptic proteins in mammalian samples. Additionally, we report the use of this method to validate a biochemical approach for the preparation of synaptic microdomain enrichments from human postmortem prefrontal cortex. Our data demonstrate that a targeted mass spectrometry approach with a true neuronal proteome standard facilitates accurate and precise quantification of over 100 synaptic proteins in mammalian samples, with the potential to quantify over 1000 proteins. Using this method, we found that protein enrichments in subcellular fractions prepared from human postmortem brain tissue were strikingly similar to those prepared from fresh mouse brain tissue. These findings demonstrate that biochemical fractionation methods paired with targeted proteomic strategies can be used in human brain tissues, with important implications for the study of neuropsychiatric disease. PMID:22942359

Alumni-based evaluation of a novel veterinary curriculum: are Nottingham graduates prepared for clinical practice?

PubMed Central

Cobb, K. A.; Brown, G. A.; Hammond, R. H.; Mossop, L. H.

2015-01-01

Introduction Outcomes-based education has been the core of the curriculum strategy of the Nottingham School of Veterinary Medicine and Science (SVMS) since its inception in 2006. As part of the ongoing curriculum evaluation, the first two graduating cohorts were invited to provide an appraisal of their preparation by the SVMS curriculum for their role in clinical practice. This paper provides brief accounts of the SVMS curriculum model, the development of the evaluation instrument and the findings of the alumni survey. Materials and Methods The evaluation instrument contained 25 attributes expected of SVMS graduates. Alumni rated their preparation for practice in relation to each attribute. Results The four highest rated characteristics were compassion for animals and the application of ethics to animal welfare; communication skills; recognising own limitations and seeking help and advice where needed and clinical examination skills. The four lowest rated were clinical case management and therapeutic strategies; dealing with veterinary public health and zoonotic issues; knowledge of current veterinary legislation and dealing with emergency and critical care cases. Free text responses were in line with these quantitative findings. Conclusion The results indicate that this sample of SVMS graduates were satisfied with their undergraduate education and felt well prepared for their role in clinical practice. PMID:26392910

Comparison between traditional strategies and classification technique (SIMCA) in the identification of old proteinaceous binders.

PubMed

Checa-Moreno, R; Manzano, E; Mirón, G; Capitan-Vallvey, L F

2008-05-15

In this paper, we performed a comparison between commonly used strategies amino acid ratios (Aa ratios), two-dimensional ratio plots (2D-Plot) and statistical correlation factor (SCF) and a classification technique, soft independent modelling of class analogy (SIMCA), to identify protein binders present in old artwork samples. To do this, we used a natural standard collection of proteinaceous binders prepared in our laboratory using old recipes and eleven samples coming from Cultural Heritage, such as mural and easel paintings, manuscripts and polychrome sculptures from the 15-18th centuries. Protein binder samples were hydrolyzed and their constitutive amino acids were determined as PITC-derivatives using HPLC-DAD. Amino acid profile data were used to perform the comparison between the four different strategies mentioned above. Traditional strategies can lead to ambiguous or non-conclusive results. With SIMCA, it is possible to provide a more robust and less subjective identification knowing the confidence level of identification. As a standard, we used proteinaceous albumin (whole egg, yolk and glair); casein (goat, cow and sheep) and collagen (mammalian and fish). The process results in a more robust understanding of proteinaceous binding media in old artworks that makes it possible to distinguish them according to their origin.

Laser-induced breakdown spectroscopy for analysis of plant materials: A review

NASA Astrophysics Data System (ADS)

Santos, Dário, Jr.; Nunes, Lidiane Cristina; de Carvalho, Gabriel Gustinelli Arantes; Gomes, Marcos da Silva; de Souza, Paulino Florêncio; Leme, Flavio de Oliveira; dos Santos, Luis Gustavo Cofani; Krug, Francisco José

2012-05-01

Developments and contributions of laser-induced breakdown spectroscopy (LIBS) for the determination of elements in plant materials are reviewed. Several applications where the solid samples are interrogated by simply focusing the laser pulses directly onto a fresh or dried surface of leaves, roots, fruits, vegetables, wood and pollen are presented. For quantitative purposes aiming at plant nutrition diagnosis, the test sample presentation in the form of pressed pellets, prepared from clean, dried and properly ground/homogenized leaves, and the use of univariate or multivariate calibration strategies are revisited.

A novel strategy using MASCOT Distiller for analysis of cleavable isotope-coded affinity tag data to quantify protein changes in plasma.

PubMed

Leung, Kit-Yi; Lescuyer, Pierre; Campbell, James; Byers, Helen L; Allard, Laure; Sanchez, Jean-Charles; Ward, Malcolm A

2005-08-01

A novel strategy consisting of cleavable Isotope-Coded Affinity Tag (cICAT) combined with MASCOT Distiller was evaluated as a tool for the quantification of proteins in "abnormal" patient plasma, prepared by pooling samples from patients with acute stroke. Quantification of all light and heavy cICAT-labelled peptide ion pairs was obtained using MASCOT Distiller combined with a proprietary software. Peptides displaying differences were selected for identification by MS. These preliminary results show the promise of our approach to identify potential biomarkers.

Advances in ultrasensitive mass spectrometry of organic molecules.

PubMed

Kandiah, Mathivathani; Urban, Pawel L

2013-06-21

Ultrasensitive mass spectrometric analysis of organic molecules is important for various branches of chemistry, and other fields including physics, earth and environmental sciences, archaeology, biomedicine, and materials science. It finds applications--as an enabling tool--in systems biology, biological imaging, clinical analysis, and forensics. Although there are a number of technical obstacles associated with the analysis of samples by mass spectrometry at ultratrace level (for example analyte losses during sample preparation, insufficient sensitivity, ion suppression), several noteworthy developments have been made over the years. They include: sensitive ion sources, loss-free interfaces, ion optics components, efficient mass analyzers and detectors, as well as "smart" sample preparation strategies. Some of the mass spectrometric methods published to date can achieve sensitivity which is by several orders of magnitude higher than that of alternative approaches. Femto- and attomole level limits of detection are nowadays common, while zepto- and yoctomole level limits of detection have also been reported. We envision that the ultrasensitive mass spectrometric assays will soon contribute to new discoveries in bioscience and other areas.

Quantum dots assisted laser desorption/ionization mass spectrometric detection of carbohydrates: qualitative and quantitative analysis.

PubMed

Bibi, Aisha; Ju, Huangxian

2016-04-01

A quantum dots (QDs) assisted laser desorption/ionization mass spectrometric (QDA-LDI-MS) strategy was proposed for qualitative and quantitative analysis of a series of carbohydrates. The adsorption of carbohydrates on the modified surface of different QDs as the matrices depended mainly on the formation of hydrogen bonding, which led to higher MS intensity than those with conventional organic matrix. The effects of QDs concentration and sample preparation method were explored for improving the selective ionization process and the detection sensitivity. The proposed approach offered a new dimension to the application of QDs as matrices for MALDI-MS research of carbohydrates. It could be used for quantitative measurement of glucose concentration in human serum with good performance. The QDs served as a matrix showed the advantages of low background, higher sensitivity, convenient sample preparation and excellent stability under vacuum. The QDs assisted LDI-MS approach has promising application to the analysis of carbohydrates in complex biological samples. Copyright © 2016 John Wiley & Sons, Ltd.

Flipped Classroom: Do Students Perceive Readiness for Advanced Discussion?

PubMed

Hoover, Carrie Ann; Dinndorf-Hogenson, Georgia Ann; Peterson, Jennifer Lee; Tollefson, Bethany Renae; Berndt, Jodi Lisbeth; Laudenbach, Nikki

2018-03-01

Use of the flipped classroom model is recognized as a popular method of instruction. Effective preclass preparation methods can create more time for instructors to reinforce application, evaluation, and analysis of information using active learning strategies. This quasi-experimental study used a convenience sample of 42 third-year baccalaureate nursing students. Students were randomized into two groups and received either a narrated video (vodcast) or guided readings for the preclass preparation. A quiz was administered to assess preparation prior to class, and students completed a survey following the classroom activities. Students preferred media preparation to guided readings. This preference translated to higher quiz scores. Positive correlations were noted between quiz scores and students' understanding and increased confidence. Students' preference for the vodcast translated to the perception of an increase in confidence and understanding of the material. [J Nurs Educ. 2018;57(3):163-165.]. Copyright 2018, SLACK Incorporated.

Plant iTRAQ-based proteomics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Handakumbura, Pubudu; Hixson, Kim K.; Purvine, Samuel O.

We present a simple one-­pot extraction protocol, which rapidly isolates hydrophyllic metabolites, lipids, and proteins from the same pulverized plant sample. Also detailed is a global plant proteomics sample preparation method utilizing iTRAQ multiplexing reagents that enables deep proteome coverage due to the use of HPLC fractionation of the peptides prior to mass spectrometric analysis. We have successfully used this protocol on several different plant tissues (e.g., roots, stems, leaves) from different plants (e.g., sorghum, poplar, Arabidopsis, soybean), and have been able to successfully detect and quantify thousands of proteins. Multiplexing strategies such as iTRAQ and the bioinformatics strategy outlinedmore » here, ultimately provide insight into which proteins are significantly changed in abundance between two or more groups (e.g., control, perturbation). Our bioinformatics strategy yields z-­score values, which normalize the expression data into a format that can easily be cross-­compared with other expression data (i.e., metabolomics, transcriptomics) obtained from different analytical methods and instrumentation.« less

High-resolution X-ray diffraction with no sample preparation

PubMed Central

Turner, S. M. R.; Degryse, P.; Shortland, A. J.

2017-01-01

It is shown that energy-dispersive X-ray diffraction (EDXRD) implemented in a back-reflection geometry is extremely insensitive to sample morphology and positioning even in a high-resolution configuration. This technique allows high-quality X-ray diffraction analysis of samples that have not been prepared and is therefore completely non-destructive. The experimental technique was implemented on beamline B18 at the Diamond Light Source synchrotron in Oxfordshire, UK. The majority of the experiments in this study were performed with pre-characterized geological materials in order to elucidate the characteristics of this novel technique and to develop the analysis methods. Results are presented that demonstrate phase identification, the derivation of precise unit-cell parameters and extraction of microstructural information on unprepared rock samples and other sample types. A particular highlight was the identification of a specific polytype of a muscovite in an unprepared mica schist sample, avoiding the time-consuming and difficult preparation steps normally required to make this type of identification. The technique was also demonstrated in application to a small number of fossil and archaeological samples. Back-reflection EDXRD implemented in a high-resolution configuration shows great potential in the crystallographic analysis of cultural heritage artefacts for the purposes of scientific research such as provenancing, as well as contributing to the formulation of conservation strategies. Possibilities for moving the technique from the synchrotron into museums are discussed. The avoidance of the need to extract samples from high-value and rare objects is a highly significant advantage, applicable also in other potential research areas such as palaeontology, and the study of meteorites and planetary materials brought to Earth by sample-return missions. PMID:28660862

Ionic liquid-mediated synthesis of meso-scale porous lanthanum-transition-metal perovskites with high CO oxidation performance

DOE PAGES

Lu, Hanfeng; Zhang, Pengfei; Qiao, Zhen-An; ...

2015-02-19

Lanthanum-transition-metal perovskites with robust meso-scale porous frameworks (meso-LaMO 3) are synthesized through use of ionic liquids. The resultant samples demonstrate a rather high activity for CO oxidation, by taking advantage of unique nanostructure-derived benefits. This synthesis strategy opens up a new opportunity for preparing functional mesoporous complex oxides of various compositions.

Ionic liquid-mediated synthesis of meso-scale porous lanthanum-transition-metal perovskites with high CO oxidation performance

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lu, Hanfeng; Zhang, Pengfei; Qiao, Zhen-An

Lanthanum-transition-metal perovskites with robust meso-scale porous frameworks (meso-LaMO 3) are synthesized through use of ionic liquids. The resultant samples demonstrate a rather high activity for CO oxidation, by taking advantage of unique nanostructure-derived benefits. This synthesis strategy opens up a new opportunity for preparing functional mesoporous complex oxides of various compositions.

Rapid and interference-free analysis of nine B-group vitamins in energy drinks using trilinear component modeling of liquid chromatography-mass spectrometry data.

PubMed

Hu, Yong; Wu, Hai-Long; Yin, Xiao-Li; Gu, Hui-Wen; Xiao, Rong; Xie, Li-Xia; Liu, Zhi; Fang, Huan; Wang, Li; Yu, Ru-Qin

2018-04-01

The aim of the present work was to develop a rapid and interference-free method based on liquid chromatography-mass spectrometry (LC-MS) for the simultaneous determination of nine B-group vitamins in various energy drinks. A smart and green strategy that modeled the three-way data array of LC-MS with second-order calibration methods based on alternating trilinear decomposition (ATLD) and alternating penalty trilinear decomposition (APTLD) algorithms was developed. By virtue of "mathematical separation" and "second-order advantage", the proposed strategy successfully solved the co-eluted peaks and unknown interferents in LC-MS analysis with the elution time less than 4.5min and simple sample preparation. Satisfactory quantitative results were obtained by the ATLD-LC-MS and APTLD-LC-MS methods for the spiked recovery assays, with the average spiked recoveries ranging from 87.2-113.9% to 92.0-111.7%, respectively. These results acquired from the proposed methods were confirmed by the LC-MS/MS method, which shows a quite good consistency with each other. All these results demonstrated that the developed chemometrics-assisted LC-MS strategy had advantages of being rapid, green, accurate and low-cost, and it could be an attractive alternative for the determination of multiple vitamins in complex food matrices, which required no laborious sample preparation, tedious condition optimization or more sophisticated instrumentations. Copyright © 2017 Elsevier B.V. All rights reserved.

Solid-phase reductive amination for glycomic analysis.

PubMed

Jiang, Kuan; Zhu, He; Xiao, Cong; Liu, Ding; Edmunds, Garrett; Wen, Liuqing; Ma, Cheng; Li, Jing; Wang, Peng George

2017-04-15

Reductive amination is an indispensable method for glycomic analysis, as it tremendously facilitates glycan characterization and quantification by coupling functional tags at the reducing ends of glycans. However, traditional in-solution derivatization based approach for the preparation of reductively aminated glycans is quite tedious and time-consuming. Here, a simpler and more efficient strategy termed solid-phase reductive amination was investigated. The general concept underlying this new approach is to streamline glycan extraction, derivatization, and purification on non-porous graphitized carbon sorbents. Neutral and sialylated standard glycans were utilized to test the feasibility of the solid-phase method. As results, almost complete labeling of those glycans with four common labels of aniline, 2-aminobenzamide (2-AB), 2-aminobenzoic acid (2-AA) and 2-amino-N-(2-aminoethyl)-benzamide (AEAB) was obtained, and negligible desialylation occurred during sample preparation. The labeled glycans derived from glycoproteins showed excellent reproducibility in high performance liquid chromatography (HPLC) and matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) analysis. Direct comparisons based on fluorescent absorbance and relative quantification using isotopic labeling demonstrated that the solid-phase strategy enabled 20-30% increase in sample recovery. In short, the solid-phase strategy is simple, reproducible, efficient, and sensitive for glycan analysis. This method was also successfully applied for N-glycan profiling of HEK 293 cells with MALDI-TOF MS, showing its attractive application in the high-throughput analysis of mammalian glycome. Published by Elsevier B.V.

Development of isotope labeling LC-MS for human salivary metabolomics and application to profiling metabolome changes associated with mild cognitive impairment.

PubMed

Zheng, Jiamin; Dixon, Roger A; Li, Liang

2012-12-18

Saliva is a readily available biofluid that may contain metabolites of interest for diagnosis and prognosis of diseases. In this work, a differential (13)C/(12)C isotope dansylation labeling method, combined with liquid chromatography Fourier transform ion cyclotron resonance mass spectrometry (LC-FTICR-MS), is described for quantitative profiling of the human salivary metabolome. New strategies are presented to optimize the sample preparation and LC-MS detection processes. The strategies allow the use of as little of 5 μL of saliva sample as a starting material to determine the concentration changes of an average of 1058 ion pairs or putative metabolites in comparative saliva samples. The overall workflow consists of several steps including acetone-induced protein precipitation, (12)C-dansylation labeling of the metabolites, and LC-UV measurement of the total concentration of the labeled metabolites in individual saliva samples. A pooled sample was prepared from all the individual samples and labeled with (13)C-dansylation to serve as a reference. Using this metabolome profiling method, it was found that compatible metabolome results could be obtained after saliva samples were stored in tubes normally used for genetic material collection at room temperature, -20 °C freezer, and -80 °C freezer over a period of 1 month, suggesting that many saliva samples already collected in genomic studies could become a valuable resource for metabolomics studies, although the effect of much longer term of storage remains to be determined. Finally, the developed method was applied for analyzing the metabolome changes of two different groups: normal healthy older adults and comparable older adults with mild cognitive impairment (MCI). Top-ranked 18 metabolites successfully distinguished the two groups, among which seven metabolites were putatively identified while one metabolite, taurine, was definitively identified.

A dilute-and-shoot sample preparation strategy for new and used lubricating oils for Ca, P, S and Zn determination by total reflection X-ray fluorescence

NASA Astrophysics Data System (ADS)

Mota, Mariana F. B.; Gama, Ednilton M.; Rodrigues, Gabrielle de C.; Rodrigues, Guilherme D.; Nascentes, Clésia C.; Costa, Letícia M.

2018-01-01

In this work, a dilute-and-shoot method was developed for Ca, P, S and Zn determination in new and used lubricating oil samples by total reflection X-ray fluorescence (TXRF). The oil samples were diluted with organic solvents followed by addition of yttrium as internal standard and the TXRF measurements were performed after solvent evaporation. The method was optimized using an interlaboratorial reference material. The experimental parameters evaluated were sample volume (50 or 100 μL), measurement time (250 or 500 s) and volume deposited on the quartz glass sample carrier (5 or 10 μL). All of them were evaluated and optimized using xylene, kerosene and hexane. Analytical figures of merit (accuracy, precision, limit of detection and quantification) were used to evaluate the performance of the analytical method for all solvents. The recovery rates varied from 99 to 111% and the relative standard deviation remained between 1.7% and 10% (n = 8). For all elements, the results obtained by applying the new method were in agreement with the certified value. After the validation step, the method was applied for Ca, P, S and Zn quantification in eight new and four used lubricating oil samples, for all solvents. The concentration of the elements in the samples varied in the ranges of 1620-3711 mg L- 1 for Ca, 704-1277 mg L- 1 for P, 2027-9147 mg L- 1 for S, and 898-1593 mg L- 1 for Zn. The association of TXRF with a dilute-and-shoot sample preparation strategy was efficient for Ca, P, S and Zn determination in lubricating oils, presenting accurate results. Additionally, the time required for analysis is short, the reagent volumes are low minimizing waste generation, and the technique does not require calibration curves.

Effects of Information Access Cost and Accountability on Medical Residents' Information Retrieval Strategy and Performance During Prehandover Preparation: Evidence From Interview and Simulation Study.

PubMed

Yang, X Jessie; Wickens, Christopher D; Park, Taezoon; Fong, Liesel; Siah, Kewin T H

2015-12-01

We aimed to examine the effects of information access cost and accountability on medical residents' information retrieval strategy and performance during prehandover preparation. Prior studies observing doctors' prehandover practices witnessed the use of memory-intensive strategies when retrieving patient information. These strategies impose potential threats to patient safety as human memory is prone to errors. Of interest in this work are the underlying determinants of information retrieval strategy and the potential impacts on medical residents' information preparation performance. A two-step research approach was adopted, consisting of semistructured interviews with 21 medical residents and a simulation-based experiment with 32 medical residents. The semistructured interviews revealed that a substantial portion of medical residents (38%) relied largely on memory for preparing handover information. The simulation-based experiment showed that higher information access cost reduced information access attempts and access duration on patient documents and harmed information preparation performance. Higher accountability led to marginally longer access to patient documents. It is important to understand the underlying determinants of medical residents' information retrieval strategy and performance during prehandover preparation. We noted the criticality of easy access to patient documents in prehandover preparation. In addition, accountability marginally influenced medical residents' information retrieval strategy. Findings from this research suggested that the cost of accessing information sources should be minimized in developing handover preparation tools. © 2015, Human Factors and Ergonomics Society.

Review of in situ derivatization techniques for enhanced bioanalysis using liquid chromatography with mass spectrometry.

PubMed

Baghdady, Yehia Z; Schug, Kevin A

2016-01-01

Accurate and specific analysis of target molecules in complex biological matrices remains a significant challenge, especially when ultra-trace detection limits are required. Liquid chromatography with mass spectrometry is often the method of choice for bioanalysis. Conventional sample preparation and clean-up methods prior to the analysis of biological fluids such as liquid-liquid extraction, solid-phase extraction, or protein precipitation are time-consuming, tedious, and can negatively affect target recovery and detection sensitivity. An alternative or complementary strategy is the use of an off-line or on-line in situ derivatization technique. In situ derivatization can be incorporated to directly derivatize target analytes in their native biological matrices, without any prior sample clean-up methods, to substitute or even enhance the extraction and preconcentration efficiency of these traditional sample preparation methods. Designed appropriately, it can reduce the number of sample preparation steps necessary prior to analysis. Moreover, in situ derivatization can be used to enhance the performance of the developed liquid chromatography with mass spectrometry-based bioanalysis methods regarding stability, chromatographic separation, selectivity, and ionization efficiency. This review presents an overview of the commonly used in situ derivatization techniques coupled to liquid chromatography with mass spectrometry-based bioanalysis to guide and to stimulate future research. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Integrated massively parallel sequencing of 15 autosomal STRs and Amelogenin using a simplified library preparation approach.

PubMed

Xue, Jian; Wu, Riga; Pan, Yajiao; Wang, Shunxia; Qu, Baowang; Qin, Ying; Shi, Yuequn; Zhang, Chuchu; Li, Ran; Zhang, Liyan; Zhou, Cheng; Sun, Hongyu

2018-04-02

Massively parallel sequencing (MPS) technologies, also termed as next-generation sequencing (NGS), are becoming increasingly popular in study of short tandem repeats (STR). However, current library preparation methods are usually based on ligation or two-round PCR that requires more steps, making it time-consuming (about 2 days), laborious and expensive. In this study, a 16-plex STR typing system was designed with fusion primer strategy based on the Ion Torrent S5 XL platform which could effectively resolve the above challenges for forensic DNA database-type samples (bloodstains, saliva stains, etc.). The efficiency of this system was tested in 253 Han Chinese participants. The libraries were prepared without DNA isolation and adapter ligation, and the whole process only required approximately 5 h. The proportion of thoroughly genotyped samples in which all the 16 loci were successfully genotyped was 86% (220/256). Of the samples, 99.7% showed 100% concordance between NGS-based STR typing and capillary electrophoresis (CE)-based STR typing. The inconsistency might have been caused by off-ladder alleles and mutations in primer binding sites. Overall, this panel enabled the large-scale genotyping of the DNA samples with controlled quality and quantity because it is a simple, operation-friendly process flow that saves labor, time and costs. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development and Psychometric Examination of the Inclusive Teaching Strategies in Nursing Education Instrument.

PubMed

Levey, Janet A

2017-08-01

Nurse educators might be unknowingly excluding learners secondary to teaching practices. Universal design for instruction (UDI) prepares and delivers accessible content and learning environments for diverse learners; however, it is not well known in nursing education. The aim of the study was to examine the psychometric properties of the Inclusive Teaching Strategies in Nursing Education (ITSinNE) 55-item instrument. Confirmatory factor analysis was performed on a sample of 311 educators in prelicensure programs. The ITSinNE scales had good to adequate estimates of reliability. The exogenous model fit the sample and model-implied covariance matrix; however, the endogenous model was not a good fit. Further instrument development is required. Measuring factors influencing nurse educators' willingness to adopt UDI will enable intervention research to enhance professional development fostering content and environmental access for all learners.

Integration of the Uncertainties of Anion and TOC Measurements into the Flammability Control Strategy for Sludge Batch 8 at the DWPF

DOE Office of Scientific and Technical Information (OSTI.GOV)

Edwards, T. B.

2013-03-14

The Savannah River National Laboratory (SRNL) has been working with the Savannah River Remediation (SRR) Defense Waste Processing Facility (DWPF) in the development and implementation of a flammability control strategy for DWPF’s melter operation during the processing of Sludge Batch 8 (SB8). SRNL’s support has been in response to technical task requests that have been made by SRR’s Waste Solidification Engineering (WSE) organization. The flammability control strategy relies on measurements that are performed on Slurry Mix Evaporator (SME) samples by the DWPF Laboratory. Measurements of nitrate, oxalate, formate, and total organic carbon (TOC) standards generated by the DWPF Laboratory aremore » presented in this report, and an evaluation of the uncertainties of these measurements is provided. The impact of the uncertainties of these measurements on DWPF’s strategy for controlling melter flammability also is evaluated. The strategy includes monitoring each SME batch for its nitrate content and its TOC content relative to the nitrate content and relative to the antifoam additions made during the preparation of the SME batch. A linearized approach for monitoring the relationship between TOC and nitrate is developed, equations are provided that integrate the measurement uncertainties into the flammability control strategy, and sample calculations for these equations are shown to illustrate the impact of the uncertainties on the flammability control strategy.« less

A new dimethyl labeling-based SID-MRM-MS method and its application to three proteases involved in insulin maturation.

PubMed

Cheng, Dongwan; Zheng, Li; Hou, Junjie; Wang, Jifeng; Xue, Peng; Yang, Fuquan; Xu, Tao

2015-01-01

The absolute quantification of target proteins in proteomics involves stable isotope dilution coupled with multiple reactions monitoring mass spectrometry (SID-MRM-MS). The successful preparation of stable isotope-labeled internal standard peptides is an important prerequisite for the SID-MRM absolute quantification methods. Dimethyl labeling has been widely used in relative quantitative proteomics and it is fast, simple, reliable, cost-effective, and applicable to any protein sample, making it an ideal candidate method for the preparation of stable isotope-labeled internal standards. MRM mass spectrometry is of high sensitivity, specificity, and throughput characteristics and can quantify multiple proteins simultaneously, including low-abundance proteins in precious samples such as pancreatic islets. In this study, a new method for the absolute quantification of three proteases involved in insulin maturation, namely PC1/3, PC2 and CPE, was developed by coupling a stable isotope dimethyl labeling strategy for internal standard peptide preparation with SID-MRM-MS quantitative technology. This method offers a new and effective approach for deep understanding of the functional status of pancreatic β cells and pathogenesis in diabetes.

Heat Management Strategies for Solid-state NMR of Functional Proteins

PubMed Central

Fowler, Daniel J.; Harris, Michael J.; Thompson, Lynmarie K.

2012-01-01

Modern solid-state NMR methods can acquire high-resolution protein spectra for structure determination. However, these methods use rapid sample spinning and intense decoupling fields that can heat and denature the protein being studied. Here we present a strategy to avoid destroying valuable samples. We advocate first creating a sacrificial sample, which contains unlabeled protein (or no protein) in buffer conditions similar to the intended sample. This sample is then doped with the chemical shift thermometer Sm2Sn2O7. We introduce a pulse scheme called TCUP (for Temperature Calibration Under Pulseload) that can characterize the heating of this sacrificial sample rapidly, under a variety of experimental conditions, and with high temporal resolution. Sample heating is discussed with respect to different instrumental variables such as spinning speed, decoupling strength and duration, and cooling gas flow rate. The effects of different sample preparation variables are also discussed, including ionic strength, the inclusion of cryoprotectants, and the physical state of the sample (i.e. liquid, solid, or slurry). Lastly, we discuss probe detuning as a measure of sample thawing that does not require retuning the probe or using chemical shift thermometer compounds. Use of detuning tests and chemical shift thermometers with representative sample conditions makes it possible to maximize the efficiency of the NMR experiment while retaining a functional sample. PMID:22868258

Rapid purification of diastereoisomers from Piper kadsura using supercritical fluid chromatography with chiral stationary phases.

PubMed

Xin, Huaxia; Dai, Zhuoshun; Cai, Jianfeng; Ke, Yanxiong; Shi, Hui; Fu, Qing; Jin, Yu; Liang, Xinmiao

2017-08-04

Supercritical fluid chromatography (SFC) with chiral stationary phases (CSPs) is an advanced solution for the separation of achiral compounds in Piper kadsura. Analogues and stereoisomers are abundant in natural products, but there are obstacles in separation using conventional method. In this paper, four lignan diastereoisomers, (-)-Galbelgin, (-)-Ganschisandrin, Galgravin and (-)-Veraguensin, from Piper kadsura were separated and purified by chiral SFC. Purification strategy was designed, considering of the compound enrichment, sample purity and purification throughput. Two-step achiral purification method on chiral preparative columns with stacked automated injections was developed. Unconventional mobile phase modifier dichloromethane (DCM) was applied to improve the sample solubility. Four diastereoisomers was prepared at the respective weight of 103.1mg, 10.0mg, 152.3mg and 178.6mg from 710mg extract with the purity of greater than 98%. Copyright © 2017 Elsevier B.V. All rights reserved.

Making the practically impossible "Merely difficult"--Cryogenic FIB lift-out for "Damage free" soft matter imaging.

PubMed

Parmenter, Christopher D J; Fay, Michael W; Hartfield, Cheryl; Eltaher, Hoda M

2016-04-01

The preparation of thinned lamellae from bulk samples for transmission electron microscopy (TEM) analysis has been possible in the focussed ion beam scanning electron microscope (FIB-SEM) for over 20 years via the in situ lift-out method. Lift-out offers a fast and site specific preparation method for TEM analysis, typically in the field of materials science. More recently it has been applied to a low-water content biological sample (Rubino 2012). This work presents the successful lift-out of high-water content lamellae, under cryogenic conditions (cryo-FIB lift-out) and using a nanomanipulator retaining its full range of motion, which are advances on the work previously done by Rubino (2012). Strategies are explored for maintaining cryogenic conditions, grid attachment using cryo-condensation of water and protection of the lamella when transferring to the TEM. © 2016 Wiley Periodicals, Inc.

Facile preparation of salivary extracellular vesicles for cancer proteomics

NASA Astrophysics Data System (ADS)

Sun, Yan; Xia, Zhijun; Shang, Zhi; Sun, Kaibo; Niu, Xiaomin; Qian, Liqiang; Fan, Liu-Yin; Cao, Cheng-Xi; Xiao, Hua

2016-04-01

Extracellular vesicles (EVs) are membrane surrounded structures released by cells, which have been increasingly recognized as mediators of intercellular communication. Recent reports indicate that EVs participate in important biological processes and could serve as potential source for cancer biomarkers. As an attractive EVs source with merit of non-invasiveness, human saliva is a unique medium for clinical diagnostics. Thus, we proposed a facile approach to prepare salivary extracellular vesicles (SEVs). Affinity chromatography column combined with filter system (ACCF) was developed to efficiently remove the high abundant proteins and viscous interferences of saliva. Protein profiling in the SEVs obtained by this strategy was compared with conventional centrifugation method, which demonstrated that about 70% more SEVs proteins could be revealed. To explore its utility for cancer proteomics, we analyzed the proteome of SEVs in lung cancer patients and normal controls. Shotgun proteomic analysis illustrated that 113 and 95 proteins have been identified in cancer group and control group, respectively. Among those 63 proteins that have been consistently discovered only in cancer group, 12 proteins are lung cancer related. Our results demonstrated that SEVs prepared through the developed strategy are valuable samples for proteomics and could serve as a promising liquid biopsy for cancer.

S100B Protein concentration in milk-formulas for preterm and term infants. Correlation with industrial preparation procedures.

PubMed

Nigro, Francesco; Gagliardi, Luigi; Ciotti, Sabina; Galvano, Fabio; Pietri, Amedeo; Tina, Gabriella Lucia; Cavallaro, Daniela; La Fauci, Luca; Iacopino, Leonardo; Bognanno, Matteo; Li Volti, Giovanni; Scacco, Antonio; Michetti, Fabrizio; Gazzolo, Diego

2008-05-01

Human milk S100B protein possesses important neurotrophic properties. However, in some conditions human milk is substituted by milk formulas. The aims of the present study were: to assess S100B concentrations in milk formulas, to verify any differences in S100B levels between preterm and term infant formulas and to evaluate the impact of industrial preparation at predetermined phases on S100B content. Two different set of samples were tested: (i) commercial preterm (n = 36) and term (n = 36) infant milk formulas; ii) milk preterm (n = 10) and term infant (n = 10) formulas sampled at the following predetermined industrial preparation time points: skimmed cow milk (Time 0); after protein sources supplementation (Time 1); after pasteurization (Time 2); after spray-drying (Time 3). Our results showed that S100B concentration in preterm formulas were higher than in term ones (p < 0.01). In addition, S100B concentrations during industrial preparation showed a significant increase (p < 0.001) at Time 1 followed by a slight decrease (p > 0.05) at Time 2, whereas a significant (p < 0.001) dip was observed at Time 3. In conclusion, S100B showed a sufficient thermostability to resist pasteurization but not spry-drying. New feeding strategies in preterm and term infants are therefore warranted in order to preserve S100B protein during industrial preparation.

Comparison of strategies for the isolation of PCR-compatible, genomic DNA from a municipal biogas plants.

PubMed

Weiss, Agnes; Jérôme, Valérie; Freitag, Ruth

2007-06-15

The goal of the project was the extraction of PCR-compatible genomic DNA representative of the entire microbial community from municipal biogas plant samples (mash, bioreactor content, process water, liquid fertilizer). For the initial isolation of representative DNA from the respective lysates, methods were used that employed adsorption, extraction, or precipitation to specifically enrich the DNA. Since no dedicated method for biogas plant samples was available, preference was given to kits/methods suited to samples that resembled either the bioreactor feed, e.g. foodstuffs, or those intended for environmental samples including wastewater. None of the methods succeeded in preparing DNA that was directly PCR-compatible. Instead the DNA was found to still contain considerable amounts of difficult-to-remove enzyme inhibitors (presumably humic acids) that hindered the PCR reaction. Based on the isolation method that gave the highest yield/purity for all sample types, subsequent purification was attempted by agarose gel electrophoresis followed by electroelution, spermine precipitation, or dialysis through nitrocellulose membrane. A combination of phenol/chloroform extraction followed by purification via dialysis constituted the most efficient sample treatment. When such DNA preparations were diluted 1:100 they did no longer inhibit PCR reactions, while they still contained sufficient genomic DNA to allow specific amplification of specific target sequences.

Preparation of genomic DNA from a single species of uncultured magnetotactic bacterium by multiple-displacement amplification.

PubMed

Arakaki, Atsushi; Shibusawa, Mie; Hosokawa, Masahito; Matsunaga, Tadashi

2010-03-01

Magnetotactic bacteria comprise a phylogenetically diverse group that is capable of synthesizing intracellular magnetic particles. Although various morphotypes of magnetotactic bacteria have been observed in the environment, bacterial strains available in pure culture are currently limited to a few genera due to difficulties in their enrichment and cultivation. In order to obtain genetic information from uncultured magnetotactic bacteria, a genome preparation method that involves magnetic separation of cells, flow cytometry, and multiple displacement amplification (MDA) using phi29 polymerase was used in this study. The conditions for the MDA reaction using samples containing 1 to 100 cells were evaluated using a pure-culture magnetotactic bacterium, "Magnetospirillum magneticum AMB-1," whose complete genome sequence is available. Uniform gene amplification was confirmed by quantitative PCR (Q-PCR) when 100 cells were used as a template. This method was then applied for genome preparation of uncultured magnetotactic bacteria from complex bacterial communities in an aquatic environment. A sample containing 100 cells of the uncultured magnetotactic coccus was prepared by magnetic cell separation and flow cytometry and used as an MDA template. 16S rRNA sequence analysis of the MDA product from these 100 cells revealed that the amplified genomic DNA was from a single species of magnetotactic bacterium that was phylogenetically affiliated with magnetotactic cocci in the Alphaproteobacteria. The combined use of magnetic separation, flow cytometry, and MDA provides a new strategy to access individual genetic information from magnetotactic bacteria in environmental samples.

Millennial Students' Preferred Methods for Learning Concepts in Psychiatric Nursing.

PubMed

Garwood, Janet K

2015-09-01

The current longitudinal, descriptive, and correlational study explored which traditional teaching strategies can engage Millennial students and adequately prepare them for the ultimate test of nursing competence: the National Council Licensure Examination. The study comprised a convenience sample of 40 baccalaureate nursing students enrolled in a psychiatric nursing course. The students were exposed to a variety of traditional (e.g., PowerPoint(®)-guided lectures) and nontraditional (e.g., concept maps, group activities) teaching and learning strategies, and rated their effectiveness. The students' scores on the final examination demonstrated that student learning outcomes met or exceeded national benchmarks. Copyright 2015, SLACK Incorporated.

Fabric phase sorptive extraction followed by UHPLC-MS/MS for the analysis of benzotriazole UV stabilizers in sewage samples.

PubMed

Montesdeoca-Esponda, Sarah; Sosa-Ferrera, Zoraida; Kabir, Abuzar; Furton, Kenneth G; Santana-Rodríguez, José Juan

2015-10-01

A fast and sensitive sample preparation strategy using fabric phase sorptive extraction followed by ultra-high-performance liquid chromatography and tandem mass spectrometry detection has been developed to analyse benzotriazole UV stabilizer compounds in aqueous samples. Benzotriazole UV stabilizer compounds are a group of compounds added to sunscreens and other personal care products which may present detrimental effects to aquatic ecosystems. Fabric phase sorptive extraction is a novel solvent minimized sample preparation approach that integrates the advantages of sol-gel derived hybrid inorganic-organic nanocomposite sorbents and the flexible, permeable and hydrophobic surface chemistry of polyester fabric. It is a highly sensitive, fast, efficient and inexpensive device that can be reused and does not suffer from coating damage, unlike SPME fibres or stir bars. In this paper, we optimized the extraction of seven benzotriazole UV filters evaluating the majority of the parameters involved in the extraction process, such as sorbent chemistry selection, extraction time, back-extraction solvent, back-extraction time and the impact of ionic strength. Under the optimized conditions, fabric phase sorptive extraction allows enrichment factors of 10 times with detection limits ranging from 6.01 to 60.7 ng L(-1) and intra- and inter-day % RSDs lower than 11 and 30 % for all compounds, respectively. The optimized sample preparation technique followed by ultra-high-performance liquid chromatography and tandem mass spectrometry detection was applied to determine the target analytes in sewage samples from wastewater treatment plants with different purification processes of Gran Canaria Island (Spain). Two UV stabilizer compounds were measured in ranges 17.0-60.5 ng mL(-1) (UV 328) and 69.3-99.2 ng mL(-1) (UV 360) in the three sewage water samples analysed.

Preparation of hydrophilic interaction/ion-exchange mixed-mode chromatographic stationary phase with adjustable selectivity by controlling different ratios of the co-monomers.

PubMed

Bo, Chunmiao; Wang, Xiaomeng; Wang, Chaozhan; Wei, Yinmao

2017-03-03

Development of mixed-mode chromatography (MMC) stationary phase with adjustable selectivity is beneficial to meet the needs of complex samples. In this work, surface-initiated atom transfer radical polymerization (SI-ATRP) using the mixture of two functional monomers was proposed as a new preparation strategy for MMC stationary phase with adjustable selectivity. The mixture of sodium 4-styrenesulfonate (NASS) and dimethylaminoethyl methacrylate (DMAEMA) underwent SI-ATRP to bond poly(NASS-co-DMAEMA) on the surface of silica to prepare hydrophilic interaction/ion-exchange mixed-mode stationary phase. Various analytes (neutral, acidic, basic analytes and strong polar nucleosides) were employed to investigate the retention behaviors. The influences of water content and pH of the mobile phase on the retention validated the mixed-mode retention mechanisms of HILIC and ion-exchange. The charge and polarity of stationary phase as well as the separation selectivity were conveniently manipulated by the ratio of NASS to DMAEMA monomer, and the use of DMAEMA in the mixture additionally endowed the column with the temperature-responsive characteristics. Moreover, the application of the developed column was demonstrated by the successful separation of nucleosides, β-agonists and safflower injection. In a word, the proposed strategy can be potentially applied in the controllable preparation of MMC stationary phase with adjustable selectivity. Copyright © 2017 Elsevier B.V. All rights reserved.

Standard operating procedures for collection of soil and sediment samples for the Sediment-bound Contaminant Resiliency and Response (SCoRR) strategy pilot study

USGS Publications Warehouse

Fisher, Shawn C.; Reilly, Timothy J.; Jones, Daniel K.; Benzel, William M.; Griffin, Dale W.; Loftin, Keith A.; Iwanowicz, Luke R.; Cohl, Jonathan A.

2015-12-17

An understanding of the effects on human and ecological health brought by major coastal storms or flooding events is typically limited because of a lack of regionally consistent baseline and trends data in locations proximal to potential contaminant sources and mitigation activities, sensitive ecosystems, and recreational facilities where exposures are probable. In an attempt to close this gap, the U.S. Geological Survey (USGS) has implemented the Sediment-bound Contaminant Resiliency and Response (SCoRR) strategy pilot study to collect regional sediment-quality data prior to and in response to future coastal storms. The standard operating procedure (SOP) detailed in this document serves as the sample-collection protocol for the SCoRR strategy by providing step-by-step instructions for site preparation, sample collection and processing, and shipping of soil and surficial sediment (for example, bed sediment, marsh sediment, or beach material). The objectives of the SCoRR strategy pilot study are (1) to create a baseline of soil-, sand-, marsh sediment-, and bed-sediment-quality data from sites located in the coastal counties from Maine to Virginia based on their potential risk of being contaminated in the event of a major coastal storm or flooding (defined as Resiliency mode); and (2) respond to major coastal storms and flooding by reoccupying select baseline sites and sampling within days of the event (defined as Response mode). For both modes, samples are collected in a consistent manner to minimize bias and maximize quality control by ensuring that all sampling personnel across the region collect, document, and process soil and sediment samples following the procedures outlined in this SOP. Samples are analyzed using four USGS-developed screening methods—inorganic geochemistry, organic geochemistry, pathogens, and biological assays—which are also outlined in this SOP. Because the SCoRR strategy employs a multi-metric approach for sample analyses, this protocol expands upon and reconciles differences in the sample collection protocols outlined in the USGS “National Field Manual for the Collection of Water-Quality Data,” which should be used in conjunction with this SOP. A new data entry and sample tracking system also is presented to ensure all relevant data and metadata are gathered at the sample locations and in the laboratories.

Bismuth-based oxide semiconductors: Mild synthesis and practical applications

NASA Astrophysics Data System (ADS)

Timmaji, Hari Krishna

In this dissertation study, bismuth based oxide semiconductors were prepared using 'mild' synthesis techniques---electrodeposition and solution combustion synthesis. Potential environmental remediation and solar energy applications of the prepared oxides were evaluated. Bismuth vanadate (BiVO4) was prepared by electrodeposition and solution combustion synthesis. A two step electrosynthesis strategy was developed and demonstrated for the first time. In the first step, a Bi film was first electrodeposited on a Pt substrate from an acidic BiCl3 medium. Then, this film was anodically stripped in a medium containing hydrolyzed vanadium precursor, to generate Bi3+, and subsequent BiVO4 formation by in situ precipitation. The photoelectrochemical data were consistent with the in situ formation of n-type semiconductor films. In the solution combustion synthesis procedure, BiVO4 powders were prepared using bismuth nitrate pentahydrate as the bismuth precursor and either vanadium chloride or vanadium oxysulfate as the vanadium precursor. Urea, glycine, or citric acid was used as the fuel. The effect of the vanadium precursor on the photocatalytic activity of combustion synthesized BiVO 4 was evaluated in this study. Methyl orange was used as a probe to test the photocatalytic attributes of the combustion synthesized (CS) samples, and benchmarked against a commercial bismuth vanadate sample. The CS samples showed superior activity to the commercial benchmark sample, and samples derived from vanadium chloride were superior to vanadium oxysulfate counterparts. The photoelectrochemical properties of the various CS samples were also studied and these samples were shown to be useful both for environmental photocatalytic remediation and water photooxidation applications. Silver bismuth tungstate (AgBiW2O8) nanoparticles were prepared for the first time by solution combustion synthesis by using silver nitrate, bismuth nitrate, sodium tungstate as precursors for Ag, Bi, and W respectively and urea as the fuel. The photocatalytic activity of these nanoparticles was superior to a sample prepared by solid-state synthesis. The combustion-synthesized particles were subsequently modified with Pt catalyst islands using a photodeposition technique and then used for the photo-generation of syngas (CO + H2). Formic acid was used in these experiments for in situ generation of CO2 and its subsequent reduction to CO. In the absence of Pt modification, H2 was not obtained. These results were compared with those obtained with acetic acid in place of formic acid, and finally the mechanistic pathways for syngas and methane photogeneration are presented.

Nuclear Strategy and World Order: The United States Imperative.

ERIC Educational Resources Information Center

Beres, Louis Rene

The current U.S. nuclear strategy goes beyond the legitimate objective of survivable strategic forces to active preparation for nuclear war. The Reagan administration strategy rejects minimum deterrence and prepares for a nuclear war that might be protracted and controlled. The strategy reflects the understanding that a combination of counterforce…

The Factor Structure and Psychometric Properties of the Persian Version of the Revised Prenatal Coping Inventory (Nu-PCI).

PubMed

Faramarzi, Mahbobeh; Pasha, Hajar; Khafri, Sorayya; Heidary, Shima

2017-03-01

Familiarity with coping strategies is essential for stress management during pregnancy. The Revised Prenatal Coping Inventory (Nu-PCI) was developed to assess coping strategies during pregnancy. This study aimed to assess the factor structure and psychometric properties of the Persian version of the Nu-PCI. After forward-backward translation, the Nu-PCI was administered to 210 pregnant women who were enrolled in two teaching referral clinics in the North of the Islamic Republic of Iran (Babol). The participants completed the Persian Nu-PCI and Ways of Coping Questionnaire (WCQ), which was used to determine the validity of the Persian Nu-PCI. To test construct validity of the Persian Nu-PCI, a principal components factor analysis was performed. Principal components analysis with varimax rotation showed a best fitting 3-factor structure similar to the original with three coping subscales: planning-preparation, avoidance, and spiritual-positive coping. The Persian Nu-PCI was internally consistent and within the acceptable range (α=0.89-0.97). The alpha coefficients for the Nu-PCI and the subscales of planning-preparation, avoidance, and spiritual-positive coping were high. Test-retest coefficients for the Nu-PCI and subscales were 0.98-0.99. The Nu-PCI and its subscales correlated with the WCQ in the entire sample and within each trimester. The Persian version of the Nu-PCI and the subscales of planning-preparation, avoidance, and spiritual-positive coping represent the first reliable standardized tool for measuring coping strategies during pregnancy in the Islamic Republic of Iran. Therefore, it can be applied as a quick and accurate preliminary screening tool for evaluating coping strategies throughout pregnancy in clinics and other medical and research settings.

Automated acoustic matrix deposition for MALDI sample preparation.

PubMed

Aerni, Hans-Rudolf; Cornett, Dale S; Caprioli, Richard M

2006-02-01

Novel high-throughput sample preparation strategies for MALDI imaging mass spectrometry (IMS) and profiling are presented. An acoustic reagent multispotter was developed to provide improved reproducibility for depositing matrix onto a sample surface, for example, such as a tissue section. The unique design of the acoustic droplet ejector and its optimization for depositing matrix solution are discussed. Since it does not contain a capillary or nozzle for fluid ejection, issues with clogging of these orifices are avoided. Automated matrix deposition provides better control of conditions affecting protein extraction and matrix crystallization with the ability to deposit matrix accurately onto small surface features. For tissue sections, matrix spots of 180-200 microm in diameter were obtained and a procedure is described for generating coordinate files readable by a mass spectrometer to permit automated profile acquisition. Mass spectral quality and reproducibility was found to be better than that obtained with manual pipet spotting. The instrument can also deposit matrix spots in a dense array pattern so that, after analysis in a mass spectrometer, two-dimensional ion images may be constructed. Example ion images from a mouse brain are presented.

Histamine monolith versatility to purify supercoiled plasmid deoxyribonucleic acid from Escherichia coli lysate.

PubMed

Sousa, A; Almeida, A M; Černigoj, U; Sousa, F; Queiroz, J A

2014-08-15

Preparation of high quantities of supercoiled plasmid DNA of pharmaceutical grade purity is a research area where intensive investigation is being performed. From this standpoint, several downstream methods have been proposed, among them the monolithic chromatographic strategies owing to excellent mass transfer properties of monolithic supports and their high binding capacity for large biomolecules. The present study explores the physicochemical properties of histamine ligand in a supercoiled plasmid DNA purification process from an Escherichia coli clarified lysate, where the emphasis is given to the elution strategy that allows higher selectivity and efficient removal of other impurities besides the open circular isoform. The combination of high NaCl concentration and acidic pH allowed the elimination of 89% of RNA during the preparative loading of the lysate sample. The results of the purification strategy with ascending sodium chloride gradient revealed that 97% of supercoiled plasmid DNA was recovered with a purity degree of 99%. In addition, using a combined purification strategy with ascending sodium chloride (capture step) and then descending ammonium sulfate (polishing step) gradient, it was achieved a lower supercoiled plasmid DNA recovery yield of 79% with a purity degree of 92%, although the dynamic binding capacity under these conditions was higher than in the previous strategy. A significant reduction of host contents, such as proteins, RNA and genomic DNA, was obtained in both purification strategies. Accordingly, histamine is a useful and versatile ligand that allows the desirable supercoiled plasmid purification with high yield and purity level. Copyright © 2014. Published by Elsevier B.V.

Preparation of Protein Samples for NMR Structure, Function, and Small Molecule Screening Studies

PubMed Central

Acton, Thomas B.; Xiao, Rong; Anderson, Stephen; Aramini, James; Buchwald, William A.; Ciccosanti, Colleen; Conover, Ken; Everett, John; Hamilton, Keith; Huang, Yuanpeng Janet; Janjua, Haleema; Kornhaber, Gregory; Lau, Jessica; Lee, Dong Yup; Liu, Gaohua; Maglaqui, Melissa; Ma, Lichung; Mao, Lei; Patel, Dayaban; Rossi, Paolo; Sahdev, Seema; Shastry, Ritu; Swapna, G.V.T.; Tang, Yeufeng; Tong, Saichiu; Wang, Dongyan; Wang, Huang; Zhao, Li; Montelione, Gaetano T.

2014-01-01

In this chapter, we concentrate on the production of high quality protein samples for NMR studies. In particular, we provide an in-depth description of recent advances in the production of NMR samples and their synergistic use with recent advancements in NMR hardware. We describe the protein production platform of the Northeast Structural Genomics Consortium, and outline our high-throughput strategies for producing high quality protein samples for nuclear magnetic resonance (NMR) studies. Our strategy is based on the cloning, expression and purification of 6X-His-tagged proteins using T7-based Escherichia coli systems and isotope enrichment in minimal media. We describe 96-well ligation-independent cloning and analytical expression systems, parallel preparative scale fermentation, and high-throughput purification protocols. The 6X-His affinity tag allows for a similar two-step purification procedure implemented in a parallel high-throughput fashion that routinely results in purity levels sufficient for NMR studies (> 97% homogeneity). Using this platform, the protein open reading frames of over 17,500 different targeted proteins (or domains) have been cloned as over 28,000 constructs. Nearly 5,000 of these proteins have been purified to homogeneity in tens of milligram quantities (see Summary Statistics, http://nesg.org/statistics.html), resulting in more than 950 new protein structures, including more than 400 NMR structures, deposited in the Protein Data Bank. The Northeast Structural Genomics Consortium pipeline has been effective in producing protein samples of both prokaryotic and eukaryotic origin. Although this paper describes our entire pipeline for producing isotope-enriched protein samples, it focuses on the major updates introduced during the last 5 years (Phase 2 of the National Institute of General Medical Sciences Protein Structure Initiative). Our advanced automated and/or parallel cloning, expression, purification, and biophysical screening technologies are suitable for implementation in a large individual laboratory or by a small group of collaborating investigators for structural biology, functional proteomics, ligand screening and structural genomics research. PMID:21371586

The economic value of transportation energy contingency planning: An objective model for analyzing the economics of domestic renewable energy for supply augmentation

NASA Astrophysics Data System (ADS)

Shaten, Richard Jay

1998-12-01

Petroleum provides 90% of transportation energy needs. Domestic production is decreasing and global demand is increasing. Risk of escalating prices and supply interruptions are compounded by environmental and military externalities and lost opportunities from the failure to develop alternative domestic resources. Within the context of "energy contingency planning" municipalities should evaluate crisis mitigation strategies. Supply augmentation using domestic renewable fuels is proposed to avert future financial liabilities. A method for calculating the economic value of this strategy is demonstrated. An objective function and associated constraints represent the cost of preparing for each of three possible scenarios: status quo, inflationary and crisis. Constraints ensure that municipal fuel needs are met. Environmental costs may be included. Optimal solutions determine the fuel supply mix for each scenario. A 3 x 3 matrix presents the range of actual costs resulting from preparing for each scenario and subsequent three possible outcomes. The distribution of probabilities of the outcomes is applied to the cost matrix and an "expected value" of preparing for each scenario is calculated. An unanticipated crisis outcome results in. The expected value of the cost of preparing for a crisis is cast as an insurance premium against potential economic liability. Policy makers accept the crisis preparation fuel mix if: (a) they agree with the calculated penalty cost, or (b) they accept the burden of the insurance premium. Green Bay Wisconsin was chosen as a sample municipality. Results show that a perceived 10% chance of crisis requires an annual tax of 4.00 per household to avert economic impacts of 50 million. At a perceived 50% chance of crisis preparing for the crisis would begin to save the municipality money.

Automated Microbial Metabolism Laboratory

NASA Technical Reports Server (NTRS)

1973-01-01

Development of the automated microbial metabolism laboratory (AMML) concept is reported. The focus of effort of AMML was on the advanced labeled release experiment. Labeled substrates, inhibitors, and temperatures were investigated to establish a comparative biochemical profile. Profiles at three time intervals on soil and pure cultures of bacteria isolated from soil were prepared to establish a complete library. The development of a strategy for the return of a soil sample from Mars is also reported.

Strategies Chosen by YMSM during Goal Setting to Reduce Risk for HIV & Other STIs: Results from the Keep It Up! 2.0 Prevention Trial

PubMed Central

Motley, Darnell N.; Hammond, Sydney; Mustanski, Brian

2018-01-01

Although there have been great advances in the prevention of HIV in the last two decades, young men who have sex with men (YMSM) continue to be disproportionately impacted. Utilizing qualitative data from a sample of YMSM (N = 292) engaged in a randomized controlled trial testing the efficacy of an internet-based HIV prevention program, we examined YMSM’s goals for sexual risk reduction. Goals tended to focus on strategies used to prepare for safer sex or strategies to be used during sex. In both areas, five categories of strategies were identified: skill-related, intrapersonal, social, contextual, and instrumental. Findings suggest opportunities for more tailored eHealth intervention by focusing on strategies in domains of most use to the individual. Future research should include longitudinal assessment of barriers and facilitators to goal adherence, utility of goals in increasing safer sex behaviors, and changes to goals over time. PMID:28195780

Strategies Chosen by YMSM During Goal Setting to Reduce Risk for HIV and Other Sexually Transmitted Infections: Results From the Keep It Up! 2.0 Prevention Trial.

PubMed

Motley, Darnell N; Hammond, Sydney; Mustanski, Brian

2017-02-01

Although there have been great advances in the prevention of HIV in the last two decades, young men who have sex with men (YMSM) continue to be disproportionately impacted. Utilizing qualitative data from a sample of YMSM (N = 292) engaged in a randomized controlled trial testing the efficacy of an internet-based HIV prevention program, we examined YMSM's goals for sexual risk reduction. Goals tended to focus on strategies used to prepare for safer sex or strategies to be used during sex. In both areas, five categories of strategies were identified: skill-related, intrapersonal, social, contextual, and instrumental. Findings suggest opportunities for more tailored eHealth intervention by focusing on strategies in domains of most use to the individual. Future research should include longitudinal assessment of barriers and facilitators to goal adherence, utility of goals in increasing safer sex behaviors, and changes to goals over time.

Inductively coupled plasma optical emission spectrometry for trace multi-element determination in vegetable oils, margarine and butter after stabilization with propan-1-ol and water

NASA Astrophysics Data System (ADS)

de Souza, Roseli M.; Mathias, Bárbara M.; da Silveira, Carmem Lúcia P.; Aucélio, Ricardo Q.

2005-06-01

The quantitative evaluation of trace elements in foodstuffs is of considerable interest due to the potential toxicity of many elements, and because the presence of some metallic species might affect the overall quality (flavor and stability) of these products. In the present work, an inductively coupled plasma optical emission spectrometric method has been developed for the determination of six elements (Cd, Co, Cr, Cu, Ni and Mn) in olive oil, soy oil, margarine and butter. Organic samples (oils and fats) were stabilized using propan-1-ol and water, which enabled long-time sample dispersion in the solution. This simple sample preparation procedure, together with an efficient sample introduction strategy (using a Meinhard K3 nebulizer and a twister cyclonic spray chamber), facilitated the overall analytical procedure, allowing quantification using calibration curves prepared with inorganic standards. Internal standardization (Sc) was used for correction of matrix effects and signal fluctuations. Good sensitivities with limits of detection in the ng g -1 range were achieved for all six elements. These sensitivities were appropriate for the intended application. The method was tested through the analysis of laboratory-fortified samples with good recoveries (between 91.3% and 105.5%).

The effect of preparation strategies, qualification and professional background on clinical nurse educator confidence.

PubMed

Nguyen, Van N B; Forbes, Helen; Mohebbi, Mohammadreza; Duke, Maxine

2018-06-12

To describe how clinical nurse educators in Vietnam are prepared for their role; to identify which preparation strategies assist development of confidence in clinical teaching; and to measure the effect of educational qualifications and professional background on perceived confidence levels. The quality of clinical teaching can directly affect the quality of the student learning experience. The role of the clinical educator is complex and dynamic and requires a period of adjustment for successful role transition to occur. Planned orientation and specific preparation programs assist transition and reduce anxiety for new clinical nurse educators. There is, however, a lack of clear evidence to identify the form this preparation should take or which strategies are likely to facilitate the development of role confidence. Descriptive survey study. Cross-sectional surveys were used to collect data from 334 clinical nurse educators during January - March 2015. Eight preparation methods commonly used in Vietnam were identified. There was a small yet significant association between preparation and clinical nurse educators' perceived confidence. Formal preparation methods, as well as postgraduate qualifications and years of clinical teaching experience were linked to increased confidence in clinical teaching. Conversely, informal mentorship was found to hinder confidence development. This study identifies several preparation strategies that significantly enhance clinical educator confidence and readiness for their complex role. These preparation strategies drawn from the Vietnamese context, provide important examples for the wider nursing community to consider. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Effect of different bleaching strategies on microhardness of a silorane-based composite resin.

PubMed

Bahari, Mahmoud; Savadi Oskoee, Siavash; Mohammadi, Narmin; Ebrahimi Chaharom, Mohammad Esmaeel; Godrati, Mostafa; Savadi Oskoee, Ayda

2016-01-01

Background. Dentists' awareness of the effects of bleaching agents on the surface and mechanical properties of restorative materials is of utmost importance. Therefore, this in vitro study was undertaken to investigate the effects of different bleaching strategies on the microhardness of a silorane-based composite resin. Methods. Eighty samples of a silorane-based composite resin (measuring 4 mm in diameter and 2 mm in thickness) were prepared within acrylic molds. The samples were polished and randomly assigned to 4 groups (n=20). Group 1 (controls) were stored in distilled water for 2 weeks. The samples in group 2 underwent a bleaching procedure with 15% carbamide peroxide for two weeks two hours daily. The samples in group 3 were bleached with 35% hydrogen peroxide twice 5 days apart for 30 minutes each time. The samples in group 4 underwent a bleaching procedure with light-activated 35% hydrogen peroxide under LED light once for 40 minutes. Then the microhardness of the samples was determined using Vickers method. Data were analyzed with one-way ANOVA and post hoc Tukey tests (P < 0.05). Results. All the bleaching agents significantly decreased microhardness compared to the control group (P < 0.05). In addition, there were significant differences in microhardness between groups 2 and 4 (P = 0.001) and between groups 3 and 4 (P<0.001). However, no significant differences were detected in microhardness between groups 2 and 3 (P > 0.05). Conclusion. Bleaching agents decreased microhardness of silorane-based composite resin restorations, the magnitude of which depending on the bleaching strategy used.

Anti-icing property of bio-inspired micro-structure superhydrophobic surfaces and heat transfer model

NASA Astrophysics Data System (ADS)

Liu, Yan; Li, Xinlin; Jin, Jingfu; Liu, Jiaan; Yan, Yuying; Han, Zhiwu; Ren, Luquan

2017-04-01

Ice accumulation is a thorny problem which may inflict serious damage even disasters in many areas, such as aircraft, power line maintenance, offshore oil platform and locators of ships. Recent researches have shed light on some promising bio-inspired anti-icing strategies to solve this problem. Inspired by typical plant surfaces with super-hydrophobic character such as lotus leaves and rose petals, structured superhydrophobic surface are prepared to discuss the anti-icing property. 7075 Al alloy, an extensively used materials in aircrafts and marine vessels, is employed as the substrates. As-prepared surfaces are acquired by laser processing after being modified by stearic acid for 1 h at room temperature. The surface morphology, chemical composition and wettability are characterized by means of SEM, XPS, Fourier transform infrared (FTIR) spectroscopy and contact angle measurements. The morphologies of structured as-prepared samples include round hump, square protuberance and mountain-range-like structure, and that the as-prepared structured surfaces shows an excellent superhydrophobic property with a WCA as high as 166 ± 2°. Furthermore, the anti-icing property of as-prepared surfaces was tested by a self-established apparatus, and the crystallization process of a cooling water on the sample was recorded. More importantly, we introduced a model to analyze heat transfer process between the droplet and the structured surfaces. This study offers an insight into understanding the heat transfer process of the superhydrophobic surface, so as to further research about its unique property against ice accumulation.

Safety in the preparation of cytotoxic drugs: How to integrate gravimetric control in the quality assurance policy?

PubMed

Lecordier, J; Heluin, Y; Plivard, C; Bureau, A; Mouawad, C; Chaillot, B; Lahet, J-J

2011-02-01

We present the way to integrate gravimetric control (GC) in a centralized preparation of cytotoxic drugs unit. Two different modalities are described. In the first strategy, the balance is located inside the isolator, whereas in the second, it is located outside in order to remove many technical and ergonomic constraints. These two modalities are compared in terms of benefits and limits. GC consists in comparing the observed weight variation with the expected weight variation using a precision balance. According to the B-in strategy, this variation is directly attributable to the weight of the cytotoxic solution injected, whereas with the B-out strategy, the weight of various additional components must be taken into account. Five hundred and seventy-seven preparations have been weighed. For "B-in" strategy, the 95% confidence interval is [1.02-1.14%] and every preparation is below the threshold of 5%. For "B-out" strategy, the 95% confidence interval is [2.34-2.63%] and 94% of preparations are below the threshold of 5%. B-in strategy is distinctly more precise than B-out strategy and can be applied to all preparations. However, B-out strategy is a feasible option in practice and enables the detection of an important mistake. All in all, results obtained from B-out strategy can be considered as a quality indicator in the production line. Results of GC are helpful in the final step of release, which the pharmacist is responsible for. Many contributions in the quality assurance policy could justify using of GC in every unit. Copyright © 2011 Elsevier Masson SAS. All rights reserved.

Hydrogen Exchange During Cell-Free Incorporation of Deuterated Amino Acids and an Approach to its Inhibition

PubMed Central

Tonelli, M.; Singarapu, K. K.; Markley, J. L.; Makino, S.; Sahu, S .C.; Matsubara, Y.; Endo, Y.; Kainosho, M.

2012-01-01

Perdeuteration, selective deuteration, and stereo array isotope labeling (SAIL) are valuable strategies for NMR studies of larger proteins and membrane proteins. To minimize scrambling of the label, it is best to use cell-free methods to prepare selectively labeled proteins. However, when proteins are prepared from deuterated amino acids by cell-free translation in H2O, exchange reactions can lead to contamination of 2H sites by 1H from the solvent. Examination of a sample of SAIL-chlorella ubiquitin prepared by Escherichia coli cell-free synthesis revealed that exchange had occurred at several residues (mainly at Gly, Ala, Asp, Asn, Glu, and Gln). We present results from a study aimed at identifying the exchanging sites and level of exchange and at testing a strategy for minimizing 1H contamination during wheat germ cell-free translation of proteins produced from deuterated amino acids by adding known inhibitors of transaminases (1 mM aminooxyacetic acid) and glutamate synthetase (0.1 mM L-methionine sulfoximine). By using a wheat germ cell-free expression system, we produced [U-2H,15N]-chlorella ubiquitin without and with added inhibitors, and [U-15N]-chlorella ubiquitin as a reference to determine the extent of deuterium incorporation. We also prepared a sample of [U-13C,15N]-chlorella ubiquitin, for use in assigning the sites of exchange. The added inhibitors did not reduce the protein yield and were successful in blocking hydrogen exchange at Cα sites with the exception of Gly. We discovered, in addition, that partial exchange occurred with or without the inhibitors at certain side-chain methyl and methylene groups: Ala-Hβ, Asn-Hβ, Asp-Hβ, Gln-Hγ, Glu-Hγ, and Lys-Hε. The side-chain labeling pattern, in particular the mixed chiral labeling resulting from partial exchange at certain sites, should be of interest in studies of large proteins, protein complexes, and membrane proteins. PMID:21984356

Relative costs of anesthesiologist prepared, hospital pharmacy prepared and outsourced anesthesia drugs.

PubMed

Jelacic, Srdjan; Craddick, Karen; Nair, Bala G; Bounthavong, Mark; Yeung, Kai; Kusulos, Dolly; Knutson, Jennifer A; Somani, Shabir; Bowdle, Andrew

2017-02-01

Anesthesia drugs can be prepared by anesthesia providers, hospital pharmacies or outsourcing facilities. The decision whether to outsource all or some anesthesia drugs is challenging since the costs associated with different anesthesia drug preparation methods remain poorly described. The costs associated with preparation of 8 commonly used anesthesia drugs were analyzed using a budget impact analysis for 4 different syringe preparation strategies: (1) all drugs prepared by anesthesiologist, (2) drugs prepared by anesthesiologist and hospital pharmacy, (3) drugs prepared by anesthesiologist and outsourcing facility, and (4) all drugs prepared by outsourcing facility. A strategy combining anesthesiologist and hospital pharmacy prepared drugs was associated with the lowest estimated annual cost in the base-case budget impact analysis with an annual cost of $225 592, which was lower than other strategies by a margin of greater than $86 000. A combination of anesthesiologist and hospital pharmacy prepared drugs resulted in the lowest annual cost in the budget impact analysis. However, the cost of drugs prepared by an outsourcing facility maybe lower if the capital investment needed for the establishment and maintenance of the US Pharmacopeial Convention Chapter <797> compliant facility is included in the budget impact analysis. Copyright © 2016 Elsevier Inc. All rights reserved.

Preliminary evaluation of a coping strategy enhancement method of preparation for labour.

PubMed

Escott, Diane; Slade, Pauline; Spiby, Helen; Fraser, Robert B

2005-09-01

To compare the use and effects of enhanced pre-existing coping strategies with the use and effects of coping strategies usually taught in National Health Service (NHS) antenatal education on women's experience of pain and emotions during labour. A between-group comparison of women who chose to attend NHS antenatal education where courses of preparation were randomly assigned to include either a new method of coping strategy enhancement (CSE) or standard taught coping strategies. Two large maternity units in one city in the North of England. 20 women participated in antenatal classes incorporating the CSE method and 21 women participated in antenatal classes incorporating the standard approach to developing coping strategies for labour. Women who attended CSE classes used enhanced coping strategies for a larger proportion of their labour than women who attended standard classes who used taught coping strategies. Birth companions were more involved in women's use of enhanced than taught strategies. Self-efficacy for use of coping strategies and subsequent experiences of pain and emotions during labour were equivalent between groups. An approach based on enhancing pre-existing coping strategies was associated with greater coping strategy use and involvement from the birth companion, and provided benefits to women's overall experience of labour at least equivalent to that associated with standard preparation. Further research should explore this novel approach in larger groups, and for women who may choose not to attend group antenatal preparation.

A novel colorimetric method based on copper nanoclusters with intrinsic peroxidase-like for detecting xanthine in serum samples

NASA Astrophysics Data System (ADS)

Yan, Zhengyu; Niu, Qianqian; Mou, Mingyao; Wu, Yi; Liu, Xiaoxuan; Liao, Shenghua

2017-07-01

A facile strategy for detecting xanthine in serum samples by copper nanocluster (CuNCs) with high intrinsic peroxidase-like activity was reported. Firstly, a simple, mild and time-saving method for preparing CuNCs was developed, in which dithiothreitol (DTT) and bovine serum albumin (BSA) were used as reductant and stabilizer, respectively. The as-prepared CuNCs exhibited a fluorescence emission at 590 nm with a quantum yield (QY) of approximately 5.29%, the fluorescence intensity of the as-prepared CuNCs exhibited no considerable change when stored under ambient condition with the lifetime is 1.75 μs. Moreover, the as-prepared CuNCs exhibited high intrinsic peroxidase-like activity with lower K m ( K m = 8.90 × 10-6 mol L-1) for H2O2, which indicated that CuNCs have a higher affinity for H2O2. Compared with natural enzyme, the as-synthesized CuNCs are more catalytic stable over a wide range of pH (4.0 13.0) and temperature (4 80 °C). Finally, an indirect method for sensing xanthine was established because xanthine oxidase can catalyse the oxidation of xanthine to produce H2O2. Xanthine could be detected as low as 3.8 × 10-7 mol L-1 with a linear range from 5.0 × 10-7 to 1.0 × 10-4 mol L-1. These results proved that the proposed method is sensitive and accurate and could be successfully applied to the determination of xanthine in the serum sample with satisfaction.

Determination of total phthalate in cosmetics using a simple three-phase sample preparation method.

PubMed

Liu, Laping; Wang, Zhengmeng; Zhao, Sihan; Duan, Jiahui; Tao, Hu; Wang, Wenji; Liu, Shuhui

2018-02-01

A simple sample preparation method requiring minimal organic solvents is proposed for the determination of the total phthalate content in cosmetics by high-performance liquid chromatography-tandem mass spectrometry. The hydrolysis of phthalates and purification of interfering substances were performed in a three-phase system that included an upper n-hexane phase, a middle ethanol phase, and a lower aqueous alkali solution. This three-phase system utilized an incremental purification strategy. The apolar ingredients were extracted with n-hexane, the polar pigments accumulated in the ethanol phase, and the hydrolysis product, phthalic acid, remained in the hydrolysate. Under the optimized conditions, the correlation coefficients (r) for the calibration curves were 0.998-0.999 in the range 0.60-12 mol L -1 . The limit of detection was 5.1 μmol kg -1 , and the limit of quantification was 9.2 μmol kg -1 . The recoveries varied from 84 to 97% with RSDs equal to or lower than 11%. The intra-day and inter-day repeatability values, expressed as the relative standard deviation, were less than 8.7 and 9.8, respectively. No obvious matrix effect existed in the different cosmetics matrices. The validated method was applied for the analysis of 57 commercial cosmetic samples. Graphical abstract Analysis of phthalates in cosmetics using a three-phase preparation method.

A target and nontarget strategy for identification or characterization of the chemical ingredients in Chinese herb preparation Shuang-Huang-Lian oral liquid by ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry.

PubMed

Zhang, Feng-Xiang; Li, Min; Yao, Zhi-Hong; Li, Chang; Qiao, Li-Rui; Shen, Xiu-Yu; Yu, Kate; Dai, Yi; Yao, Xin-Sheng

2018-03-01

A target and nontarget strategy based on in-house chemical components library was developed for rapid and comprehensive analysis of complicated components from traditional Chinese medicine preparation Shuang-Huang-Lian oral liquid. The sample was analyzed by ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry using generic acquisition parameters. Automated detection and data filtering were performed on the UNIFI™ software and the detected peaks were evaluated against an in-house library. As a result, a total of 170 chemical components (110 target compounds and 60 nontarget ones) were identified or tentatively characterized, including 54 flavonoids, 30 phenylethanoid glycosides, 16 iridoid glycosides, 14 lignans, 32 organic acids, 19 triterpenoid saponins and five other types of compounds. Among them, 44 compounds were further confirmed by comparison with reference standards. It was demonstrated that this systematical approach could be successfully applied for rapid identification of multiple compounds in traditional Chinese medicine and its preparations. Furthermore, this work established the foundation for the further investigation on the metabolic fates of multiple ingredients in Shuang-Huang-Lian oral liquid. Copyright © 2017 John Wiley & Sons, Ltd.

Struggling to be part of Swedish society: Strategies used by immigrants with late effects of polio.

PubMed

Santos Tavares Silva, Iolanda; Thorén-Jönsson, Anna-Lisa

2015-01-01

To explore and describe strategies in daily occupations among immigrants with late effects of polio. The strategies were explored by interviews with 12 immigrants from Eastern Africa with late effects of polio. Sampling and data analysis was carried out according to grounded theory. The participants struggled for occupational participation and normality in an effort to participate in, and be part of, society. The study identified 14 strategies used by the immigrants in their daily occupations. The strategies can be presented in the following four categories: managing physical capacity; promoting occupational performance; strategies for gaining respect; and preparing the ground for one's existence. The participants struggled to find a balance between physical capacity and meaningful occupations, conception of their own and others' norms and values, and living conditions in Swedish society. The strategies were related to the participants' will to manage daily occupations, maintain social relationships, and be part of society. The strategies revealed that the participants strive to participate in occupations and society. This study reinforces the importance of occupation for immigrants with disability. The results highlight the need for adequate health care and rehabilitation but should also alert other social institutions.

Chemical Speciation and Metallomics.

PubMed

de Jesus, Jemmyson Romário; da Costa, Luana Ferreira; Lehmann, Eraldo Luiz; Galazzi, Rodrigo Moretto; Madrid, Katherine Chacón; Arruda, Marco Aurélio Zezzi

2018-01-01

Chemical speciation approaches is an inherent part of metallomics, once metals/metalloids and organic structures need to be currently evaluated for attaining metallomics studies. Then, this chapter focuses on the applications of the chemical speciation applied to the human health risk, food and human diet, drugs, forensic, nanoscience, and geological metallomics, also pointing out the advances in such area. Some aspects regarding sample preparation is commented along this chapter, and some strategies for maintaining the integrity of the metallomics information are also emphasized.

Metabolomics strategy for the mapping of volatile exometabolome from Saccharomyces spp. widely used in the food industry based on comprehensive two-dimensional gas chromatography.

PubMed

Martins, Cátia; Brandão, Tiago; Almeida, Adelaide; Rocha, Sílvia M

2017-05-01

Saccharomyces spp. are widely used in the food and beverages industries. Their cellular excreted metabolites are important for general quality of products and can contribute to product differentiation. This exploratory study presents a metabolomics strategy for the comprehensive mapping of cellular metabolites of two yeast species, Saccharomyces cerevisiae and S. pastorianus (both collected in an industrial context) through a multidimensional chromatography platform. Solid-phase microextraction was used as a sample preparation method. The yeast viability, a specific technological quality parameter, was also assessed. This untargeted analysis allowed the putative identification of 525 analytes, distributed over 14 chemical families, the origin of which may be explained through the pathways network associated with yeasts metabolism. The expression of the different metabolic pathways was similar for both species, event that seems to be yeast genus dependent. Nevertheless, these species showed different growth rates, which led to statistically different metabolites content. This was the first in-depth approach that characterizes the headspace content of S. cerevisiae and S. pastorianus species cultures. The combination of a sample preparation method capable of providing released volatile metabolites directly from yeast culture headspace with comprehensive two-dimensional gas chromatography was successful in uncovering a specific metabolomic pattern for each species. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The associations among family meal frequency, food preparation frequency, self-efficacy for cooking, and food preparation techniques in children and adolescents.

PubMed

Woodruff, Sarah J; Kirby, Ashley R

2013-01-01

The purpose of this study was to describe family dinner frequency (FDF) by food preparation frequency (prep), self-efficacy for cooking (SE), and food preparation techniques (techniques) among a small sample in southwestern Ontario, Canada. A cross-sectional survey was administered under the supervision of the research team. After-school programs, sports programs, and 1 elementary school. The sample included 145 participants (41% boys, 59% girls) in grades 4-8. Demographics, prep, SE, techniques, FDF, and family meal attitudes and behaviors. Exploratory 1-way ANOVA and chi-square analyses were used. An ordinal regression analysis was used to determine the associations between FDF with descriptor variables (sex, grade, and ethnicity) and prep, SE, techniques, FDF, and family meal attitudes and behaviors (P < .05). Approximately 59% reported family dinners on 6 or 7 days per week. Half of participants were involved with prep 1-6 times per week. Mean SE was 25.3 (scale 1-32), and girls performed more techniques than boys (P = .02). Participants with greater SE (odds ratio = 1.15) and higher family meal attitudes and behaviors (odds ratio = 1.15) were more likely to have a higher FDF. Future health promotion strategies for family meals should aim at increasing children's and adolescents' SE. Copyright © 2013 Society for Nutrition Education and Behavior. Published by Elsevier Inc. All rights reserved.

Which food-related behaviours are associated with healthier intakes of fruits and vegetables among women?

PubMed

Crawford, David; Ball, Kylie; Mishra, Gita; Salmon, Jo; Timperio, Anna

2007-03-01

To examine associations between shopping, food preparation, meal and eating behaviours and fruit and vegetable intake among women. Cross-sectional survey. Community-based sample from metropolitan Melbourne, Australia. A sample of 1136 women aged 18-65 years, randomly selected from the electoral roll. Food-related behaviours reflecting organisation and forward-planning, as well as enjoyment of and high perceived value of meal shopping, preparation and consumption were associated with healthier intakes of fruits and vegetables. For example, women who more frequently planned meals before they went shopping, wrote a shopping list, enjoyed food shopping, planned in the morning what they will eat for dinner that night, planned what they will eat for lunch, reported they enjoy cooking, liked trying new recipes and who reported they sometimes prepare dishes ahead of time were more likely to consume two or more servings of vegetables daily. Conversely, women who frequently found cooking a chore, spent less than 15 minutes preparing dinner, decided on the night what they will eat for dinner, ate in a fast-food restaurant, ate takeaway meals from a fast-food restaurant, ate dinner and snacks while watching television and who frequently ate on the run were less likely to eat two or more servings of vegetables daily. Practical strategies based on these behavioural characteristics could be trialled in interventions aimed at promoting fruit and vegetable consumption among women.

Preparation and characterization of molecularly homogeneous silica-titania film by sol-gel process with different synthetic strategies.

PubMed

Chen, Hsueh-Shih; Huang, Sheng-Hsin; Perng, Tsong-Pyng

2012-10-24

Three silica-titania thin films with various degrees of molecular homogeneity were synthesized by the sol-gel process with the same precursor formula but different reaction paths. The dried films prepared by a single spin-coating process have a thickness of 500-700 nm and displayed no cracks or pin holes. The transmittances and refractive indices of the samples are >97.8% in the range of 350-1800 nm and 1.62-1.65 at 500 nm, respectively. The in-plane and out-of-plane chemical homogeneities of the films were analyzed by X-ray photoelectron spectroscopy and Auger electron spectroscopy, respectively. For the film with the highest degree of homogeneity, the deviations of O, Si, and Ti atomic contents in both in-plane and out-of-plane directions are less than 1.5%, indicating that the film is highly molecularly homogeneous. It also possesses the highest transparency and the lowest refractive index among the three samples.

Methodologies and Perspectives of Proteomics Applied to Filamentous Fungi: From Sample Preparation to Secretome Analysis

PubMed Central

Bianco, Linda; Perrotta, Gaetano

2015-01-01

Filamentous fungi possess the extraordinary ability to digest complex biomasses and mineralize numerous xenobiotics, as consequence of their aptitude to sensing the environment and regulating their intra and extra cellular proteins, producing drastic changes in proteome and secretome composition. Recent advancement in proteomic technologies offers an exciting opportunity to reveal the fluctuations of fungal proteins and enzymes, responsible for their metabolic adaptation to a large variety of environmental conditions. Here, an overview of the most commonly used proteomic strategies will be provided; this paper will range from sample preparation to gel-free and gel-based proteomics, discussing pros and cons of each mentioned state-of-the-art technique. The main focus will be kept on filamentous fungi. Due to the biotechnological relevance of lignocellulose degrading fungi, special attention will be finally given to their extracellular proteome, or secretome. Secreted proteins and enzymes will be discussed in relation to their involvement in bio-based processes, such as biomass deconstruction and mycoremediation. PMID:25775160

Methodologies and perspectives of proteomics applied to filamentous fungi: from sample preparation to secretome analysis.

PubMed

Bianco, Linda; Perrotta, Gaetano

2015-03-12

Filamentous fungi possess the extraordinary ability to digest complex biomasses and mineralize numerous xenobiotics, as consequence of their aptitude to sensing the environment and regulating their intra and extra cellular proteins, producing drastic changes in proteome and secretome composition. Recent advancement in proteomic technologies offers an exciting opportunity to reveal the fluctuations of fungal proteins and enzymes, responsible for their metabolic adaptation to a large variety of environmental conditions. Here, an overview of the most commonly used proteomic strategies will be provided; this paper will range from sample preparation to gel-free and gel-based proteomics, discussing pros and cons of each mentioned state-of-the-art technique. The main focus will be kept on filamentous fungi. Due to the biotechnological relevance of lignocellulose degrading fungi, special attention will be finally given to their extracellular proteome, or secretome. Secreted proteins and enzymes will be discussed in relation to their involvement in bio-based processes, such as biomass deconstruction and mycoremediation.

[Iron concentration and acceptation of yoghurt prepared in casting iron pots (iron migration and acceptation of yogurt)].

PubMed

Quintaes, Késia Diego; Almeyda Haj-Isa, Niurka M; Morgano, Marcelo Antônio

2005-12-01

Food fortification is an interesting strategy to treat and prevent iron anemia. This study aims to quantify the iron in yoghurt, with gelatin and sugar and without, prepared in iron and glass containers. Sensorial test was use to evaluate the acceptance and preference of the both products. The yoghurt was prepared in containers of iron and glass with UHT milk, powder milk and natural industrialized yoghurt. After fermentation, half of the product received addition of sugar and strawberry flavor gelatin. The collected samples get the total iron quantified by ICP OES. Sensorial analysis involving 105 consumers was use to determine the acceptance and preference of the products. 0,018 and 0,882mg of iron per 100g added in the natural yoghurt prepared in the glass and in the iron pots, respectively. The yoghurt with gelatin presented 0,037 and 1,302mg of iron per 100g when prepared in the glass and in the iron pots, respectively. The preference was low for the yoghurt prepared in the iron pot (29,5%), but when added strawberry gelatin it was about 51,5%. The yoghurt prepared in iron pots, is easily home made and adds important amount of iron. Add gelatin and sugar can favored its consumption.

A cognitive behavioral course for at-risk senior nursing students preparing to take the NCLEX.

PubMed

Poorman, Susan G; Mastorovich, Melissa L; Liberto, Terri L; Gerwick, Michele

2010-01-01

For some nursing students, the stress of preparing for and taking the NCLEX can lead to maladaptive behaviors such as poor test performance and inadequate preparation. A different approach to NCLEX preparation for at-risk seniors is described. A 3-credit course that combines cognitive behavioral techniques, metacognitive strategies, test-taking strategies, and simulated NCLEX experience with practice questions is presented. Students also develop an individualized plan of preparation from graduation until they take the NCLEX.

Effects of Instructional Preparation Strategies on Problem Solving in a Web-Based Learning Environment

ERIC Educational Resources Information Center

Lee, Young-Jin

2010-01-01

This study reports the effects of different types of instructional preparation strategies on the problem solving performance of college students taking an introductory physics class. Students were divided into four equally skilled groups and solved the same physics problems after receiving different instructional preparations (engaging in…

Dual Recognition Strategy for Specific and Sensitive Detection of Bacteria Using Aptamer-Coated Magnetic Beads and Antibiotic-Capped Gold Nanoclusters.

PubMed

Cheng, Dan; Yu, Mengqun; Fu, Fei; Han, Weiye; Li, Gan; Xie, Jianping; Song, Yang; Swihart, Mark T; Song, Erqun

2016-01-05

Food poisoning and infectious diseases caused by pathogenic bacteria such as Staphylococcus aureus (SA) are serious public health concerns. A method of specific, sensitive, and rapid detection of such bacteria is essential and important. This study presents a strategy that combines aptamer and antibiotic-based dual recognition units with magnetic enrichment and fluorescent detection to achieve specific and sensitive quantification of SA in authentic specimens and in the presence of much higher concentrations of other bacteria. Aptamer-coated magnetic beads (Apt-MB) were employed for specific capture of SA. Vancomycin-stabilized fluorescent gold nanoclusters (AuNCs@Van) were prepared by a simple one-step process and used for sensitive quantification of SA in the range of 32-10(8) cfu/mL with the detection limit of 16 cfu/mL via a fluorescence intensity measurement. And using this strategy, about 70 cfu/mL of SA in complex samples (containing 3 × 10(8) cfu/mL of other different contaminated bacteria) could be successfully detected. In comparison to prior studies, the developed strategy here not only simplifies the preparation procedure of the fluorescent probes (AuNCs@Van) to a great extent but also could sensitively quantify SA in the presence of much higher concentrations of other bacteria directly with good accuracy. Moreover, the aptamer and antibiotic used in this strategy are much less expensive and widely available compared to common-used antibodies, making it cost-effective. This general aptamer- and antibiotic-based dual recognition strategy, combined with magnetic enrichment and fluorescent detection of trace bacteria, shows great potential application in monitoring bacterial food contamination and infectious diseases.

A review of microdialysis coupled to microchip electrophoresis for monitoring biological events

PubMed Central

Saylor, Rachel A.; Lunte, Susan M.

2015-01-01

Microdialysis is a powerful sampling technique that enables monitoring of dynamic processes in vitro and in vivo. The combination of microdialysis with chromatographic or electrophoretic methods yields along with selective detection methods yields a “separation-based sensor” capable of monitoring multiple analytes in near real time. Analysis of microdialysis samples requires techniques that are fast (<1 min), have low volume requirements (nL–pL), and, ideally, can be employed on-line. Microchip electrophoresis fulfills these requirements and also permits the possibility of integrating sample preparation and manipulation with detection strategies directly on-chip. Microdialysis coupled to microchip electrophoresis has been employed for monitoring biological events in vivo and in vitro. This review discusses technical considerations for coupling microdialysis sampling and microchip electrophoresis, including various interface designs, and current applications in the field. PMID:25637011

Designing MgFe2O4 decorated on green mediated reduced graphene oxide sheets showing photocatalytic performance and luminescence property

NASA Astrophysics Data System (ADS)

Shetty, Krushitha; Lokesh, S. V.; Rangappa, Dinesh; Nagaswarupa, H. P.; Nagabhushana, H.; Anantharaju, K. S.; Prashantha, S. C.; Vidya, Y. S.; Sharma, S. C.

2017-02-01

Here, a green route has been reported to convert Graphene Oxide (GO) to reduced graphene oxide (RGO) using clove extract. A modest and eco-accommodating sol-gel strategy has been employed to prepare MgFe2O4 nanoparticles, MgFe2O4-RGO nanocomposite samples. The samples were analyzed by Powder X-ray diffraction (PXRD), Fourier Transform Infrared Spectroscopy (FTIR), UV-Visible Spectroscopy, Scanning Electron Microcopy (SEM), Transmission Electron Microscopy (TEM), Photoluminescence (PL) and Electrochemical Impedance Spectroscopy (EIS). PXRD result revealed that the prepared samples were cubic spinel in nature. SEM results uncovered flake like surface morphology of the prepared nanomaterial. Better PL emission signature was observed when excited at 329 nm. PL studies demonstrated that the present samples were potential for the fabrication of white component of white light emitting diodes (WLEDs). Further, MgFe2O4-RGO nanocomposite showed enhanced photocatalytic movement (PCM) and photostability under Sunlight in the decomposition of Malachite Green (MG) compared to MgFe2O4. This can be attributed to the interaction of MgFe2O4 surface with RGO sheets which results in PL quenching, demonstrates that the recombination of photo-induced electrons and holes in MgFe2O4-RGO nanocomposite is more effectively inhibited. A possible mechanism for the enhanced properties of MgFe2O4-RGO nanocomposite was discussed. Moreover, MgFe2O4-RGO photocatalyst also showed easy magnetic separation with high reusability. These results unveil that the synthesized sample can be used in display applications and also as a potential photocatalyst.

Influence of professional preparation and class structure on sexuality topics taught in middle and high schools.

PubMed

Rhodes, Darson L; Kirchofer, Gregg; Hammig, Bart J; Ogletree, Roberta J

2013-05-01

This study examined the impact of professional preparation and class structure on sexuality topics taught and use of practice-based instructional strategies in US middle and high school health classes. Data from the classroom-level file of the 2006 School Health Policies and Programs were used. A series of multivariable logistic regression models were employed to determine if sexuality content taught was dependent on professional preparation and /or class structure (HE only versus HE/another subject combined). Additional multivariable logistic regression models were employed to determine if use of practice-based instructional strategies was dependent upon professional preparation and/or class structure. Years of teaching health topics and size of the school district were included as covariates in the multivariable logistic regression models. Findings indicated professionally prepared health educators were significantly more likely to teach 7 of the 13 sexuality topics as compared to nonprofessionally prepared health educators. There was no statistically significant difference in the instructional strategies used by professionally prepared and nonprofessionally prepared health educators. Exclusively health education classes versus combined classes were significantly more likely to have included 6 of the 13 topics and to have incorporated practice-based instructional strategies in the curricula. This study indicated professional preparation and class structure impacted sexuality content taught. Class structure also impacted whether opportunities for students to practice skills were made available. Results support the need for continued advocacy for professionally prepared health educators and health only courses. © 2013, American School Health Association.

C-Terminal Protein Characterization by Mass Spectrometry: Isolation of C-Terminal Fragments from Cyanogen Bromide-Cleaved Protein

PubMed Central

Nika, Heinz; Hawke, David H.; Angeletti, Ruth Hogue

2014-01-01

A sample preparation method for protein C-terminal peptide isolation from cyanogen bromide (CNBr) digests has been developed. In this strategy, the analyte was reduced and carboxyamidomethylated, followed by CNBr cleavage in a one-pot reaction scheme. The digest was then adsorbed on ZipTipC18 pipette tips for conjugation of the homoserine lactone-terminated peptides with 2,2′-dithiobis (ethylamine) dihydrochloride, followed by reductive release of 2-aminoethanethiol from the derivatives. The thiol-functionalized internal and N-terminal peptides were scavenged on activated thiol sepharose, leaving the C-terminal peptide in the flow-through fraction. The use of reversed-phase supports as a venue for peptide derivatization enabled facile optimization of the individual reaction steps for throughput and completeness of reaction. Reagents were replaced directly on the support, allowing the reactions to proceed at minimal sample loss. By this sequence of solid-phase reactions, the C-terminal peptide could be recognized uniquely in mass spectra of unfractionated digests by its unaltered mass signature. The use of the sample preparation method was demonstrated with low-level amounts of a whole, intact model protein. The C-terminal fragments were retrieved selectively and efficiently from the affinity support. The use of covalent chromatography for C-terminal peptide purification enabled recovery of the depleted material for further chemical and/or enzymatic manipulation. The sample preparation method provides for robustness and simplicity of operation and is anticipated to be expanded to gel-separated proteins and in a scaled-up format to high-throughput protein profiling in complex biological mixtures. PMID:24688319

Opportunistic Resource Usage in CMS

NASA Astrophysics Data System (ADS)

Kreuzer, Peter; Hufnagel, Dirk; Dykstra, D.; Gutsche, O.; Tadel, M.; Sfiligoi, I.; Letts, J.; Wuerthwein, F.; McCrea, A.; Bockelman, B.; Fajardo, E.; Linares, L.; Wagner, R.; Konstantinov, P.; Blumenfeld, B.; Bradley, D.; Cms Collaboration

2014-06-01

CMS is using a tiered setup of dedicated computing resources provided by sites distributed over the world and organized in WLCG. These sites pledge resources to CMS and are preparing them especially for CMS to run the experiment's applications. But there are more resources available opportunistically both on the GRID and in local university and research clusters which can be used for CMS applications. We will present CMS' strategy to use opportunistic resources and prepare them dynamically to run CMS applications. CMS is able to run its applications on resources that can be reached through the GRID, through EC2 compliant cloud interfaces. Even resources that can be used through ssh login nodes can be harnessed. All of these usage modes are integrated transparently into the GlideIn WMS submission infrastructure, which is the basis of CMS' opportunistic resource usage strategy. Technologies like Parrot to mount the software distribution via CVMFS and xrootd for access to data and simulation samples via the WAN are used and will be described. We will summarize the experience with opportunistic resource usage and give an outlook for the restart of LHC data taking in 2015.

Using segmented regression analysis of interrupted time series data to assess colonoscopy quality outcomes of a web-enhanced implementation toolkit to support evidence-based practices for bowel preparation: a study protocol.

PubMed

Ramsey, Alex T; Maki, Julia; Prusaczyk, Beth; Yan, Yan; Wang, Jean; Lobb, Rebecca

2015-06-07

While there is convincing evidence on interventions to improve bowel preparation for patients, the evidence on how to implement these evidence-based practices (EBPs) in outpatient colonoscopy settings is less certain. The Strategies to Improve Colonoscopy (STIC) study compares the effect of two implementation strategies, physician education alone versus physician education plus an implementation toolkit for staff, on adoption of three EBPs (split-dosing of bowel preparation, low-literacy education, teach-back) to improve pre-procedure and intra-procedure quality measures. The implementation toolkit contains a staff education module, website containing tools to support staff in delivering EBPs, tailored patient education materials, and brief consultation with staff to determine how the EBPs can be integrated into the existing workflow. Given adaptations to the implementation plan and intentional flexibility in the delivery of the EBPs, we utilize a pragmatic study to balance external validity with demonstrating effectiveness of the implementation strategies. Participants will include all outpatient colonoscopy physicians, staff, and patients from a convenience sample of six endoscopy settings. Aim #1 will explore the relative effect of two strategies to implement patient-level EBPs on adoption and clinical quality outcomes. We will assess the change in level and trends of clinical quality outcomes (i.e., adequacy of bowel preparation, adenoma detection) using segmented regression analysis of interrupted time series data with two groups (intervention and delayed start). Aim #2 will examine the influence of organizational readiness to change on EBP implementation. We use a PRECIS diagram to reflect the extent to which each indicator of the study was pragmatic versus explanatory, revealing a largely pragmatic study. Implementation challenges have already motivated several adaptations to the original plan, reflecting the nature of implementation in real-world healthcare settings. The pragmatic study responds to the evolving needs of its healthcare partners and allows for flexibility in intervention delivery, thereby informing clinical decision-making in real-world settings. The current study will provide information about what works (intervention effectiveness), for whom it works (influence of Medicaid versus other insurance), in which contexts it works (setting characteristics that influence implementation), and how it works best (comparison of implementation strategies).

MUET Preparation Language Learning Strategies

ERIC Educational Resources Information Center

Kuen, Yoong Li; Embi, Mohamed Amin

2012-01-01

The main objective of the study was to examine the English language learning strategies (LLS) used by Lower Six students in secondary schools who are sitting for their MUET test. It analyzed the language learning strategies that students use in order to prepare for the MUET test. Data were collected using a survey questionnaire with 300 students.…

Strategies Instruction to Improve the Preparation for English Oral Exams

ERIC Educational Resources Information Center

Abad, José Vicente; Alzate, Paula Andrea

2016-01-01

This article presents the results of an inter-institutional research study that assessed the impact of strategies instruction on students' preparation for and performance in oral exams. Two teacher-researchers at different universities trained 26 students in their respective B1-English-level courses in using language learning strategies. The study…

Problems faced and coping strategies used by adolescents with mentally ill parents in Delhi.

PubMed

George, Shoba; Shaiju, Bindu; Sharma, Veena

2012-01-01

The present study was conducted to assess the problems faced by adolescents whose parents suffer from major mental illness at selected mental health institutes of Delhi. The objectives also included assessment of the coping strategies of the adolescents in dealing with these problems. The Stuart Stress Adaptation Model of Psychiatric Nursing Care was used as the conceptual framework. A descriptive survey approach with cross-sectional design was used in the study. A structured interview schedule was prepared. Purposive non-probability sampling technique was employed to interview 50 adolescents whose parents suffer from major mental illness. Data gathered was analysed and interpreted using both descriptive and inferential statistics. The study showed that majority of the adolescents had moderate problems as a result of their parent's mental illness. Area-wise analysis of the problems revealed that the highest problems faced were in family relationship and support and majority of the adolescents used maladaptive coping strategies. A set of guidelines on effective coping strategies was disseminated to these adolescents.

Multiplexed MRM-Based Protein Quantitation Using Two Different Stable Isotope-Labeled Peptide Isotopologues for Calibration.

PubMed

LeBlanc, André; Michaud, Sarah A; Percy, Andrew J; Hardie, Darryl B; Yang, Juncong; Sinclair, Nicholas J; Proudfoot, Jillaine I; Pistawka, Adam; Smith, Derek S; Borchers, Christoph H

2017-07-07

When quantifying endogenous plasma proteins for fundamental and biomedical research - as well as for clinical applications - precise, reproducible, and robust assays are required. Targeted detection of peptides in a bottom-up strategy is the most common and precise mass spectrometry-based quantitation approach when combined with the use of stable isotope-labeled peptides. However, when measuring protein in plasma, the unknown endogenous levels prevent the implementation of the best calibration strategies, since no blank matrix is available. Consequently, several alternative calibration strategies are employed by different laboratories. In this study, these methods were compared to a new approach using two different stable isotope-labeled standard (SIS) peptide isotopologues for each endogenous peptide to be quantified, enabling an external calibration curve as well as the quality control samples to be prepared in pooled human plasma without interference from endogenous peptides. This strategy improves the analytical performance of the assay and enables the accuracy of the assay to be monitored, which can also facilitate method development and validation.

A systematic assessment of goblet cell sampling of the bulbar conjunctiva by impression cytology.

PubMed

Doughty, Michael J

2015-07-01

The purpose of this study was to assess the apparent goblet cell density (GCD) from conjunctival impression cytology (CIC) samples in relation to the number of conjunctival cells collected onto the filters. CIC specimens were collected from the superior-temporal bulbar conjunctiva of 16 pigmented rabbits onto Biopore (Millicell-CM) membranes, fixed with buffered glutaraldehyde and stained with Giemsa. Different numbers of microscope fields of view in each of the specimens were imaged by light microscopy using a 20× magnification objective lens (200× final magnification), and the goblet cells marked and counted. The GCD values/sq. mm were calculated. The same conjunctival region of 3 other rabbits was also prepared for transmission electron microscopy (TEM) by fixation, in situ, with the same buffered glutaraldehyde. Mean values for GCD estimates were found to vary from 399 to 1576 cells/sq. mm, depending on the image sampling and analysis strategy chosen, with the lowest inter-sample variance of around 10% being found if a maximum goblet cell count was taken on substantially multilayered regions of the CIC specimens. Counts of the number of goblet cells per 1000 visible conjunctival epithelial cells yielded a value of close to 90 (range 36-151), with modest inter-sample variability of around 30%. A three or ten 200× microscope field and random sampling strategy yielded mean GCD values between 542 and 670 cells/sq. mm, but with very high intra- and inter-sample variance of at least 60% and sometimes higher than 100%. TEM confirmed the multilayered organization of the conjunctiva and the deeper lying goblet cells. The general use of a goblet cell count as an objective marker for conjunctival normality or health is likely to be highly variable unless a more specific strategy is adopted. Beyond providing details of exactly the counting strategy used, it would be very useful to provide full details of the actual microscope field size used as well as information on the intra-sample variability in goblet cell counts. Copyright © 2015 Elsevier Ltd. All rights reserved.

Effect of preparation methods and doping on the structural and tunable emissions of CdS

NASA Astrophysics Data System (ADS)

Mohamed, Mohamed Bakr; Abdel-Kader, M. H.; Alhazime, Ali A.; Almarashi, Jamal Q. M.

2018-03-01

Fe, Mn and Mg doped CdS samples were prepared by thermolysis method in air and under flow of nitrogen. Structural, compositional and optical properties of the prepared samples were investigated using x-ray powder diffraction (XRD), scanning electron microscope (SEM/EDS mapping), Fourier transform infrared red (FTIR), UV-vis absorption and photoluminescence (PL) spectroscopes. Rietveld refinement of x-ray data showed that all the undoped and doped CdS samples prepared in air and under flow of nitrogen have both cubic and hexagonal structures. The percentages of hexagonal and cubic phases for all prepared samples were determined. The crystallite size increased for CdS prepared under flow of N2 compared with the sample prepared in air. The energy gap of all the samples was calculated using UV data. The intensity of PL emission changed according to the method of preparation and the kind of doping elements. PL emission revealed a blue shift for CdS prepared in air compared with CdS prepared under flow of nitrogen; also all doped samples showed a red shift of PL spectra compared with undoped samples. Undoped and doped CdS with Fe and Mg samples emitted violet and blue sub-spectra. Mn doped CdS prepared in air revealed violet, blue and yellow sub-spectra, while the sample prepared under flow of N2 emitted violet, blue and green sub-spectra.

Highly Enhanced Thermoelectric Properties of Bi/Bi2S3 Nanocomposites.

PubMed

Ge, Zhen-Hua; Qin, Peng; He, DongSheng; Chong, Xiaoyu; Feng, Dan; Ji, Yi-Hong; Feng, Jing; He, Jiaqing

2017-02-08

Bismuth sulfide (Bi 2 S 3 ) has been of high interest for thermoelectric applications due to the high abundance of sulfur on Earth. However, the low electrical conductivity of pristine Bi 2 S 3 results in a low figure of merit (ZT). In this work, Bi 2 S 3 @Bi core-shell nanowires with different Bi shell thicknesses were prepared by a hydrothermal method. The core-shell nanowires were densified to Bi/Bi 2 S 3 nanocomposite by spark plasma sintering (SPS), and the structure of the nanowire was maintained as the nanocomposite due to rapid SPS processing and low sintering temperature. The thermoelectric properties of bulk samples were investigated. The electrical conductivity of a bulk sample after sintering at 673 K for 5 min using Bi 2 S 3 @Bi nanowire powders prepared by treating Bi 2 S 3 nanowires in a hydrazine solution for 3 h is 3 orders of magnitude greater than that of a pristine Bi 2 S 3 sample. The nanocomposite possessed the highest ZT value of 0.36 at 623 K. This represents a new strategy for densifying core-shell powders to enhance their thermoelectric properties.

Multivariate study of parameters in the determination of pesticide residues in apple by headspace solid phase microextraction coupled to gas chromatography-mass spectrometry using experimental factorial design.

PubMed

Abdulra'uf, Lukman Bola; Tan, Guan Huat

2013-12-15

Solid-phase microextraction (SPME) is a solvent-less sample preparation method which combines sample preparation, isolation, concentration and enrichment into one step. In this study, multivariate strategy was used to determine the significance of the factors affecting the solid phase microextraction of pesticide residues (fenobucarb, diazinon, chlorothalonil and chlorpyrifos) using a randomised factorial design. The interactions and effects of temperature, time and salt addition on the efficiency of the extraction of the pesticide residues were evaluated using 2(3) factorial designs. The analytes were extracted with 100 μm PDMS fibres according to the factorial design matrix and desorbed into a gas chromatography-mass spectrometry detector. The developed method was applied for the analysis of apple samples and the limits of detection were between 0.01 and 0.2 μg kg(-)(1), which were lower than the MRLs for apples. The relative standard deviations (RSD) were between 0.1% and 13.37% with average recovery of 80-105%. The linearity ranges from 0.5-50 μg kg(-)(1) with correlation coefficient greater than 0.99. Copyright © 2013 Elsevier Ltd. All rights reserved.

Green and Mild Oxidation: An Efficient Strategy toward Water-Dispersible Graphene.

PubMed

You, Xiaofei; Yang, Siwei; Li, Jipeng; Deng, Yuan; Dai, Lianqi; Peng, Xiong; Huang, Haoguang; Sun, Jing; Wang, Gang; He, Peng; Ding, Guqiao; Xie, Xiaoming

2017-01-25

Scalable fabrication of water-dispersible graphene (W-Gr) is highly desirable yet technically challenging for most practical applications of graphene. Herein, a green and mild oxidation strategy to prepare bulk W-Gr (dispersion, slurry, and powder) with high yield was proposed by fully exploiting structure defects of thermally reduced graphene oxide (TRGO) and oxidizing radicals generated from hydrogen peroxide (H 2 O 2 ). Owing to the increased carboxyl group from the mild oxidation process, the obtained W-Gr can be redispersed in low-boiling solvents with a reasonable concentration. Benefiting from the modified surface chemistry, macroscopic samples processed from the W-Gr show good hydrophilicity (water contact angle of 55.7°) and excellent biocompatibility, which is expected to be an alternative biomaterial for bone, vessel, and skin regeneration. In addition, the green and mild oxidation strategy is also proven to be effective for dispersing other carbon nanomaterials in a water system.

Single-Drop Raman Imaging Exposes the Trace Contaminants in Milk.

PubMed

Tan, Zong; Lou, Ting-Ting; Huang, Zhi-Xuan; Zong, Jing; Xu, Ke-Xin; Li, Qi-Feng; Chen, Da

2017-08-02

Better milk safety control can offer important means to promote public health. However, few technologies can detect different types of contaminants in milk simultaneously. In this regard, the present work proposes a single-drop Raman imaging (SDRI) strategy for semiquantitation of multiple hazardous factors in milk solutions. By developing SDRI strategy that incorporates the coffee-ring effect (a natural phenomenon often presents in a condensed circle pattern after a drop evaporated) for sample pretreatment and discrete wavelet transform for spectra processing, the method serves well to expose typical hazardous molecular species in milk products, such as melamine, sodium thiocyanate and lincomycin hydrochloride, with little sample preparation. The detection sensitivity for melamine, sodium thiocyanate, and lincomycin hydrochloride are 0.1 mg kg -1 , 1 mg kg -1 , and 0.1 mg kg -1 , respectively. Theoretically, we establish that the SDRI represents a novel and environment-friendly method that screens the milk safety efficiently, which could be well extended to inspection of other food safety.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harrison, W.; Dravnieks, A.; Zussman, R.

Samples of malodorous air and dredged material were collected at diked disposal sites at the following locations: Buffalo, NY; Milwaukee, WI; Mobile, AL; York Harbor, ME; Houston, TX; Detroit, MI; and Anacortes, WA; during the period July--October, 1975. Odorous compounds in the air samples were identified by gas chromatography/mass spectrometry, while the detection threshold, intensity, and character of the various odors were determined by experienced panelists using a dynamic, forced-choice-triangle olfactometer. Although significant problems with malodors were not observed beyond the disposal-area dikes during site visits, noteworthy odor episodes had occurred at some sites. An odor-abatement strategy is presented formore » handling the expected range of odor conditions at dredged-material disposal sites. Its aim is to reduce to an acceptable level the intensity of malodors in an affected community. The main steps in the strategy cover selection of the disposal site, site preparation, odor characterization of sediments to be dredged, malodor abatement during dredging and disposal operations, malodor abatement after filling of the disposal site, and the handling of malodor complaints.« less

PCL foamed scaffolds loaded with 5-fluorouracil anti-cancer drug prepared by an eco-friendly route.

PubMed

Salerno, Aurelio; Domingo, Concepción; Saurina, Javier

2017-06-01

This study describes a new preparation method, which combines freeze drying and supercritical CO 2 foaming approaches, for the preparation of drug delivery scaffolds of polycaprolactone loaded with 5-fluorouracil, an anti-cancer drug, with low solubility in scCO 2 . It is a principal objective of this work to design a scCO 2 strategy to reduce 5-Fu solubility limitations in its homogeneous distribution into a PCL scaffold through the design of an innovative processing method. The design of this process is considered valuable for the development of clean technology in pharmacy and medicine, since most of the active agents have a null solubility in scCO 2 ·Supercritical CO 2 is used as a blowing agent to induce polymer foaming by means of the low temperature pressure quench process. The resulting samples have been prepared under different operational conditions focused on enhancing the performance of the release process. In this case, design of experiments (DOE) was considered for a more comprehensive and systematic optimization of the product. In particular, drug amount, equals to 4.8 or 9.1wt%, process temperature, of 45 or 50°C and depressurization rate, equals to 0.1MPas -1 or 2MPas -1 were selected as the factors to be investigated by a three-factor at two-level full factorial design. Samples were characterized to establish porosity data, drug loading percentage and, especially, release profile chromatographically monitored. Results from DOE have concluded which are the best samples providing a sustained drug release for several days, which may be of great interest to develop materials for tissue engineering and sustained release applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of a Strategy Based on the Surface Plasmon Resonance Technology for Platelet Compatibility Testing.

PubMed

Wu, Chang-Lin; He, Jian-An; Gu, Da-Yong; Shao, Chao-Peng; Zhu, Yi; Dang, Xin-Tang

2018-01-01

This study was aimed to establish a novel strategy based on the surface plasmon resonance (SPR) technology for platelet compatibility testing. A novel surface matrix was prepared based on poly (OEGMA-co-HEMA) via surface-initiated polymerization as a biosensor surface platform. Type O universal platelets and donor platelets were immobilized on these novel matrices via amine-coupling reaction and worked as a capturing ligand for binding the platelet antibody. Antibodies binding to platelets were monitored in real time by injecting the samples into a microfluidic channel. Clinical serum samples (n = 186) with multiple platelet transfusions were assayed for platelet antibodies using the SPR technology and monoclonal antibody-immobilized platelet antigen (MAIPA) assay. The novel biosensor surface achieved nonfouling background and high immobilization capacity and showed good repeatability and stability after regeneration. The limit of detection of the SPR biosensor for platelet antibody was estimated to be 50 ng/mL. The sensitivity and specificity were 92% and 98.7%. It could detect the platelet antibody directly in serum samples, and the results were similar to MAIPA assay. A novel strategy to facilitate the sensitive and reliable detection of platelet compatibility for developing an SPR-based biosensor was established in this study. The SPR-based biosensor combined with novel surface chemistry is a promising method for platelet compatibility testing.

7 CFR 27.21 - Preparation of samples of cotton.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 7 Agriculture 2 2012-01-01 2012-01-01 false Preparation of samples of cotton. 27.21 Section 27.21... REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.21 Preparation of samples of cotton. The samples from each bale shall be prepared as specified in this section...

7 CFR 27.21 - Preparation of samples of cotton.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 2 2010-01-01 2010-01-01 false Preparation of samples of cotton. 27.21 Section 27.21... REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.21 Preparation of samples of cotton. The samples from each bale shall be prepared as specified in this section...

7 CFR 27.21 - Preparation of samples of cotton.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 2 2011-01-01 2011-01-01 false Preparation of samples of cotton. 27.21 Section 27.21... REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.21 Preparation of samples of cotton. The samples from each bale shall be prepared as specified in this section...

Aerosol dilution as a simple strategy for analysis of complex samples by ICP-MS.

PubMed

Barros, Ariane I; Pinheiro, Fernanda C; Amaral, Clarice D B; Lorençatto, Rodolfo; Nóbrega, Joaquim A

2018-02-01

This study investigated the capability of High Matrix Introduction (HMI) strategy for analysis of dialysis solution and urine samples using inductively coupled plasma mass spectrometry. The use of HMI enables the direct introduction of urine samples and dialysis solutions 2-fold diluted with 0.14molL -1 HNO 3 . Bismuth, Ge, Ir, Li, Pt, Rh, Sc and Tl were evaluated as internal standards for Al, Ag, As, Be, Cd, Cr, Pb, Sb, Se, Tl, and Hg determination in dialysis solution and As, Cd, Hg and Pb determination in urine samples. Helium collision cell mode (4.5mLmin -1 ) was efficient to overcome polyatomic interferences in As, Se and Cr determinations. Mercury memory effects were evaluated by washing with 0.12molL -1 HCl or an alkaline diluent solution prepared with n-butanol, NH 4 OH, EDTA, and Triton X-100. This later solution was efficient for avoiding Hg memory effects in 6h of analysis. Linear calibration curves were obtained for all analytes and detection limits were lower than maximum amounts allowed by Brazilian legislations. Recoveries for all analytes in dialysis solutions and urine samples ranged from 82% to 125% and relative standard deviations for all elements and samples were lower than 7%. Analysis of control internal urine samples was in agreement with certified values at 95% confidence level (t-test; p < 0.05). Copyright © 2017 Elsevier B.V. All rights reserved.

MIPs in Aqueous Environments.

PubMed

Wan, Ying-chun; Ma, Hui-ting; Lu, Bin

2015-01-01

When organic solvent-compatible molecularly imprinted polymers (MIPs) are used in aqueous environment, how to reduce nonspecific binding is a major challenge. By modifying the binding solvents and introducing appropriate washing and elution steps, even relatively hydrophobic MIPs can gain optimal rebinding selectivity in aqueous conditions. Furthermore, water-compatible MIPs that can be used to treat aqueous samples directly have been prepared. The use of hydrophilic co-monomers, the controlled surface modification through controlled radical polymerization, and the new interfacial molecular imprinting methods are different strategies to prepare water-compatible MIPs. By combining MIPs with other techniques, both organic solvent-compatible and water-compatible MIPs can display better functional performances in aqueous conditions. Intensive studies on MIPs in aqueous conditions can provide new MIPs with much-improved compatibilities that will lead to more interesting applications in biomedicine and biotechnology.

Protocol for Microplastics Sampling on the Sea Surface and Sample Analysis

PubMed Central

Kovač Viršek, Manca; Palatinus, Andreja; Koren, Špela; Peterlin, Monika; Horvat, Petra; Kržan, Andrej

2016-01-01

Microplastic pollution in the marine environment is a scientific topic that has received increasing attention over the last decade. The majority of scientific publications address microplastic pollution of the sea surface. The protocol below describes the methodology for sampling, sample preparation, separation and chemical identification of microplastic particles. A manta net fixed on an »A frame« attached to the side of the vessel was used for sampling. Microplastic particles caught in the cod end of the net were separated from samples by visual identification and use of stereomicroscopes. Particles were analyzed for their size using an image analysis program and for their chemical structure using ATR-FTIR and micro FTIR spectroscopy. The described protocol is in line with recommendations for microplastics monitoring published by the Marine Strategy Framework Directive (MSFD) Technical Subgroup on Marine Litter. This written protocol with video guide will support the work of researchers that deal with microplastics monitoring all over the world. PMID:28060297

Protocol for Microplastics Sampling on the Sea Surface and Sample Analysis.

PubMed

Kovač Viršek, Manca; Palatinus, Andreja; Koren, Špela; Peterlin, Monika; Horvat, Petra; Kržan, Andrej

2016-12-16

Microplastic pollution in the marine environment is a scientific topic that has received increasing attention over the last decade. The majority of scientific publications address microplastic pollution of the sea surface. The protocol below describes the methodology for sampling, sample preparation, separation and chemical identification of microplastic particles. A manta net fixed on an »A frame« attached to the side of the vessel was used for sampling. Microplastic particles caught in the cod end of the net were separated from samples by visual identification and use of stereomicroscopes. Particles were analyzed for their size using an image analysis program and for their chemical structure using ATR-FTIR and micro FTIR spectroscopy. The described protocol is in line with recommendations for microplastics monitoring published by the Marine Strategy Framework Directive (MSFD) Technical Subgroup on Marine Litter. This written protocol with video guide will support the work of researchers that deal with microplastics monitoring all over the world.

A high-throughput Sanger strategy for human mitochondrial genome sequencing

PubMed Central

2013-01-01

Background A population reference database of complete human mitochondrial genome (mtGenome) sequences is needed to enable the use of mitochondrial DNA (mtDNA) coding region data in forensic casework applications. However, the development of entire mtGenome haplotypes to forensic data quality standards is difficult and laborious. A Sanger-based amplification and sequencing strategy that is designed for automated processing, yet routinely produces high quality sequences, is needed to facilitate high-volume production of these mtGenome data sets. Results We developed a robust 8-amplicon Sanger sequencing strategy that regularly produces complete, forensic-quality mtGenome haplotypes in the first pass of data generation. The protocol works equally well on samples representing diverse mtDNA haplogroups and DNA input quantities ranging from 50 pg to 1 ng, and can be applied to specimens of varying DNA quality. The complete workflow was specifically designed for implementation on robotic instrumentation, which increases throughput and reduces both the opportunities for error inherent to manual processing and the cost of generating full mtGenome sequences. Conclusions The described strategy will assist efforts to generate complete mtGenome haplotypes which meet the highest data quality expectations for forensic genetic and other applications. Additionally, high-quality data produced using this protocol can be used to assess mtDNA data developed using newer technologies and chemistries. Further, the amplification strategy can be used to enrich for mtDNA as a first step in sample preparation for targeted next-generation sequencing. PMID:24341507

An efficient one-step condensation and activation strategy to synthesize porous carbons with optimal micropore sizes for highly selective CO₂ adsorption.

PubMed

Wang, Jiacheng; Liu, Qian

2014-04-21

A series of microporous carbons (MPCs) were successfully prepared by an efficient one-step condensation and activation strategy using commercially available dialdehyde and diamine as carbon sources. The resulting MPCs have large surface areas (up to 1881 m(2) g(-1)), micropore volumes (up to 0.78 cm(3) g(-1)), and narrow micropore size distributions (0.7-1.1 nm). The CO₂ uptakes of the MPCs prepared at high temperatures (700-750 °C) are higher than those prepared under mild conditions (600-650 °C), because the former samples possess optimal micropore sizes (0.7-0.8 nm) that are highly suitable for CO₂ capture due to enhanced adsorbate-adsorbent interactions. At 1 bar, MPC-750 prepared at 750 °C demonstrates the best CO₂ capture performance and can efficiently adsorb CO₂ molecules at 2.86 mmol g(-1) and 4.92 mmol g(-1) at 25 and 0 °C, respectively. In particular, the MPCs with optimal micropore sizes (0.7-0.8 nm) have extremely high CO₂/N₂ adsorption ratios (47 and 52 at 25 and 0 °C, respectively) at 1 bar, and initial CO₂/N₂ adsorption selectivities of up to 81 and 119 at 25 °C and 0 °C, respectively, which are far superior to previously reported values for various porous solids. These excellent results, combined with good adsorption capacities and efficient regeneration/recyclability, make these carbons amongst the most promising sorbents reported so far for selective CO₂ adsorption in practical applications.

Investigating How Nontraditional Elementary Pre-service Teachers Negotiate the Teaching of Science

NASA Astrophysics Data System (ADS)

Shelton, Mythianne

This qualitative study was designed to investigate the influences on nontraditional preservice teachers as they negotiated the teaching of science in elementary school. Based upon a sociocultural theoretical framework with an identity-in-practice lens, these influences included beliefs about science teaching, life experiences, and the impact of the teacher preparation program. The study sample consisted of two nontraditional preservice teachers who were student teaching in an elementary classroom. Data, collected over a five-month period, included in-depth individual interviews, classroom observations, audio recordings, and reviews of documentations. Interviews focused on the participants' beliefs relating to the teaching of science, prior experiences, and their teacher preparation program experiences relating to the teaching of science. Classroom observations provided additional insights into the classroom setting, participants' teaching strategies, and participants' interactions with the students and cooperating teacher. A whole-text analysis of the interview transcripts, observational field notes, audio recordings and documents generated eight major categories: beliefs about science teaching, role of family, teaching science in the classroom, teacher identity, non-teacher identity, relationships with others, discourses of classroom teaching, and discourses of teachers. The following significant findings emerged from the data: (a) the identity of nontraditional student teachers as science teachers related to early life experiences in science classes; (b) the identity of nontraditional student teachers as science teachers was influenced by their role as parents; (c) nontraditional student teachers learned strategies that supported their beliefs about inquiry learning; and (d) nontraditional student teachers valued the teacher preparation program support system. The results from this qualitative study suggest that sociocultural theory with an identity-in-practice lens provides a theoretical framework for understanding the influences that affect why nontraditional preservice teachers select strategies to teach science in the elementary classroom.

Practical coaching by mentors: student midwives' perceptions.

PubMed

Finnerty, Gina; Collington, Val

2013-11-01

The objective of this paper was to explore some of the specific strategies used by midwife mentors to mediate practice learning from the perspective of a sample of student midwives. Audio-diaries were completed by student midwives over ten days in practice and were transcribed using discourse analysis. A sub-sample from 19 students' learning diaries from a national midwifery education study conducted by Pope et al. (2003) has been selected as the diaries informed a separate study. The sample of student midwives were studying on degree and diploma programmes at five case study sites in England. Students described how their mentors apparently successfully tailored their teaching to the students' needs. However, there was perceived disparity in techniques used by individual mentors to pass on their practice know-how. The findings demonstrate the pivotal role of the mentor for 'scaffolding' learning and also using 'fading' techniques within a cognitive apprenticeship model. Mentors need assistance to adapt their mentoring styles and to use a wider range of instruction strategies for student midwives. This has practical implications for mentor preparation programmes and mentorship models. Crown Copyright © 2012. Published by Elsevier Ltd. All rights reserved.

Complementary Sample Preparation Strategies for Analysis of Cereal β-Glucan Oxidation Products by UPLC-MS/MS.

PubMed

Boulos, Samy; Nyström, Laura

2017-01-01

The oxidation of cereal (1→3,1→4)-β-D-glucan can influence the health promoting and technological properties of this linear, soluble homopolysaccharide by introduction of new functional groups or chain scission. Apart from deliberate oxidative modifications, oxidation of β-glucan can already occur during processing and storage, which is mediated by hydroxyl radicals (HO • ) formed by the Fenton reaction. We present four complementary sample preparation strategies to investigate oat and barley β-glucan oxidation products by hydrophilic interaction ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), employing selective enzymatic digestion, graphitized carbon solid phase extraction (SPE), and functional group labeling techniques. The combination of these methods allows for detection of both lytic (C1, C3/4, C5) and non-lytic (C2, C4/3, C6) oxidation products resulting from HO • -attack at different glucose-carbons. By treating oxidized β-glucan with lichenase and β-glucosidase, only oxidized parts of the polymer remained in oligomeric form, which could be separated by SPE from the vast majority of non-oxidized glucose units. This allowed for the detection of oligomers with mid-chain glucuronic acids (C6) and carbonyls, as well as carbonyls at the non-reducing end from lytic C3/C4 oxidation. Neutral reducing ends were detected by reductive amination with anthranilic acid/amide as labeled glucose and cross-ring cleaved units (arabinose, erythrose) after enzyme treatment and SPE. New acidic chain termini were observed by carbodiimide-mediated amidation of carboxylic acids as anilides of gluconic, arabinonic, and erythronic acids. Hence, a full characterization of all types of oxidation products was possible by combining complementary sample preparation strategies. Differences in fine structure depending on source (oat vs. barley) translates to the ratio of observed oxidized oligomers, with in-depth analysis corroborating a random HO • -attack on glucose units irrespective of glycosidic linkage and neighborhood. The method was demonstrated to be (1) sufficiently sensitive to allow for the analysis of oxidation products also from a mild ascorbate-driven Fenton reaction, and (2) to be specific for cereal β-glucan even in the presence of other co-oxidized polysaccharides. This opens doors to applications in food processing to assess potential oxidations and provides the detailed structural basis to understand the effect oxidized functional groups have on β-glucan's health promoting and technological properties.

Complementary Sample Preparation Strategies for Analysis of Cereal β-Glucan Oxidation Products by UPLC-MS/MS

PubMed Central

Boulos, Samy; Nyström, Laura

2017-01-01

The oxidation of cereal (1→3,1→4)-β-D-glucan can influence the health promoting and technological properties of this linear, soluble homopolysaccharide by introduction of new functional groups or chain scission. Apart from deliberate oxidative modifications, oxidation of β-glucan can already occur during processing and storage, which is mediated by hydroxyl radicals (HO•) formed by the Fenton reaction. We present four complementary sample preparation strategies to investigate oat and barley β-glucan oxidation products by hydrophilic interaction ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), employing selective enzymatic digestion, graphitized carbon solid phase extraction (SPE), and functional group labeling techniques. The combination of these methods allows for detection of both lytic (C1, C3/4, C5) and non-lytic (C2, C4/3, C6) oxidation products resulting from HO•-attack at different glucose-carbons. By treating oxidized β-glucan with lichenase and β-glucosidase, only oxidized parts of the polymer remained in oligomeric form, which could be separated by SPE from the vast majority of non-oxidized glucose units. This allowed for the detection of oligomers with mid-chain glucuronic acids (C6) and carbonyls, as well as carbonyls at the non-reducing end from lytic C3/C4 oxidation. Neutral reducing ends were detected by reductive amination with anthranilic acid/amide as labeled glucose and cross-ring cleaved units (arabinose, erythrose) after enzyme treatment and SPE. New acidic chain termini were observed by carbodiimide-mediated amidation of carboxylic acids as anilides of gluconic, arabinonic, and erythronic acids. Hence, a full characterization of all types of oxidation products was possible by combining complementary sample preparation strategies. Differences in fine structure depending on source (oat vs. barley) translates to the ratio of observed oxidized oligomers, with in-depth analysis corroborating a random HO•-attack on glucose units irrespective of glycosidic linkage and neighborhood. The method was demonstrated to be (1) sufficiently sensitive to allow for the analysis of oxidation products also from a mild ascorbate-driven Fenton reaction, and (2) to be specific for cereal β-glucan even in the presence of other co-oxidized polysaccharides. This opens doors to applications in food processing to assess potential oxidations and provides the detailed structural basis to understand the effect oxidized functional groups have on β-glucan's health promoting and technological properties. PMID:29164106

Complementary sample preparation strategies for analysis of cereal β-glucan oxidation products by UPLC-MS/MS

NASA Astrophysics Data System (ADS)

Boulos, Samy; Nyström, Laura

2017-11-01

The oxidation of cereal (1→3,1→4)-β-D-glucan can influence the health promoting and technological properties of this linear, soluble homopolysaccharide by introduction of new functional groups or chain scission. Apart from deliberate oxidative modifications, oxidation of β-glucan can already occur during processing and storage, which is mediated by hydroxyl radicals (HO•) formed by the Fenton reaction. We present four complementary sample preparation strategies to investigate oat and barley β-glucan oxidation products by hydrophilic interaction ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), employing selective enzymatic digestion, graphitized carbon solid phase extraction (SPE), and functional group labeling techniques. The combination of these methods allows for detection of both lytic (C1, C3/4, C5) and non-lytic (C2, C4/3, C6) oxidation products resulting from HO•-attack at different glucose-carbons. By treating oxidized β-glucan with lichenase and β-glucosidase, only oxidized parts of the polymer remained in oligomeric form, which could be separated by SPE from the vast majority of non-oxidized glucose units. This allowed for the detection of oligomers with mid-chain glucuronic acids (C6) and carbonyls, as well as carbonyls at the non-reducing end from lytic C3/C4 oxidation. Neutral reducing ends were detected by reductive amination with anthranilic acid/amide as labeled glucose and cross-ring cleaved units (arabinose, erythrose) after enzyme treatment and SPE. New acidic chain termini were observed by carbodiimide-mediated amidation of carboxylic acids as anilides of gluconic, arabinonic, and erythronic acids. Hence, a full characterization of all types of oxidation products was possible by combining complementary sample preparation strategies. Differences in fine structure depending on source (oat vs. barley) translates to the ratio of observed oxidized oligomers, with in-depth analysis corroborating a random HO•-attack on glucose units irrespective of glycosidic linkage and neighborhood. The method was demonstrated to be 1) sufficiently sensitive to allow for the analysis of oxidation products also from a mild ascorbate-driven Fenton reaction, and 2) to be specific for cereal β-glucan even in the presence of other co-oxidized polysaccharides. This opens doors to applications in food processing to assess potential oxidations and provides the detailed structural basis to understand the effect oxidized functional groups have on β-glucan’s health promoting and technological properties.

Improved Dielectric Properties via Mechano-Chemical Activation in Ba0.80Pb0.20TiO3 Ceramics

NASA Astrophysics Data System (ADS)

Kumar, Parveen; Rani, Renu; Singh, Sangeeta; Juneja, J. K.; Prakash, Chandra; Raina, K. K.

2011-12-01

The present report is about the preparation and dielectric properties of commonly used Ba0.80Pb0.20TiO3 (BPT) ferroelectric ceramic via Mechano-Chemical Activation (MCA). Results were compared by the BPT sample prepared by conventional solid state method. The BPT sample prepared via MCA technique was found to have decreased tetragonality, dielectric constant value (ɛRT = 450 and ɛmax = 6170) approximately double the value for sample prepared by conventional method (ɛRT = 260 and ɛmax = 3275). Also, the sample prepared by MCA was found to be less frequency dependent. Thus, the BPT sample prepared via MCA is more suitable for capacitor applications requiring lesser frequency dependency than the conventionally prepared BPT sample.

A protected annealing strategy to enhanced light emission and photostability of YAG:Ce nanoparticle-based films

NASA Astrophysics Data System (ADS)

Revaux, Amelie; Dantelle, Geraldine; George, Nathan; Seshadri, Ram; Gacoin, Thierry; Boilot, Jean-Pierre

2011-05-01

A significant obstacle in the development of YAG:Ce nanoparticles as light converters in white LEDs and as biological labels is associated with the difficulty of finding preparative conditions that allow simultaneous control of structure, particle size and size distribution, while maintaining the optical properties of bulk samples. Preparation conditions frequently involve high-temperature treatments of precursors (up to 1400 °C), which result in increased particle size and aggregation, and lead to oxidation of Ce(iii) to Ce(iv). We report here a process that we term protected annealing, that allows the thermal treatment of preformed precursor particles at temperatures up to 1000 °C while preserving their small size and state of dispersion. In a first step, pristine nanoparticles are prepared by a glycothermal reaction, leading to a mixture of YAG and boehmite crystalline phases. The preformed nanoparticles are then dispersed in a porous silica. Annealing of the composite material at 1000 °C is followed by dissolution of the amorphous silica by hydrofluoric acid to recover the annealed particles as a colloidal dispersion. This simple process allows completion of YAG crystallization while preserving their small size. The redox state of Ce ions can be controlled through the annealing atmosphere. The obtained particles of YAG:Ce (60 +/- 10 nm in size) can be dispersed as nearly transparent aqueous suspensions, with a luminescence quantum yield of 60%. Transparent YAG:Ce nanoparticle-based films of micron thickness can be deposited on glass substrates using aerosol spraying. Films formed from particles prepared by the protected annealing strategy display significantly improved photostability over particles that have not been subject to such annealing.A significant obstacle in the development of YAG:Ce nanoparticles as light converters in white LEDs and as biological labels is associated with the difficulty of finding preparative conditions that allow simultaneous control of structure, particle size and size distribution, while maintaining the optical properties of bulk samples. Preparation conditions frequently involve high-temperature treatments of precursors (up to 1400 °C), which result in increased particle size and aggregation, and lead to oxidation of Ce(iii) to Ce(iv). We report here a process that we term protected annealing, that allows the thermal treatment of preformed precursor particles at temperatures up to 1000 °C while preserving their small size and state of dispersion. In a first step, pristine nanoparticles are prepared by a glycothermal reaction, leading to a mixture of YAG and boehmite crystalline phases. The preformed nanoparticles are then dispersed in a porous silica. Annealing of the composite material at 1000 °C is followed by dissolution of the amorphous silica by hydrofluoric acid to recover the annealed particles as a colloidal dispersion. This simple process allows completion of YAG crystallization while preserving their small size. The redox state of Ce ions can be controlled through the annealing atmosphere. The obtained particles of YAG:Ce (60 +/- 10 nm in size) can be dispersed as nearly transparent aqueous suspensions, with a luminescence quantum yield of 60%. Transparent YAG:Ce nanoparticle-based films of micron thickness can be deposited on glass substrates using aerosol spraying. Films formed from particles prepared by the protected annealing strategy display significantly improved photostability over particles that have not been subject to such annealing. Electronic supplementary information (ESI) available: Thermogravimetric analysis curve, picture of a YAG:Ce3+ thin film. See DOI: 10.1039/c0nr01000f

Preparation and characterisation of core-shell CNTs@MIPs nanocomposites and selective removal of estrone from water samples.

PubMed

Gao, Ruixia; Su, Xiaoqian; He, Xiwen; Chen, Langxing; Zhang, Yukui

2011-01-15

This paper reports the preparation of carbon nanotubes (CNTs) functionalized with molecularly imprinted polymers (MIPs) for advanced removal of estrone. CNTs@Est-MIPs nanocomposites with a well-defined core-shell structure were obtained using a semi-covalent imprinting strategy, which employed a thermally reversible covalent bond at the surface of silica-coated CNTs for a large-scale production. The morphology and structure of the products were characterised by transmission electron microscopy and Fourier transform infrared spectroscopy. The adsorption properties were demonstrated by equilibrium rebinding experiments and Scatchard analysis. The results demonstrate that the imprinted nanocomposites possess favourable selectivity, high capacity and fast kinetics for template molecule uptake, yielding an adsorption capacity of 113.5 μmol/g. The synthetic process is quite simple, and the different batches of synthesized CNTs@Est-MIPs nanocomposites showed good reproducibility in template binding. The feasibility of removing estrogenic compounds from environmental water using the CNTs@Est-MIPs nanocomposites was demonstrated using water samples spiked with estrone. Copyright © 2010 Elsevier B.V. All rights reserved.

Applications of DART-MS for food quality and safety assurance in food supply chain.

PubMed

Guo, Tianyang; Yong, Wei; Jin, Yong; Zhang, Liya; Liu, Jiahui; Wang, Sai; Chen, Qilong; Dong, Yiyang; Su, Haijia; Tan, Tianwei

2017-03-01

Direct analysis in real time (DART) represents a new generation of ion source which is used for rapid ionization of small molecules under ambient conditions. The combination of DART and various mass spectrometers allows analyzing multiple food samples with simple or no sample treatment, or in conjunction with prevailing protocolized sample preparation methods. Abundant applications by DART-MS have been reviewed in this paper. The DART-MS strategy applied to food supply chain (FSC), including production, processing, and storage and transportation, provides a comprehensive solution to various food components, contaminants, authenticity, and traceability. Additionally, typical applications available in food analysis by other ambient ionization mass spectrometers were summarized, and fundamentals mainly including mechanisms, devices, and parameters were discussed as well. © 2015 Wiley Periodicals, Inc. Mass Spec Rev. 36:161-187, 2017. © 2015 Wiley Periodicals, Inc.

Preanalytical requirements of urinalysis

PubMed Central

Delanghe, Joris; Speeckaert, Marijn

2014-01-01

Urine may be a waste product, but it contains an enormous amount of information. Well-standardized procedures for collection, transport, sample preparation and analysis should become the basis of an effective diagnostic strategy for urinalysis. As reproducibility of urinalysis has been greatly improved due to recent technological progress, preanalytical requirements of urinalysis have gained importance and have become stricter. Since the patients themselves often sample urine specimens, urinalysis is very susceptible to preanalytical issues. Various sampling methods and inappropriate specimen transport can cause important preanalytical errors. The use of preservatives may be helpful for particular analytes. Unfortunately, a universal preservative that allows a complete urinalysis does not (yet) exist. The preanalytical aspects are also of major importance for newer applications (e.g. metabolomics). The present review deals with the current preanalytical problems and requirements for the most common urinary analytes. PMID:24627718

Recent advances in applications of nanomaterials for sample preparation.

PubMed

Xu, Linnan; Qi, Xiaoyue; Li, Xianjiang; Bai, Yu; Liu, Huwei

2016-01-01

Sample preparation is a key step for qualitative and quantitative analysis of trace analytes in complicated matrix. Along with the rapid development of nanotechnology in material science, numerous nanomaterials have been developed with particularly useful applications in analytical chemistry. Benefitting from their high specific areas, increased surface activities, and unprecedented physical/chemical properties, the potentials of nanomaterials for rapid and efficient sample preparation have been exploited extensively. In this review, recent progress of novel nanomaterials applied in sample preparation has been summarized and discussed. Both nanoparticles and nanoporous materials are evaluated for their unusual performance in sample preparation. Various compositions and functionalizations extended the applications of nanomaterials in sample preparations, and distinct size and shape selectivity was generated from the diversified pore structures of nanoporous materials. Such great variety make nanomaterials a kind of versatile tools in sample preparation for almost all categories of analytes. Copyright © 2015 Elsevier B.V. All rights reserved.

The Recent Developments in Sample Preparation for Mass Spectrometry-Based Metabolomics.

PubMed

Gong, Zhi-Gang; Hu, Jing; Wu, Xi; Xu, Yong-Jiang

2017-07-04

Metabolomics is a critical member in systems biology. Although great progress has been achieved in metabolomics, there are still some problems in sample preparation, data processing and data interpretation. In this review, we intend to explore the roles, challenges and trends in sample preparation for mass spectrometry- (MS-) based metabolomics. The newly emerged sample preparation methods were also critically examined, including laser microdissection, in vivo sampling, dried blood spot, microwave, ultrasound and enzyme-assisted extraction, as well as microextraction techniques. Finally, we provide some conclusions and perspectives for sample preparation in MS-based metabolomics.

A novel ultra high-throughput 16S rRNA gene amplicon sequencing library preparation method for the Illumina HiSeq platform.

PubMed

de Muinck, Eric J; Trosvik, Pål; Gilfillan, Gregor D; Hov, Johannes R; Sundaram, Arvind Y M

2017-07-06

Advances in sequencing technologies and bioinformatics have made the analysis of microbial communities almost routine. Nonetheless, the need remains to improve on the techniques used for gathering such data, including increasing throughput while lowering cost and benchmarking the techniques so that potential sources of bias can be better characterized. We present a triple-index amplicon sequencing strategy to sequence large numbers of samples at significantly lower c ost and in a shorter timeframe compared to existing methods. The design employs a two-stage PCR protocol, incorpo rating three barcodes to each sample, with the possibility to add a fourth-index. It also includes heterogeneity spacers to overcome low complexity issues faced when sequencing amplicons on Illumina platforms. The library preparation method was extensively benchmarked through analysis of a mock community in order to assess biases introduced by sample indexing, number of PCR cycles, and template concentration. We further evaluated the method through re-sequencing of a standardized environmental sample. Finally, we evaluated our protocol on a set of fecal samples from a small cohort of healthy adults, demonstrating good performance in a realistic experimental setting. Between-sample variation was mainly related to batch effects, such as DNA extraction, while sample indexing was also a significant source of bias. PCR cycle number strongly influenced chimera formation and affected relative abundance estimates of species with high GC content. Libraries were sequenced using the Illumina HiSeq and MiSeq platforms to demonstrate that this protocol is highly scalable to sequence thousands of samples at a very low cost. Here, we provide the most comprehensive study of performance and bias inherent to a 16S rRNA gene amplicon sequencing method to date. Triple-indexing greatly reduces the number of long custom DNA oligos required for library preparation, while the inclusion of variable length heterogeneity spacers minimizes the need for PhiX spike-in. This design results in a significant cost reduction of highly multiplexed amplicon sequencing. The biases we characterize highlight the need for highly standardized protocols. Reassuringly, we find that the biological signal is a far stronger structuring factor than the various sources of bias.

Multiscale microstructures and improved thermoelectric performance of Mg2(Si0.4Sn0.6)Sbx solid solutions

NASA Astrophysics Data System (ADS)

Zhang, Xin; Liu, Hongliang; Li, Songhao; Zhang, Feipeng; Lu, Qingmei; Li, Jingfeng

2014-03-01

A series of Sb-doped Mg2(Si0.4Sn0.6)Sbx (0 ≤ x ≤ 0.025) solid solutions were prepared by an induction melting, Melt Spinning (MS) and Spark Plasma Sintering (SPS) method, namely the non-equilibrium technique MS-SPS, using bulks of Magnesium, Silicon, Tin, and Antimony as raw materials. The non-equilibrium technique generates the unique multiscale microstructures of samples containing micronscale grains and nanoscale precipitates, the multiscale microstructures remarkably make the lattice thermal conductivities decreased, particularly for samples with the nanoscale precipitates having the size of 10-20 nm. Meanwhile, Sb-doping greatly increased the electrical performance of samples. Consequently, the Sb-doping combined with the multiscale microstructures strategy remarkably improves the overall thermoelectric (TE) performance of Sb doped samples, and a high dimensionless figure of merit (ZT) value of up to 1.25 at 723 K is obtained with Mg2(Si0.4Sn0.6)Sb0.02 sample in a relatively wide temperature range.

Cassidy conducts BASS Experiment Test Operations

NASA Image and Video Library

2013-04-05

ISS035-E-015081 (5 April 2013) --- Astronaut Chris Cassidy, Expedition 35 flight engineer, conducts a session of the Burning and Suppression of Solids (BASS) experiment onboard the Earth-orbiting International Space Station. Following a series of preparations, Cassidy conducted a run of the experiment, which examined the burning and extinction characteristics of a wide variety of fuel samples in microgravity and will guide strategies for extinguishing fires in microgravity. BASS results contribute to the combustion computational models used in the design of fire detection and suppression systems in microgravity and on Earth.

Visualizing fungal metabolites during mycoparasitic interaction by MALDI mass spectrometry imaging

PubMed Central

Holzlechner, Matthias; Reitschmidt, Sonja; Gruber, Sabine; Zeilinger, Susanne

2016-01-01

Studying microbial interactions by MALDI mass spectrometry imaging (MSI) directly from growing media is a difficult task if high sensitivity is demanded. We present a quick and robust sample preparation strategy for growing fungi (Trichoderma atroviride, Rhizoctonia solani) on glass slides to establish a miniaturized confrontation assay. By this we were able to visualize metabolite distributions by MALDI MSI after matrix deposition with a home‐built sublimation device and thorough recrystallization. We present for the first time MALDI MSI data for secondary metabolite release during active mycoparasitism. PMID:26959280

[Advances in mass spectrometry-based approaches for neuropeptide analysis].

PubMed

Ji, Qianyue; Ma, Min; Peng, Xin; Jia, Chenxi; Ji, Qianyue

2017-07-25

Neuropeptides are an important class of endogenous bioactive substances involved in the function of the nervous system, and connect the brain and other neural and peripheral organs. Mass spectrometry-based neuropeptidomics are designed to study neuropeptides in a large-scale manner and obtain important molecular information to further understand the mechanism of nervous system regulation and the pathogenesis of neurological diseases. This review summarizes the basic strategies for the study of neuropeptides using mass spectrometry, including sample preparation and processing, qualitative and quantitative methods, and mass spectrometry imagining.

EOS Laser Atmosphere Wind Sounder (LAWS) investigation

NASA Technical Reports Server (NTRS)

Emmitt, George D.

1991-01-01

The related activities of the contract are outlined for the first year. These include: (1) attend team member meetings; (2) support EOS Project with science related activities; (3) prepare and Execution Phase plan; and (4) support LAWS and EOSDIS related work. Attached to the report is an appendix, 'LAWS Algorithm Development and Evaluation Laboratory (LADEL)'. Also attached is a copy of a proposal to the NASA EOS for 'LAWS Sampling Strategies and Wind Computation Algorithms -- Storm-Top Divergence Studies. Volume I: Investigation and Technical Plan, Data Plan, Computer Facilities Plan, Management Plan.'

"Sign-on/off" sensing interface design and fabrication for propyl gallate recognition and sensitive detection.

PubMed

Dai, Yunlong; Li, Xueyan; Fan, Limei; Lu, Xiaojing; Kan, Xianwen

2016-12-15

A new strategy based on sign-on and sign-off was proposed for propyl gallate (PG) determination by an electrochemical sensor. The successively modified poly(thionine) (PTH) and molecular imprinted polymer (MIP) showed an obvious electrocatalysis and a good recognition toward PG, respectively. Furthermore, the rebound PG molecules in imprinted cavities not only were oxidized but also blocked the electron transmission channels for PTH redox. Thus, a sign-on from PG current and a sign-off from PTH current were combined as a dual-sign for PG detection. Meanwhile, the modified MIP endowed the sensor with recognition capacity. The electrochemical experimental results demonstrated that the prepared sensor possessed good selectivity and high sensitivity. A linear ranging from 5.0×10(-8) to 1.0×10(-4)mol/L for PG detection was obtained with a limit of detection of 2.4×10(-8)mol/L. And the sensor has been applied to analyze PG in real samples with satisfactory results. The simple, low cost, and effective strategy reported here can be further used to prepare electrochemical sensors for other compounds selective recognition and sensitive detection. Copyright © 2016 Elsevier B.V. All rights reserved.

Opportunistic Resource Usage in CMS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kreuzer, Peter; Hufnagel, Dirk; Dykstra, D.

2014-01-01

CMS is using a tiered setup of dedicated computing resources provided by sites distributed over the world and organized in WLCG. These sites pledge resources to CMS and are preparing them especially for CMS to run the experiment's applications. But there are more resources available opportunistically both on the GRID and in local university and research clusters which can be used for CMS applications. We will present CMS' strategy to use opportunistic resources and prepare them dynamically to run CMS applications. CMS is able to run its applications on resources that can be reached through the GRID, through EC2 compliantmore » cloud interfaces. Even resources that can be used through ssh login nodes can be harnessed. All of these usage modes are integrated transparently into the GlideIn WMS submission infrastructure, which is the basis of CMS' opportunistic resource usage strategy. Technologies like Parrot to mount the software distribution via CVMFS and xrootd for access to data and simulation samples via the WAN are used and will be described. We will summarize the experience with opportunistic resource usage and give an outlook for the restart of LHC data taking in 2015.« less

Optimization and validation of sample preparation for metagenomic sequencing of viruses in clinical samples.

PubMed

Lewandowska, Dagmara W; Zagordi, Osvaldo; Geissberger, Fabienne-Desirée; Kufner, Verena; Schmutz, Stefan; Böni, Jürg; Metzner, Karin J; Trkola, Alexandra; Huber, Michael

2017-08-08

Sequence-specific PCR is the most common approach for virus identification in diagnostic laboratories. However, as specific PCR only detects pre-defined targets, novel virus strains or viruses not included in routine test panels will be missed. Recently, advances in high-throughput sequencing allow for virus-sequence-independent identification of entire virus populations in clinical samples, yet standardized protocols are needed to allow broad application in clinical diagnostics. Here, we describe a comprehensive sample preparation protocol for high-throughput metagenomic virus sequencing using random amplification of total nucleic acids from clinical samples. In order to optimize metagenomic sequencing for application in virus diagnostics, we tested different enrichment and amplification procedures on plasma samples spiked with RNA and DNA viruses. A protocol including filtration, nuclease digestion, and random amplification of RNA and DNA in separate reactions provided the best results, allowing reliable recovery of viral genomes and a good correlation of the relative number of sequencing reads with the virus input. We further validated our method by sequencing a multiplexed viral pathogen reagent containing a range of human viruses from different virus families. Our method proved successful in detecting the majority of the included viruses with high read numbers and compared well to other protocols in the field validated against the same reference reagent. Our sequencing protocol does work not only with plasma but also with other clinical samples such as urine and throat swabs. The workflow for virus metagenomic sequencing that we established proved successful in detecting a variety of viruses in different clinical samples. Our protocol supplements existing virus-specific detection strategies providing opportunities to identify atypical and novel viruses commonly not accounted for in routine diagnostic panels.

On the use of ultracentrifugal devices for routine sample preparation in biomolecular magic-angle-spinning NMR

PubMed Central

Mandal, Abhishek; Boatz, Jennifer C.; Wheeler, Travis; van der Wel, Patrick C. A.

2017-01-01

A number of recent advances in the field of magic-angle-spinning (MAS) solid-state NMR have enabled its application to a range of biological systems of ever increasing complexity. To retain biological relevance, these samples are increasingly studied in a hydrated state. At the same time, experimental feasibility requires the sample preparation process to attain a high sample concentration within the final MAS rotor. We discuss these considerations, and how they have led to a number of different approaches to MAS NMR sample preparation. We describe our experience of how custom-made (or commercially available) ultracentrifugal devices can facilitate a simple, fast and reliable sample preparation process. A number of groups have since adopted such tools, in some cases to prepare samples for sedimentation-style MAS NMR experiments. Here we argue for a more widespread adoption of their use for routine MAS NMR sample preparation. PMID:28229262

Clinically relevant advances in on-chip affinity-based electrophoresis and electrochromatography.

PubMed

Hou, Chenlu; Herr, Amy E

2008-08-01

Clinical and point-of-care disease diagnostics promise to play an important role in personalized medicine, new approaches to global health, and health monitoring. Emerging instrument platforms based on lab-on-a-chip technology can confer performance advantages successfully exploited in electrophoresis and electrochromatography to affinity-based electrokinetic separations. This review surveys lab-on-a-chip diagnostic developments in affinity-based electrokinetic separations for quantitation of proteins, integration of preparatory functions needed for subsequent analysis of diverse biological samples, and initial forays into multiplexed analyses. The technologies detailed here underpin new clinical and point-of-care diagnostic strategies. The techniques and devices promise to advance translation of until now laboratory-based sample preparation and analytical assays to near-patient settings.

Comparison of active and passive sampling strategies for the monitoring of pesticide contamination in streams

NASA Astrophysics Data System (ADS)

Assoumani, Azziz; Margoum, Christelle; Guillemain, Céline; Coquery, Marina

2014-05-01

The monitoring of water bodies regarding organic contaminants, and the determination of reliable estimates of concentrations are challenging issues, in particular for the implementation of the Water Framework Directive. Several strategies can be applied to collect water samples for the determination of their contamination level. Grab sampling is fast, easy, and requires little logistical and analytical needs in case of low frequency sampling campaigns. However, this technique lacks of representativeness for streams with high variations of contaminant concentrations, such as pesticides in rivers located in small agricultural watersheds. Increasing the representativeness of this sampling strategy implies greater logistical needs and higher analytical costs. Average automated sampling is therefore a solution as it allows, in a single analysis, the determination of more accurate and more relevant estimates of concentrations. Two types of automatic samplings can be performed: time-related sampling allows the assessment of average concentrations, whereas flow-dependent sampling leads to average flux concentrations. However, the purchase and the maintenance of automatic samplers are quite expensive. Passive sampling has recently been developed as an alternative to grab or average automated sampling, to obtain at lower cost, more realistic estimates of the average concentrations of contaminants in streams. These devices allow the passive accumulation of contaminants from large volumes of water, resulting in ultratrace level detection and smoothed integrative sampling over periods ranging from days to weeks. They allow the determination of time-weighted average (TWA) concentrations of the dissolved fraction of target contaminants, but they need to be calibrated in controlled conditions prior to field applications. In other words, the kinetics of the uptake of the target contaminants into the sampler must be studied in order to determine the corresponding sampling rate constants (Rs). Each constant links the mass of the a target contaminant accumulated in the sampler to its concentration in water. At the end of the field application, the Rs are used to calculate the TWA concentration of each target contaminant with the final mass of the contaminants accumulated in the sampler. Stir Bar Sorptive Extraction (SBSE) is a solvent free sample preparation technique dedicated to the analysis of moderately hydrophobic to hydrophobic compounds in liquid and gas samples. It is composed of a magnet enclosed in a glass tube coated with a thick film of polydimethysiloxane (PDMS). We recently developed the in situ application of SBSE as a passive sampling technique (herein named "Passive SBSE") for the monitoring of agricultural pesticides. The aim of this study is to perform the calibration of the passive SBSE in the laboratory, and to apply and compare this technique to active sampling strategies for the monitoring of 16 relatively hydrophobic to hydrophobic pesticides in streams, during 2 1-month sampling campaigns. Time-weighted averaged concentrations of the target pesticides obtained from passive SBSE were compared to the target pesticide concentrations of grab samples, and time-related and flow-dependent samples of the streams. Results showed passive SBSE as an efficient alternative to conventional active sampling strategies.

Optimal selection of epitopes for TXP-immunoaffinity mass spectrometry.

PubMed

Planatscher, Hannes; Supper, Jochen; Poetz, Oliver; Stoll, Dieter; Joos, Thomas; Templin, Markus F; Zell, Andreas

2010-06-25

Mass spectrometry (MS) based protein profiling has become one of the key technologies in biomedical research and biomarker discovery. One bottleneck in MS-based protein analysis is sample preparation and an efficient fractionation step to reduce the complexity of the biological samples, which are too complex to be analyzed directly with MS. Sample preparation strategies that reduce the complexity of tryptic digests by using immunoaffinity based methods have shown to lead to a substantial increase in throughput and sensitivity in the proteomic mass spectrometry approach. The limitation of using such immunoaffinity-based approaches is the availability of the appropriate peptide specific capture antibodies. Recent developments in these approaches, where subsets of peptides with short identical terminal sequences can be enriched using antibodies directed against short terminal epitopes, promise a significant gain in efficiency. We show that the minimal set of terminal epitopes for the coverage of a target protein list can be found by the formulation as a set cover problem, preceded by a filtering pipeline for the exclusion of peptides and target epitopes with undesirable properties. For small datasets (a few hundred proteins) it is possible to solve the problem to optimality with moderate computational effort using commercial or free solvers. Larger datasets, like full proteomes require the use of heuristics.

Minimizing back exchange in the hydrogen exchange-mass spectrometry experiment.

PubMed

Walters, Benjamin T; Ricciuti, Alec; Mayne, Leland; Englander, S Walter

2012-12-01

The addition of mass spectrometry (MS) analysis to the hydrogen exchange (HX) proteolytic fragmentation experiment extends powerful HX methodology to the study of large biologically important proteins. A persistent problem is the degradation of HX information due to back exchange of deuterium label during the fragmentation-separation process needed to prepare samples for MS measurement. This paper reports a systematic analysis of the factors that influence back exchange (solution pH, ionic strength, desolvation temperature, LC column interaction, flow rates, system volume). The many peptides exhibit a range of back exchange due to intrinsic amino acid HX rate differences. Accordingly, large back exchange leads to large variability in D-recovery from one residue to another as well as one peptide to another that cannot be corrected for by reference to any single peptide-level measurement. The usual effort to limit back exchange by limiting LC time provides little gain. Shortening the LC elution gradient by 3-fold only reduced back exchange by ~2%, while sacrificing S/N and peptide count. An unexpected dependence of back exchange on ionic strength as well as pH suggests a strategy in which solution conditions are changed during sample preparation. Higher salt should be used in the first stage of sample preparation (proteolysis and trapping) and lower salt (<20 mM) and pH in the second stage before electrospray injection. Adjustment of these and other factors together with recent advances in peptide fragment detection yields hundreds of peptide fragments with D-label recovery of 90% ± 5%.

Assays for therapeutic drug monitoring of β-lactam antibiotics: A structured review.

PubMed

Carlier, Mieke; Stove, Veronique; Wallis, Steven C; De Waele, Jan J; Verstraete, Alain G; Lipman, Jeffrey; Roberts, Jason A

2015-10-01

In some patient groups, including critically ill patients, the pharmacokinetics of β-lactam antibiotics may be profoundly disturbed due to pathophysiological changes in distribution and elimination. Therapeutic drug monitoring (TDM) is a strategy that may help to optimise dosing. The aim of this review was to identify and analyse the published literature on the methods used for β-lactam quantification in TDM programmes. Sixteen reports described methods for the simultaneous determination of three or more β-lactam antibiotics in plasma/serum. Measurement of these antibiotics, due to low frequency of usage relative to some other tests, is generally limited to in-house chromatographic methods coupled to ultraviolet or mass spectrometric detection. Although many published methods state they are fit for TDM, they are inconvenient because of intensive sample preparation and/or long run times. Ideally, methods used for routine TDM should have a short turnaround time (fast run-time and fast sample preparation), a low limit of quantification and a sufficiently high upper limit of quantification. The published assays included a median of 6 analytes [interquartile range (IQR) 4-10], with meropenem and piperacillin being the most frequently measured β-lactam antibiotics. The median run time was 8 min (IQR 5.9-21.3 min). There is also a growing number of methods measuring free concentrations. An assay that measures antibiotics without any sample preparation would be the next step towards real-time monitoring; no such method is currently available. Copyright © 2015 Elsevier B.V. and the International Society of Chemotherapy. All rights reserved.

Minimizing Back Exchange in the Hydrogen Exchange-Mass Spectrometry Experiment

NASA Astrophysics Data System (ADS)

Walters, Benjamin T.; Ricciuti, Alec; Mayne, Leland; Englander, S. Walter

2012-12-01

The addition of mass spectrometry (MS) analysis to the hydrogen exchange (HX) proteolytic fragmentation experiment extends powerful HX methodology to the study of large biologically important proteins. A persistent problem is the degradation of HX information due to back exchange of deuterium label during the fragmentation-separation process needed to prepare samples for MS measurement. This paper reports a systematic analysis of the factors that influence back exchange (solution pH, ionic strength, desolvation temperature, LC column interaction, flow rates, system volume). The many peptides exhibit a range of back exchange due to intrinsic amino acid HX rate differences. Accordingly, large back exchange leads to large variability in D-recovery from one residue to another as well as one peptide to another that cannot be corrected for by reference to any single peptide-level measurement. The usual effort to limit back exchange by limiting LC time provides little gain. Shortening the LC elution gradient by 3-fold only reduced back exchange by ~2 %, while sacrificing S/N and peptide count. An unexpected dependence of back exchange on ionic strength as well as pH suggests a strategy in which solution conditions are changed during sample preparation. Higher salt should be used in the first stage of sample preparation (proteolysis and trapping) and lower salt (<20 mM) and pH in the second stage before electrospray injection. Adjustment of these and other factors together with recent advances in peptide fragment detection yields hundreds of peptide fragments with D-label recovery of 90 % ± 5 %.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Scheele, R.D.

In 1995, available subsegment samples of wastes taken from the Hanford Site underground radioactive waste storage tanks 241-C-112 (C-112) and 241-C-109 (C-109) were reanalyzed to determine the nickel concentrations in the samples and to determine whether the use of a nickel crucible in the analytical sample preparation biased the reported nickel concentrations reported by Simpson and coworkers and in the original report that this report supplements. The reanalysis strategy to determine nickel was to use a sodium peroxide flux in a zirconium crucible instead of the previously used potassium hydroxide flux in a nickel crucible. This supplemental report provides themore » results of the reanalyses and updates tables from the original report which reflect the new nickel analyses. Nickel is important with respect to management of the potentially reactive ferrocyanide wastes as it is one of the key defining characteristics of the solids that resulted from scavenging radiocesium using ferrocyanides. In Hanford Site wastes, few other processes introduced nickel into the wastes other than radiocobalt scavenging, which was often coupled with the ferrocyanide-scavenging process. Thus the presence of nickel in a waste provides strong evidence that the original waste was or contained ferrocyanide waste at one time. Given the potential import of nickel as a defining characteristic and marker for ferrocyanide wastes, the Pacific Northwest Laboratory`s (PNL) Analytical Chemistry Laboratory (ACL) reanalyzed available samples from tanks C-112 and C-109 using inductively coupled argon plasma/atomic emission spectrometry (ICP/AES) and an alternative sample preparation method which precluded contamination of the analytical samples with nickel.« less

A ratiometric strategy -based electrochemical sensing interface for the sensitive and reliable detection of imidacloprid.

PubMed

Li, Xueyan; Kan, Xianwen

2018-04-30

In this study, a ratiometric strategy-based electrochemical sensor was developed by electropolymerization of thionine (THI) and β-cyclodextrin (β-CD) composite films on a glassy carbon electrode surface for imidacloprid (IMI) detection. THI played the role of an inner reference element to provide a built-in correction. In addition, the modified β-CD showed good selective enrichment for IMI to improve the sensitivity and anti-interference ability of the sensor. The current ratio between IMI and THI was calculated as the detected signal for IMI sensing. Compared with common single-signal sensing, the proposed ratiometric strategy showed a higher linear range and a lower limit of detection of 4.0 × 10-8-1.0 × 10-5 mol L-1 and 1.7 × 10-8 mol L-1, respectively, for IMI detection. On the other hand, the ratiometric strategy endowed the sensor with good accuracy, reproducibility, and stability. The sensor was also used for IMI determination in real samples with satisfactory results. The simple, effective, and reliable way reported in this study can be further used to prepare ratiometric strategy-based electrochemical sensors for the selective and sensitive detection of other compounds with good accuracy and stability.

A protected annealing strategy to enhanced light emission and photostability of YAG:Ce nanoparticle-based films.

PubMed

Revaux, Amelie; Dantelle, Geraldine; George, Nathan; Seshadri, Ram; Gacoin, Thierry; Boilot, Jean-Pierre

2011-05-01

A significant obstacle in the development of YAG:Ce nanoparticles as light converters in white LEDs and as biological labels is associated with the difficulty of finding preparative conditions that allow simultaneous control of structure, particle size and size distribution, while maintaining the optical properties of bulk samples. Preparation conditions frequently involve high-temperature treatments of precursors (up to 1400 °C), which result in increased particle size and aggregation, and lead to oxidation of Ce(iii) to Ce(iv). We report here a process that we term protected annealing, that allows the thermal treatment of preformed precursor particles at temperatures up to 1000 °C while preserving their small size and state of dispersion. In a first step, pristine nanoparticles are prepared by a glycothermal reaction, leading to a mixture of YAG and boehmite crystalline phases. The preformed nanoparticles are then dispersed in a porous silica. Annealing of the composite material at 1000 °C is followed by dissolution of the amorphous silica by hydrofluoric acid to recover the annealed particles as a colloidal dispersion. This simple process allows completion of YAG crystallization while preserving their small size. The redox state of Ce ions can be controlled through the annealing atmosphere. The obtained particles of YAG:Ce (60 ± 10 nm in size) can be dispersed as nearly transparent aqueous suspensions, with a luminescence quantum yield of 60%. Transparent YAG:Ce nanoparticle-based films of micron thickness can be deposited on glass substrates using aerosol spraying. Films formed from particles prepared by the protected annealing strategy display significantly improved photostability over particles that have not been subject to such annealing. © The Royal Society of Chemistry 2011

Classroom Participation Strategy in Principles of Finance Courses

ERIC Educational Resources Information Center

Fewings, David R.; Wonder, Nicholas X.

2009-01-01

The challenge of introductory finance courses often surprises junior level university students. This paper describes a strategy that effectively motivates students to prepare solutions to problems for each class and to be prepared to check work presented by classmates. Empirically, the participation grade was found to be positively and…

Developing Democratic and Transformational School Leaders: Graduates' Perceptions of the Impact of Their Preparation Program

ERIC Educational Resources Information Center

Stevenson, Robert B.; Doolittle, Gini

2003-01-01

As administrative preparation programs ground strategies for developing new genres of school leaders in transformational and democratic communities, of particular interest are the instructional and programmatic strategies that contribute to successful program outcomes. Constructed over time, this article highlights the specific contribution of…

The Meaning of Visual Thinking Strategies for Nursing Students

ERIC Educational Resources Information Center

Moorman, Margaret M.

2013-01-01

Nurse educators are called upon to provide creative, innovative experiences for students in order to prepare nurses to work in complex healthcare settings. As part of this preparation, teaching observational and communication skills is critical for nurses and can directly affect patient outcomes. Visual thinking strategies (VTS) are a teaching…

Preparing Teachers To Help Children and Families of Divorce.

ERIC Educational Resources Information Center

Kramer, Pamela A.

A survey of 25 institutions of higher education was completed to identify strategies that are being used to prepare future teachers to help children and families of divorce. Ten individual strategies are discussed, including case studies, journal articles and reflective papers, use of children's literature, student teaching experiences, and…

Pacesetting Schools Share Successful Strategies to Prepare Students for the Future. Best Practices Newsletter

ERIC Educational Resources Information Center

Southern Regional Education Board (SREB), 2013

2013-01-01

Pacesetting high schools, middle grades schools and technology centers have changed classroom and other practices to prepare students to meet postsecondary requirements and rising workplace needs. The strategies include raising expectations, project-based learning, guidance and advisement, improving students' reading and writing skills,…

A "three-in-one" sample preparation method for simultaneous determination of B-group water-soluble vitamins in infant formula using VitaFast(®) kits.

PubMed

Zhang, Heng; Lan, Fang; Shi, Yupeng; Wan, Zhi-Gang; Yue, Zhen-Feng; Fan, Fang; Lin, Yan-Kui; Tang, Mu-Jin; Lv, Jing-Zhang; Xiao, Tan; Yi, Changqing

2014-06-15

VitaFast(®) test kits designed for the microbiological assay in microtiter plate format can be applied to quantitative determination of B-group water-soluble vitamins such as vitamin B12, folic acid and biotin, et al. Compared to traditional microbiological methods, VitaFast(®) kits significantly reduce sample processing time and provide greater reliability, higher productivity and better accuracy. Recently, simultaneous determination of vitamin B12, folic acid and biotin in one sample is urgently required when evaluating the quality of infant formulae in our practical work. However, the present sample preparation protocols which are developed for individual test systems, are incompatible with simultaneous determination of several analytes. To solve this problem, a novel "three-in-one" sample preparation method is herein developed for simultaneous determination of B-group water-soluble vitamins using VitaFast(®) kits. The performance of this novel "three-in-one" sample preparation method was systematically evaluated through comparing with individual sample preparation protocols. The experimental results of the assays which employed "three-in-one" sample preparation method were in good agreement with those obtained from conventional VitaFast(®) extraction methods, indicating that the proposed "three-in-one" sample preparation method is applicable to the present three VitaFast(®) vitamin test systems, thus offering a promising alternative for the three independent sample preparation methods. The proposed new sample preparation method will significantly improve the efficiency of infant formulae inspection. Copyright © 2013 Elsevier Ltd. All rights reserved.

Simple preparation of fluorescent composite films based on cerium and europium doped LaF3 nanoparticles

NASA Astrophysics Data System (ADS)

Secco, Henrique de L.; Ferreira, Fabio F.; Péres, Laura O.

2018-03-01

The combination of materials to form hybrids with unique properties, different from those of the isolated components, is a strategy used to prepare functional materials with improved properties aiming to allow their application in specific fields. The doping of lanthanum fluoride with other rare earth elements is used to obtain luminescent particles, which may be useful to the manufacturing of electronic devices' displays and biological markers, for instance. The application of the powder of nanoparticles has limitations in some fields; to overcome this, the powder may be incorporated in a suitable polymeric matrix. In this work, lanthanum fluoride nanoparticles, undoped and doped with cerium and europium, were synthesized through the co-precipitation method in aqueous solution. Aiming the formation of solid state films, composites of nanoparticles in an elastomeric matrix, the nitrile rubber (NBR), were prepared. The flexibility and the transparency of the matrix in the regions of interest are advantages for the application of the luminescent composites. The composites were applied as films using the casting and the spin coating techniques and luminescent materials were obtained in the samples doped with europium and cerium. Scanning electron microscopy images showed an adequate dispersion of the particles in the matrix in both film formation techniques. Aggregates of the particles were detected in the samples which may affect the uniformity of the emission of the composites.

Standardized Sample Preparation Using a Drop-on-Demand Printing Platform

DTIC Science & Technology

2013-05-07

successful and robust methodology for energetic sample preparation. Keywords: drop-on-demand; inkjet printing; sample preparation OPEN ACCESS...on a similar length scale. Recently, drop-on-demand inkjet printing technology has emerged as an effective approach to produce test materials to...which most of the material is concentrated along the edges, samples prepared using drop-on-demand inkjet technology demonstrate excellent uniform

Coping with Work-related Traumatic Situations among Crime Scene Technicians.

PubMed

Pavšič Mrevlje, Tinkara

2016-10-01

Crime scene technicians collect evidence related to crime and are therefore exposed to many traumatic situations. The coping strategies they use are thus very important in the process of facing the psychological consequences of such work. The available literature shows that crime scene technicians are an understudied subgroup of police workers. Our study is therefore the first unfolding insights into technicians' coping strategies, post-traumatic symptomatology and somatic health, based on a sample of 64 male crime scene technicians (85% of all Slovene technicians). Crime scene technicians mainly use avoidance coping strategies. Approach strategies that are more effective in the long-term-i.e. lead to a larger buffering of the effects of traumatic stress-are more frequently used if technicians are familiar with the nature of the task, when they have time to prepare for it, and if they feel that past situations have been positively resolved. Behavioural avoidance strategies were found to be least effective when dealing with traumatic experiences and are also related to more frequent problems of physical health. Results indicate that appropriate trainings for future technicians would facilitate the use of more effective coping strategies and consequently lead to a more effective and satisfied worker. Copyright © 2014 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

Identification and quantification of nitrofurazone metabolites by ultraperformance liquid chromatography-quadrupole time-of-flight high-resolution mass spectrometry with precolumn derivatization.

PubMed

Zhang, Shuai; Li, PeiPei; Yan, Zhongyong; Long, Ju; Zhang, Xiaojun

2017-03-01

An ultraperformance liquid chromatography-quadrupole time-of-flight high-resolution mass spectrometry method was developed and validated for the determination of nitrofurazone metabolites. Precolumn derivatization with 2,4-dinitrophenylhydrazine and p-dimethylaminobenzaldehyde as an internal standard was used successfully to determine the biomarker 5-nitro-2-furaldehyde. In negative electrospray ionization mode, the precise molecular weights of the derivatives were 320.0372 for the biomarker and 328.1060 for the internal standard (relative error 1.08 ppm). The matrix effect was evaluated and the analytical characteristics of the method and derivatization reaction conditions were validated. For comparison purposes, spiked samples were tested by both internal and external standard methods. The results show high precision can be obtained with p-dimethylaminobenzaldehyde as an internal standard for the identification and quantification of nitrofurazone metabolites in complex biological samples. Graphical Abstract A simplified preparation strategy for biological samples.

Soil and leaf litter metaproteomics—a brief guideline from sampling to understanding

PubMed Central

Keiblinger, Katharina M.; Fuchs, Stephan; Zechmeister-Boltenstern, Sophie; Riedel, Katharina

2016-01-01

The increasing application of soil metaproteomics is providing unprecedented, in-depth characterization of the composition and functionality of in situ microbial communities. Despite recent advances in high-resolution mass spectrometry, soil metaproteomics still suffers from a lack of effective and reproducible protein extraction protocols and standardized data analyses. This review discusses the opportunities and limitations of selected techniques in soil-, and leaf litter metaproteomics, and presents a step-by-step guideline on their application, covering sampling, sample preparation, extraction and data evaluation strategies. In addition, we present recent applications of soil metaproteomics and discuss how such approaches, linking phylogenetics and functionality, can help gain deeper insights into terrestrial microbial ecology. Finally, we strongly recommend that to maximize the insights environmental metaproteomics may provide, such methods should be employed within a holistic experimental approach considering relevant aboveground and belowground ecosystem parameters. PMID:27549116

VUV absorption spectroscopy of bacterial spores and DNA components

NASA Astrophysics Data System (ADS)

Fiebrandt, Marcel; Lackmann, Jan-Wilm; Raguse, Marina; Moeller, Ralf; Awakowicz, Peter; Stapelmann, Katharina

2017-01-01

Low-pressure plasmas can be used to inactivate bacterial spores and sterilize goods for medical and pharmaceutical applications. A crucial factor are damages induced by UV and VUV radiation emitted by the plasma. To analyze inactivation processes and protection strategies of spores, absorption spectra of two B. subtilis strains are measured. The results indicate, that the inner and outer coat of the spore significantly contribute to the absorption of UV-C and also of the VUV, protecting the spore against radiation based damages. As the sample preparation can significantly influence the absorption spectra due to salt residues, the cleaning procedure and sample deposition is tested for its reproducibility by measuring DNA oligomers and pUC18 plasmid DNA. The measurements are compared and discussed with results from the literature, showing a strong decrease of the salt content enabling the detection of absorption structures in the samples.

Colorimetric and Fluorescent Dual Mode Sensing of Alcoholic Strength in Spirit Samples with Stimuli-Responsive Infinite Coordination Polymers.

PubMed

Deng, Jingjing; Ma, Wenjie; Yu, Ping; Mao, Lanqun

2015-07-07

This study demonstrates a new strategy for colorimetric and fluorescent dual mode sensing of alcoholic strength (AS) in spirit samples based on stimuli-responsive infinite coordination polymers (ICPs). The ICP supramolecular network is prepared with 1,4-bis(imidazol-1-ylmethyl)benzene (bix) as the ligand and Zn(2+) as the central metal ion in ethanol, in which rhodamine B (RhB) is encapsulated through self-adaptive chemistry. In pure ethanol solvent, the as-formed RhB/Zn(bix) is well dispersed and quite stable. However, the addition of water into the ethanol dispersion of RhB/Zn(bix) destroys Zn(bix) network structure, resulting in the release of RhB from ICP into the solvent. As a consequence, the solvent displays the color of released RhB and, at the meantime, turns on the fluorescence of RhB, which constitutes a new mechanism for colorimetric and fluorescent dual mode sensing of AS in commercial spirit samples. With the method developed here, we could distinguish the AS of different commercial spirit samples by the naked eye within a wide linear range from 20 to 100% vol and by monitoring the increase of fluorescent intensity of the released RhB. This study not only offers a new method for on-spot visible detection of AS in commercial spirit samples, but also provides a strategy for designing dual mode sensing mechanisms for different analytical purposes based on novel stimuli-responsive materials.

Simplified PCR for detection of Haemophilus ducreyi and diagnosis of chancroid.

PubMed Central

West, B; Wilson, S M; Changalucha, J; Patel, S; Mayaud, P; Ballard, R C; Mabey, D

1995-01-01

A simplified PCR was developed for detection of Haemophilus ducreyi in samples from chancroid patients. The strategy included a straightforward chloroform extraction sample preparation method, a one-tube nested PCR to minimize contamination risks, and a colorimetric method for detection of products. Primers were designed from published nucleotide sequences of the 16S rRNA gene of H. ducreyi, with longer outer primers for annealing at a higher temperature and shorter inner primers labelled with biotin and digoxigenin for binding with avidin and colorimetric detection. The PCR technique detected all 35 strains of H. ducreyi tested, from four different geographical regions, and was negative for other, related strains of bacteria and for the common contaminating bacteria tested. Of 25 samples from H. ducreyi culture-positive chancroid patients, 24 were PCR positive and 1 produced a weak reaction. Of 83 samples from clinical cases of chancroid in the Republic of South Africa, 69 were PCR positive. The sensitivity of PCR compared with that of clinical diagnosis was 83%. All 50 negative control samples were negative. Encouraging results were also obtained with a consecutive series of 25 genital ulcer patients in Tanzania, of whom 9 were PCR positive. The adaptations of this simplified PCR strategy, at the sensitivity and specificity levels obtained, mean it will be useful for detection of H. ducreyi in areas where the organism is endemic, particularly where testing by culture is difficult or impossible. PMID:7540625

Coping with matrix effects in headspace solid phase microextraction gas chromatography using multivariate calibration strategies.

PubMed

Ferreira, Vicente; Herrero, Paula; Zapata, Julián; Escudero, Ana

2015-08-14

SPME is extremely sensitive to experimental parameters affecting liquid-gas and gas-solid distribution coefficients. Our aims were to measure the weights of these factors and to design a multivariate strategy based on the addition of a pool of internal standards, to minimize matrix effects. Synthetic but real-like wines containing selected analytes and variable amounts of ethanol, non-volatile constituents and major volatile compounds were prepared following a factorial design. The ANOVA study revealed that even using a strong matrix dilution, matrix effects are important and additive with non-significant interaction effects and that it is the presence of major volatile constituents the most dominant factor. A single internal standard provided a robust calibration for 15 out of 47 analytes. Then, two different multivariate calibration strategies based on Partial Least Square Regression were run in order to build calibration functions based on 13 different internal standards able to cope with matrix effects. The first one is based in the calculation of Multivariate Internal Standards (MIS), linear combinations of the normalized signals of the 13 internal standards, which provide the expected area of a given unit of analyte present in each sample. The second strategy is a direct calibration relating concentration to the 13 relative areas measured in each sample for each analyte. Overall, 47 different compounds can be reliably quantified in a single fully automated method with overall uncertainties better than 15%. Copyright © 2015 Elsevier B.V. All rights reserved.

Lack of latex allergen contamination of solutions withdrawn from vials with natural rubber stoppers.

PubMed

Thomsen, D J; Burke, T G

2000-01-01

The effect on latex allergen contamination and microbial growth of a latex-allergy precaution technique for preparing injectable products was studied. The study consisted of three parts: (1) preparation of 20 samples from vials with latex-containing stoppers in accordance with conventional guidelines, (2) preparation of 20 samples in accordance with latex-allergy precaution guidelines, and (3) preparation of 5 latex-free samples and 1 latex-contaminated sample as negative and positive controls, respectively. The conventional method involved swabbing a vial top with an alcohol prep pad, puncturing the dry natural rubber stopper with an 18-gauge needle attached to a latex-free syringe, and withdrawing the contents of the vial into the syringe. The latex-allergy precaution preparation technique was similar, except that the stopper was removed before the vial contents were withdrawn. There was essentially no difference in latex allergen concentrations between the two drug preparation methods. None of the samples prepared with the standard method supported any microbial growth. One sample prepared with the latex-allergy precaution method grew bacteria. Removal of the dry rubber stopper from vials did not yield solutions with less latex allergen than solutions prepared according to conventional guidelines.

Prevalence, Level, and Types of Salmonella Isolated from North American In-Shell Pecans over Four Harvest Years.

PubMed

Brar, Pardeepinder K; Strawn, Laura K; Danyluk, Michelle D

2016-03-01

In-shell pecan samples (500 g) were collected over four harvest seasons (2010 to 2014) from seven pecan shelling facilities located in five U.S. states. Four varieties of pecans were analyzed: Mexican Improved, Native Seedlings, Southern Improved, and Western Improved. Pecan samples (100 g) were sent to a third party laboratory for initial Salmonella screening. When a sample was positive for Salmonella, the pathogen level was determined by the most-probable-number (MPN) method (25, 2.5, and 0.25 g). Two sample preparation strategies were used for the MPN analysis, and both strategies were combined for the reported MPN values. Forty-four (0.95%) of 4,641 in-shell pecan samples were positive for Salmonella during initial screening; prevalence by year was 0.47 to 1.4%. Prevalence was not significantly different between varieties: Mexican Improved, 1.2%; Native/Seedling, 0.99%; Southern Improved, 0.97%; and Western Improved, 0.75%. Salmonella was not isolated from 31 of 44 samples upon retesting during MPN analysis (<0.47 MPN/100 g). When Salmonella was detected, the levels were 0.47 to 39 MPN/100 g, with a mean of 2.4 MPN/100 g. Thirty-one Salmonella serotypes were obtained from 42 Salmonella-positive pecan samples; Enteritidis was the most common (12% of samples) followed by Javiana (9%) and Braenderup (7%). All Salmonella Enteritidis isolates were phage type 8. Pulsed-field gel electrophoresis analysis (XbaI) revealed within-serotype diversity, indicating introduction of contamination from a variety of sources. Most (64%) of the isolates were resistant to streptomycin or tetracycline, and 13% were resistant to three or more antibiotics. Salmonella prevalence and level on in-shell pecans is comparable to that on other nuts.

Microtubules in Plant Cells: Strategies and Methods for Immunofluorescence, Transmission Electron Microscopy and Live Cell Imaging

PubMed Central

Celler, Katherine; Fujita, Miki; Kawamura, Eiko; Ambrose, Chris; Herburger, Klaus; Wasteneys, Geoffrey O.

2016-01-01

Microtubules are required throughout plant development for a wide variety of processes, and different strategies have evolved to visualize and analyze them. This chapter provides specific methods that can be used to analyze microtubule organization and dynamic properties in plant systems and summarizes the advantages and limitations for each technique. We outline basic methods for preparing samples for immunofluorescence labelling, including an enzyme-based permeabilization method, and a freeze-shattering method, which generates microfractures in the cell wall to provide antibodies access to cells in cuticle-laden aerial organs such as leaves. We discuss current options for live cell imaging of MTs with fluorescently tagged proteins (FPs), and provide chemical fixation, high pressure freezing/freeze substitution, and post-fixation staining protocols for preserving MTs for transmission electron microscopy and tomography. PMID:26498784

Micronucleated Erythrocytes in Peripheral Blood from Neonate Rats Exposed by Breastfeeding to Cyclophosphamide, Colchicine, or Cytosine-Arabinoside.

PubMed

Gómez-Meda, Belinda C; Bañales-Martínez, Luis R; Zamora-Perez, Ana L; Lemus-Varela, María de Lourdes; Trujillo, Xóchitl; Sánchez-Parada, María G; Torres-Mendoza, Blanca M; Armendáriz-Borunda, Juan; Zúñiga-González, Guillermo M

2016-01-01

Genotoxic exposure to chemical substances is common, and nursing mothers could transmit harmful substances or their metabolites to their offspring through breast milk. We explored the possibility of determining genotoxic effects in the erythrocytes of breastfeeding rat pups whose mothers received a genotoxic compound while nursing. Ten groups of female rats and five pups per dam were studied. The control group received sterile water, and the experimental groups received one of three different doses of cyclophosphamide, colchicine, or cytosine-arabinoside. Blood smears were prepared from samples taken from each dam and pup every 24 h for six days. There were increased numbers of micronucleated erythrocytes (MNEs) and micronucleated polychromatic erythrocytes (MNPCEs) in the samples from pups in the experimental groups ( P < 0.02) and increased MNPCE frequencies in the samples from the dams ( P < 0.05). These results demonstrate the vertical transmission of the genotoxic effect of the compounds tested. In conclusion, assessing MNEs in breastfeeding neonate rats to assess DNA damage may be a useful approach for identifying genotoxic compounds and/or cytotoxic effects. This strategy could help in screening for therapeutic approaches that are genotoxic during the lactation stage and these assessments might also be helpful for developing preventive strategies to counteract harmful effects.

Micronucleated Erythrocytes in Peripheral Blood from Neonate Rats Exposed by Breastfeeding to Cyclophosphamide, Colchicine, or Cytosine-Arabinoside

PubMed Central

Bañales-Martínez, Luis R.; Lemus-Varela, María de Lourdes; Trujillo, Xóchitl; Sánchez-Parada, María G.; Armendáriz-Borunda, Juan; Zúñiga-González, Guillermo M.

2016-01-01

Genotoxic exposure to chemical substances is common, and nursing mothers could transmit harmful substances or their metabolites to their offspring through breast milk. We explored the possibility of determining genotoxic effects in the erythrocytes of breastfeeding rat pups whose mothers received a genotoxic compound while nursing. Ten groups of female rats and five pups per dam were studied. The control group received sterile water, and the experimental groups received one of three different doses of cyclophosphamide, colchicine, or cytosine-arabinoside. Blood smears were prepared from samples taken from each dam and pup every 24 h for six days. There were increased numbers of micronucleated erythrocytes (MNEs) and micronucleated polychromatic erythrocytes (MNPCEs) in the samples from pups in the experimental groups (P < 0.02) and increased MNPCE frequencies in the samples from the dams (P < 0.05). These results demonstrate the vertical transmission of the genotoxic effect of the compounds tested. In conclusion, assessing MNEs in breastfeeding neonate rats to assess DNA damage may be a useful approach for identifying genotoxic compounds and/or cytotoxic effects. This strategy could help in screening for therapeutic approaches that are genotoxic during the lactation stage and these assessments might also be helpful for developing preventive strategies to counteract harmful effects. PMID:28018917

[High-sensitive detection of multiple allergenic proteins in infant food with high-resolution mass spectrometry].

PubMed

Wu, Ci; Chen, Xi; Liu, Jianhui; Zhang, Xiaolin; Xue, Weifeng; Liang, Zhen; Liu, Mengyao; Cui, Yan; Huang, Daliang; Zhang, Lihua

2017-10-08

A novel method of the simultaneous detection of multiple kinds of allergenic proteins in infant food with parallel reaction monitoring (PRM) mode using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established. In this method, unique peptides with good stability and high sensibility were used to quantify the corresponding allergenic proteins. Furthermore, multiple kinds of allergenic proteins are inspected simultaneously with high sensitivity. In addition, such method was successfully used for the detection of multiple allergenic proteins in infant food. As for the sample preparation for infant food, compared with the traditional acetone precipitation strategy, the protein extraction efficiency and capacity of resisting disturbance are both higher with in-situ filter-aided sample pretreatment (i-FASP) method. All allergenic proteins gave a good linear response with the correlation coefficients ( R 2 ) ≥ 0.99, and the largest concentration range of the allergenic proteins could be four orders of magnitude, and the lowest detection limit was 0.028 mg/L, which was better than that reported in references. Finally, the method was conveniently used to detect the allergens from four imported infant food real samples. All the results demonstrate that this novel strategy is of great significance for providing a rapid and reliable analytical technique for allergen proteomics.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

This volume contains the interim change notice for sample preparation methods. Covered are: acid digestion for metals analysis, fusion of Hanford tank waste solids, water leach of sludges/soils/other solids, extraction procedure toxicity (simulate leach in landfill), sample preparation for gamma spectroscopy, acid digestion for radiochemical analysis, leach preparation of solids for free cyanide analysis, aqueous leach of solids for anion analysis, microwave digestion of glasses and slurries for ICP/MS, toxicity characteristic leaching extraction for inorganics, leach/dissolution of activated metal for radiochemical analysis, extraction of single-shell tank (SST) samples for semi-VOC analysis, preparation and cleanup of hydrocarbon- containing samples for VOCmore » and semi-VOC analysis, receiving of waste tank samples in onsite transfer cask, receipt and inspection of SST samples, receipt and extrusion of core samples at 325A shielded facility, cleaning and shipping of waste tank samplers, homogenization of solutions/slurries/sludges, and test sample preparation for bioassay quality control program.« less

Effects of Sample Preparation on the Infrared Reflectance Spectra of Powders

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brauer, Carolyn S.; Johnson, Timothy J.; Myers, Tanya L.

2015-05-22

While reflectance spectroscopy is a useful tool in identifying molecular compounds, laboratory measurement of solid (particularly powder) samples often is confounded by sample preparation methods. For example, both the packing density and surface roughness can have an effect on the quantitative reflectance spectra of powdered samples. Recent efforts in our group have focused on developing standard methods for measuring reflectance spectra that accounts for sample preparation, as well as other factors such as particle size and provenance. In this work, the effect of preparation method on sample reflectivity was investigated by measuring the directional-hemispherical spectra of samples that were hand-packedmore » as well as pressed into pellets using an integrating sphere attached to a Fourier transform infrared spectrometer. The results show that the methods used to prepare the sample have a substantial effect on the measured reflectance spectra, as do other factors such as particle size.« less

Effects of sample preparation on the infrared reflectance spectra of powders

NASA Astrophysics Data System (ADS)

Brauer, Carolyn S.; Johnson, Timothy J.; Myers, Tanya L.; Su, Yin-Fong; Blake, Thomas A.; Forland, Brenda M.

2015-05-01

While reflectance spectroscopy is a useful tool for identifying molecular compounds, laboratory measurement of solid (particularly powder) samples often is confounded by sample preparation methods. For example, both the packing density and surface roughness can have an effect on the quantitative reflectance spectra of powdered samples. Recent efforts in our group have focused on developing standard methods for measuring reflectance spectra that accounts for sample preparation, as well as other factors such as particle size and provenance. In this work, the effect of preparation method on sample reflectivity was investigated by measuring the directional-hemispherical spectra of samples that were hand-loaded as well as pressed into pellets using an integrating sphere attached to a Fourier transform infrared spectrometer. The results show that the methods used to prepare the sample can have a substantial effect on the measured reflectance spectra, as do other factors such as particle size.

Site characterization summary report for dry weather surface water sampling upper East Fork Poplar Creek characterization area Oak Ridge Y-12 Plant, Oak Ridge, Tennessee

DOE Office of Scientific and Technical Information (OSTI.GOV)

NONE

This report describes activities associated with conducting dry weather surface water sampling of Upper East Fork Poplar Creek (UEFPC) at the Oak Ridge Y-12 Plant, Oak Ridge, Tennessee. This activity is a portion of the work to be performed at UEFPC Operable Unit (OU) 1 [now known as the UEFPC Characterization Area (CA)], as described in the RCRA Facility Investigation Plan for Group 4 at the Oak- Ridge Y-12 Plant, Oak Ridge, Tennessee and in the Response to Comments and Recommendations on RCRA Facility Investigation Plan for Group 4 at the Oak Ridge Y-12 Plant, Oak Ridge, Tennessee, Volume 1,more » Operable Unit 1. Because these documents contained sensitive information, they were labeled as unclassified controlled nuclear information and as such are not readily available for public review. To address this issue the U.S. Department of Energy (DOE) published an unclassified, nonsensitive version of the initial plan, text and appendixes, of this Resource Conservation and Recovery Act (RCRA) Facility Investigation (RFI) Plan in early 1994. These documents describe a program for collecting four rounds of wet weather and dry weather surface water samples and one round of sediment samples from UEFPC. They provide the strategy for the overall sample collection program including dry weather sampling, wet weather sampling, and sediment sampling. Figure 1.1 is a schematic flowchart of the overall sampling strategy and other associated activities. A Quality Assurance Project Plan (QAPJP) was prepared to specifically address four rounds of dry weather surface water sampling and one round of sediment sampling. For a variety of reasons, sediment sampling has not been conducted and has been deferred to the UEFPC CA Remedial Investigation (RI), as has wet weather sampling.« less

Utilizing the ultrasensitive Schistosoma up-converting phosphor lateral flow circulating anodic antigen (UCP-LF CAA) assay for sample pooling-strategies.

PubMed

Corstjens, Paul L A M; Hoekstra, Pytsje T; de Dood, Claudia J; van Dam, Govert J

2017-11-01

Methodological applications of the high sensitivity genus-specific Schistosoma CAA strip test, allowing detection of single worm active infections (ultimate sensitivity), are discussed for efficient utilization in sample pooling strategies. Besides relevant cost reduction, pooling of samples rather than individual testing can provide valuable data for large scale mapping, surveillance, and monitoring. The laboratory-based CAA strip test utilizes luminescent quantitative up-converting phosphor (UCP) reporter particles and a rapid user-friendly lateral flow (LF) assay format. The test includes a sample preparation step that permits virtually unlimited sample concentration with urine, reaching ultimate sensitivity (single worm detection) at 100% specificity. This facilitates testing large urine pools from many individuals with minimal loss of sensitivity and specificity. The test determines the average CAA level of the individuals in the pool thus indicating overall worm burden and prevalence. When requiring test results at the individual level, smaller pools need to be analysed with the pool-size based on expected prevalence or when unknown, on the average CAA level of a larger group; CAA negative pools do not require individual test results and thus reduce the number of tests. Straightforward pooling strategies indicate that at sub-population level the CAA strip test is an efficient assay for general mapping, identification of hotspots, determination of stratified infection levels, and accurate monitoring of mass drug administrations (MDA). At the individual level, the number of tests can be reduced i.e. in low endemic settings as the pool size can be increased as opposed to prevalence decrease. At the sub-population level, average CAA concentrations determined in urine pools can be an appropriate measure indicating worm burden. Pooling strategies allowing this type of large scale testing are feasible with the various CAA strip test formats and do not affect sensitivity and specificity. It allows cost efficient stratified testing and monitoring of worm burden at the sub-population level, ideally for large-scale surveillance generating hard data for performance of MDA programs and strategic planning when moving towards transmission-stop and elimination.

Etching of Cr tips for scanning tunneling microscopy of cleavable oxides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huang, Dennis; Liu, Stephen; Zeljkovic, Ilija

Here, we report a detailed three-step roadmap for the fabrication and characterization of bulk Cr tips for spin-polarized scanning tunneling microscopy. Our strategy uniquely circumvents the need for ultra-high vacuum preparation of clean surfaces or films. First, we demonstrate the role of ex situ electrochemical etch parameters on Cr tip apex geometry, using scanning electron micrographs of over 70 etched tips. Second, we describe the suitability of the in situ cleaved surface of the layered antiferromagnet La 1.4Sr 1.6Mn 2O 7 to evaluate the spin characteristics of the Cr tip, replacing the ultra-high vacuum-prepared test samples that have been usedmore » in prior studies. Third, we outline a statistical algorithm that can effectively delineate closely spaced or irregular cleaved step edges, to maximize the accuracy of step height and spin-polarization measurements.« less

Future preparation of occupational health nurse managers.

PubMed

Scalzi, C C; Wilson, D L; Ebert, R

1991-03-01

This article presents the results of a national survey of job activities of corporate level occupational health nurse managers. The survey was designed to identify the relative amount of time spent and importance attributed to specific areas of their current job. In general this sample tended to have more management experience and educational preparation than previously cited studies: over 50% had completed a graduate degree. The scores for importance and time spent were highly correlated. That is, occupational health corporate nurse managers seemed to allocate their time to job responsibilities they considered most important. Management activities related to policy, practice standards, quality assurance, staff development, and systems for client care delivery appear to represent the core responsibilities of occupational health nursing management. Curriculum recommendations for management positions in occupational health include: health policy, program planning, and evaluation; business strategy; applications of management information systems; quality assurance; and marketing.

Etching of Cr tips for scanning tunneling microscopy of cleavable oxides

DOE PAGES

Huang, Dennis; Liu, Stephen; Zeljkovic, Ilija; ...

2017-02-21

Here, we report a detailed three-step roadmap for the fabrication and characterization of bulk Cr tips for spin-polarized scanning tunneling microscopy. Our strategy uniquely circumvents the need for ultra-high vacuum preparation of clean surfaces or films. First, we demonstrate the role of ex situ electrochemical etch parameters on Cr tip apex geometry, using scanning electron micrographs of over 70 etched tips. Second, we describe the suitability of the in situ cleaved surface of the layered antiferromagnet La 1.4Sr 1.6Mn 2O 7 to evaluate the spin characteristics of the Cr tip, replacing the ultra-high vacuum-prepared test samples that have been usedmore » in prior studies. Third, we outline a statistical algorithm that can effectively delineate closely spaced or irregular cleaved step edges, to maximize the accuracy of step height and spin-polarization measurements.« less

Comprehensive two-dimensional gas chromatography and food sensory properties: potential and challenges.

PubMed

Cordero, Chiara; Kiefl, Johannes; Schieberle, Peter; Reichenbach, Stephen E; Bicchi, Carlo

2015-01-01

Modern omics disciplines dealing with food flavor focus the analytical efforts on the elucidation of sensory-active compounds, including all possible stimuli of multimodal perception (aroma, taste, texture, etc.) by means of a comprehensive, integrated treatment of sample constituents, such as physicochemical properties, concentration in the matrix, and sensory properties (odor/taste quality, perception threshold). Such analyses require detailed profiling of known bioactive components as well as advanced fingerprinting techniques to catalog sample constituents comprehensively, quantitatively, and comparably across samples. Multidimensional analytical platforms support comprehensive investigations required for flavor analysis by combining information on analytes' identities, physicochemical behaviors (volatility, polarity, partition coefficient, and solubility), concentration, and odor quality. Unlike other omics, flavor metabolomics and sensomics include the final output of the biological phenomenon (i.e., sensory perceptions) as an additional analytical dimension, which is specifically and exclusively triggered by the chemicals analyzed. However, advanced omics platforms, which are multidimensional by definition, pose challenging issues not only in terms of coupling with detection systems and sample preparation, but also in terms of data elaboration and processing. The large number of variables collected during each analytical run provides a high level of information, but requires appropriate strategies to exploit fully this potential. This review focuses on advances in comprehensive two-dimensional gas chromatography and analytical platforms combining two-dimensional gas chromatography with olfactometry, chemometrics, and quantitative assays for food sensory analysis to assess the quality of a given product. We review instrumental advances and couplings, automation in sample preparation, data elaboration, and a selection of applications.

Potential artifacts associated with historical preparation of joint compound samples and reported airborne asbestos concentrations.

PubMed

Brorby, G P; Sheehan, P J; Berman, D W; Bogen, K T; Holm, S E

2011-05-01

Airborne samples collected in the 1970s for drywall workers using asbestos-containing joint compounds were likely prepared and analyzed according to National Institute of Occupational Safety and Health Method P&CAM 239, the historical precursor to current Method 7400. Experimentation with a re-created, chrysotile-containing, carbonate-based joint compound suggested that analysis following sample preparation by the historical vs. current method produces different fiber counts, likely because of an interaction between the different clearing and mounting chemicals used and the carbonate-based joint compound matrix. Differences were also observed during analysis using Method 7402, depending on whether acetic acid/dimethylformamide or acetone was used during preparation to collapse the filter. Specifically, air samples of sanded chrysotile-containing joint compound prepared by the historical method yielded fiber counts significantly greater (average of 1.7-fold, 95% confidence interval: 1.5- to 2.0-fold) than those obtained by the current method. In addition, air samples prepared by Method 7402 using acetic acid/dimethylformamide yielded fiber counts that were greater (2.8-fold, 95% confidence interval: 2.5- to 3.2-fold) than those prepared by this method using acetone. These results indicated (1) there is an interaction between Method P&CAM 239 preparation chemicals and the carbonate-based joint compound matrix that reveals fibers that were previously bound in the matrix, and (2) the same appeared to be true for Method 7402 preparation chemicals acetic acid/dimethylformamide. This difference in fiber counts is the opposite of what has been reported historically for samples of relatively pure chrysotile dusts prepared using the same chemicals. This preparation artifact should be considered when interpreting historical air samples for drywall workers prepared by Method P&CAM 239. Copyright © 2011 JOEH, LLC

Sample Preparation of Corn Seed Tissue to Prevent Analyte Relocations for Mass Spectrometry Imaging

NASA Astrophysics Data System (ADS)

Kim, Shin Hye; Kim, Jeongkwon; Lee, Young Jin; Lee, Tae Geol; Yoon, Sohee

2017-08-01

Corn seed tissue sections were prepared by the tape support method using an adhesive tape, and mass spectrometry imaging (MSI) was performed. The effect of heat generated during sample preparation was investigated by time-of-flight secondary mass spectrometry (TOF-SIMS) imaging of corn seed tissue prepared by the tape support and the thaw-mounted methods. Unlike thaw-mounted sample preparation, the tape support method does not cause imaging distortion because of the absence of heat, which can cause migration of the analytes on the sample. By applying the tape-support method, the corn seed tissue was prepared without structural damage and MSI with accurate spatial information of analytes was successfully performed.

MARS: bringing the automation of small-molecule bioanalytical sample preparations to a new frontier.

PubMed

Li, Ming; Chou, Judy; Jing, Jing; Xu, Hui; Costa, Aldo; Caputo, Robin; Mikkilineni, Rajesh; Flannelly-King, Shane; Rohde, Ellen; Gan, Lawrence; Klunk, Lewis; Yang, Liyu

2012-06-01

In recent years, there has been a growing interest in automating small-molecule bioanalytical sample preparations specifically using the Hamilton MicroLab(®) STAR liquid-handling platform. In the most extensive work reported thus far, multiple small-molecule sample preparation assay types (protein precipitation extraction, SPE and liquid-liquid extraction) have been integrated into a suite that is composed of graphical user interfaces and Hamilton scripts. Using that suite, bioanalytical scientists have been able to automate various sample preparation methods to a great extent. However, there are still areas that could benefit from further automation, specifically, the full integration of analytical standard and QC sample preparation with study sample extraction in one continuous run, real-time 2D barcode scanning on the Hamilton deck and direct Laboratory Information Management System database connectivity. We developed a new small-molecule sample-preparation automation system that improves in all of the aforementioned areas. The improved system presented herein further streamlines the bioanalytical workflow, simplifies batch run design, reduces analyst intervention and eliminates sample-handling error.

Preparing for High Technology: Successful Co-op Strategies. Research and Development Series No. 263.

ERIC Educational Resources Information Center

Franchak, Stephen J.; Smith, O. H. Michael

This document has been prepared to assist program administrators and practitioners in planning and implementing cooperative (co-op) programs in high technology occupational areas. Information focuses on the key elements, strategies, and procedures of successful co-op programs. The guide contains nine chapters and is based on a review of the…

Passing the Leadership Test: Strategies for Success on the Leadership Licensure Exam. Second Edition

ERIC Educational Resources Information Center

Jones, Leslie; Kennedy, Eugene

2012-01-01

"Passing the Leadership Test: Strategies for Success on the Leadership Licensure Exam" is a study guide for the School Leaders Licensure Examination (SLLA.) The book presents a comprehensive, practical guide for preparing for the SLLA. It is divided into two sections: basic principles of test preparation and the ISLLC standards with implications…

Development of Strategies for the Preservation of School Counselor Preparation Programs: A Monograph.

ERIC Educational Resources Information Center

Cecil, Jean Houchins; Comas, Robert E.

A project dealing with strategies to preserve school counselor preparation programs, evolving from the work of the Southern Association for Counselor Education and Supervision (SACES) Round Table of Department Heads, is described. Factors involved in what SACES believes may be the demise of school counseling, at least as it is known presently, are…

Preferred Instructional Design Strategies for Preparation of Pre-Service Teachers of Integrated STEM Education

ERIC Educational Resources Information Center

Roberts, Amanda Shackleford

2013-01-01

The purpose of this study was to identify the preferred instructional design strategies for the preparation of pre-service teachers who will deliver integrated STEM lessons. The research objectives were threefold and included identifying a preferred definition of integrated STEM education, developing its purpose statement, and creating a list of…

The Impact of Vocabulary Preparation on L2 Listening Comprehension, Confidence and Strategy Use

ERIC Educational Resources Information Center

Chang, Anna Ching-Shyang

2007-01-01

Building on previous studies of the effects of planning on second language learners' (L2) oral narratives and writing, this research reports an investigation of the effects of vocabulary preparation prior to a listening comprehension test on L2 learners' vocabulary performance, listening comprehension, confidence levels and strategy use. The…

Learning from the Learners: Preparing Future Teachers to Leverage the Benefits of Laptop Computers

ERIC Educational Resources Information Center

Grundmeyer, Trent; Peters, Randal

2016-01-01

Technology is changing the teaching and learning landscape. Teacher preparation programs must produce teachers who have new skills and strategies to leverage the benefits of laptop computers in their classrooms. This study used a phenomenological strategy to explain first-year college students' perceptions of the effects of a 1:1 laptop experience…

Randomly picked cosmid clones overlap the pyrB and oriC gap in the physical map of the E. coli chromosome.

PubMed Central

Knott, V; Rees, D J; Cheng, Z; Brownlee, G G

1988-01-01

Sets of overlapping cosmid clones generated by random sampling and fingerprinting methods complement data at pyrB (96.5') and oriC (84') in the published physical map of E. coli. A new cloning strategy using sheared DNA, and a low copy, inducible cosmid vector were used in order to reduce bias in libraries, in conjunction with micro-methods for preparing cosmid DNA from a large number of clones. Our results are relevant to the design of the best approach to the physical mapping of large genomes. PMID:2834694

BASS Experiment Imagery

NASA Image and Video Library

2013-04-05

ISS035-E-014971 (6 April 2013) --- This is a close-up image photographed during a run of the Burning and Suppression of Solids (BASS) experiment onboard the Earth-orbiting International Space Station. Following a series of preparations, NASA astronaut Chris Cassidy (out of frame) conducted runs of the experiment, which examines the burning and extinction characteristics of a wide variety of fuel samples in microgravity. The experiment is planned for guiding strategies for extinguishing fires in microgravity. BASS results contribute to the combustion computational models used in the design of fire detection and suppression systems in microgravity and on Earth.

BASS Experiment Imagery

NASA Image and Video Library

2013-04-09

ISS035-E-015900 (10 April 2013) --- This is one of a series of close-up images photographed during a run of the Burning and Suppression of Solids (BASS) experiment onboard the Earth-orbiting International Space Station. Following a series of preparations, NASA astronaut Chris Cassidy (out of frame) conducted several runs of the experiment, which examines the burning and extinction characteristics of a wide variety of fuel samples in microgravity. The experiment is planned for guiding strategies for extinguishing fires in microgravity. BASS results contribute to the combustion computational models used in the design of fire detection and suppression systems in microgravity and on Earth.

BASS Experiment Imagery

NASA Image and Video Library

2013-04-09

ISS035-E-015679 (10 April 2013) --- This is one of a series of close-up images photographed during a run of the Burning and Suppression of Solids (BASS) experiment onboard the Earth-orbiting International Space Station. Following a series of preparations, NASA astronaut Chris Cassidy (out of frame) conducted a series of runs of the experiment, which examines the burning and extinction characteristics of a wide variety of fuel samples in microgravity. The experiment is planned for guiding strategies for extinguishing fires in microgravity. BASS results contribute to the combustion computational models used in the design of fire detection and suppression systems in microgravity and on Earth.

BASS-II Experiment

NASA Image and Video Library

2014-07-23

ISS040-E-073120 (23 July 2014) --- This is a close-up image photographed during a run of the Burning and Suppression of Solids (BASS) experiment onboard the Earth-orbiting International Space Station. Following a series of preparations, NASA astronaut Reid Wiseman (out of frame), Expedition 40 flight engineer, conducted runs of the experiment, which examines the burning and extinction characteristics of a wide variety of fuel samples in microgravity. The experiment is planned for guiding strategies for extinguishing fires in microgravity. BASS results contribute to the combustion computational models used in the design of fire detection and suppression systems in microgravity and on Earth.

BASS Experiment Imagery

NASA Image and Video Library

2013-04-05

ISS035-E-014987 (6 April 2013) --- This is a close-up image photographed during a run of the Burning and Suppression of Solids (BASS) experiment onboard the Earth-orbiting International Space Station. Following a series of preparations, NASA astronaut Chris Cassidy (out of frame) conducted runs of the experiment, which examines the burning and extinction characteristics of a wide variety of fuel samples in microgravity. The experiment is planned for guiding strategies for extinguishing fires in microgravity. BASS results contribute to the combustion computational models used in the design of fire detection and suppression systems in microgravity and on Earth.

BASS Experiment Imagery

NASA Image and Video Library

2013-04-09

ISS035-E-015827 (10 April 2013) --- This is one of a series of close-up images photographed during a run of the Burning and Suppression of Solids (BASS) experiment onboard the Earth-orbiting International Space Station. Following a series of preparations, NASA astronaut Chris Cassidy (out of frame) conducted a series of runs of the experiment, which examines the burning and extinction characteristics of a wide variety of fuel samples in microgravity. The experiment is planned for guiding strategies for extinguishing fires in microgravity. BASS results contribute to the combustion computational models used in the design of fire detection and suppression systems in microgravity and on Earth.

BASS Experiment Imagery

NASA Image and Video Library

2013-04-09

ISS035-E-015930 (10 April 2013) --- This is one of a series of close-up images photographed during a run of the Burning and Suppression of Solids (BASS) experiment onboard the Earth-orbiting International Space Station. Following a series of preparations, NASA astronaut Chris Cassidy (out of frame) conducted several runs of the experiment, which examines the burning and extinction characteristics of a wide variety of fuel samples in microgravity. The experiment is planned for guiding strategies for extinguishing fires in microgravity. BASS results contribute to the combustion computational models used in the design of fire detection and suppression systems in microgravity and on Earth.

BASS-II Experiment

NASA Image and Video Library

2014-06-27

ISS040-E-023287 (27 June 2014) --- This is a close-up image photographed during a run of the Burning and Suppression of Solids (BASS) experiment onboard the Earth-orbiting International Space Station. Following a series of preparations, NASA astronaut Reid Wiseman (out of frame), Expedition 40 flight engineer, conducted runs of the experiment, which examines the burning and extinction characteristics of a wide variety of fuel samples in microgravity. The experiment is planned for guiding strategies for extinguishing fires in microgravity. BASS results contribute to the combustion computational models used in the design of fire detection and suppression systems in microgravity and on Earth.

Targeted Selected Reaction Monitoring Mass Spectrometric Immunoassay for Insulin-like Growth Factor 1

PubMed Central

Niederkofler, Eric E.; Phillips, David A.; Krastins, Bryan; Kulasingam, Vathany; Kiernan, Urban A.; Tubbs, Kemmons A.; Peterman, Scott M.; Prakash, Amol; Diamandis, Eleftherios P.; Lopez, Mary F.; Nedelkov, Dobrin

2013-01-01

Insulin-like growth factor 1 (IGF1) is an important biomarker of human growth disorders that is routinely analyzed in clinical laboratories. Mass spectrometry-based workflows offer a viable alternative to standard IGF1 immunoassays, which utilize various pre-analytical preparation strategies. In this work we developed an assay that incorporates a novel sample preparation method for dissociating IGF1 from its binding proteins. The workflow also includes an immunoaffinity step using antibody-derivatized pipette tips, followed by elution, trypsin digestion, and LC-MS/MS separation and detection of the signature peptides in a selected reaction monitoring (SRM) mode. The resulting quantitative mass spectrometric immunoassay (MSIA) exhibited good linearity in the range of 1 to 1,500 ng/mL IGF1, intra- and inter-assay precision with CVs of less than 10%, and lowest limits of detection of 1 ng/mL. The linearity and recovery characteristics of the assay were also established, and the new method compared to a commercially available immunoassay using a large cohort of human serum samples. The IGF1 SRM MSIA is well suited for use in clinical laboratories. PMID:24278387

Technical Considerations for Reduced Representation Bisulfite Sequencing with Multiplexed Libraries

PubMed Central

Chatterjee, Aniruddha; Rodger, Euan J.; Stockwell, Peter A.; Weeks, Robert J.; Morison, Ian M.

2012-01-01

Reduced representation bisulfite sequencing (RRBS), which couples bisulfite conversion and next generation sequencing, is an innovative method that specifically enriches genomic regions with a high density of potential methylation sites and enables investigation of DNA methylation at single-nucleotide resolution. Recent advances in the Illumina DNA sample preparation protocol and sequencing technology have vastly improved sequencing throughput capacity. Although the new Illumina technology is now widely used, the unique challenges associated with multiplexed RRBS libraries on this platform have not been previously described. We have made modifications to the RRBS library preparation protocol to sequence multiplexed libraries on a single flow cell lane of the Illumina HiSeq 2000. Furthermore, our analysis incorporates a bioinformatics pipeline specifically designed to process bisulfite-converted sequencing reads and evaluate the output and quality of the sequencing data generated from the multiplexed libraries. We obtained an average of 42 million paired-end reads per sample for each flow-cell lane, with a high unique mapping efficiency to the reference human genome. Here we provide a roadmap of modifications, strategies, and trouble shooting approaches we implemented to optimize sequencing of multiplexed libraries on an a RRBS background. PMID:23193365

Large and stable reversible lithium-ion storages from mesoporous SnO2 nanosheets with ultralong lifespan over 1000 cycles

NASA Astrophysics Data System (ADS)

Zhang, Xiao; Jiang, Bin; Guo, Jinxue; Xie, Yaping; Tang, Lin

2014-12-01

The major challenge to promote the commercialization of SnO2 anode materials is to construct unique structures and/or composites that could alleviate the volume effect and extend the lifespan. This study develops an efficient synthetic solution for the preparation of mesoporous SnO2 nanosheets, which involves an evaporation-induced selfassembly process and the following thermal treatment. Surfactant F127 is used as the soft template to form abundant cores. The as-prepared sample intrinsically inherits flexible sheet-like structure and porous features, as characterized with XRD, SEM, TEM and BET techniques. Based on these combining structural benefits, the sample is utilized as anode materials for lithium-ion batteries and exhibits excellent Li+ storage performance such as large and stable reversible capacity, good rate capability, and especially the outstanding durable cycling life of over 1000 cycles, which meets the demands of practical applications. The structural changes of SnO2 nanosheets are observed from the decomposed electrodes after different electrochemical cycles. Moreover, this synthesis strategy may offer an alternative and universal approach for synthesis of other transitional metal oxides or their binary composites as high-performance anode materials for lithium-ion batteries.

Rehabilitation strategies enhancing participation in shopping malls for persons living with a disability.

PubMed

Alary Gauvreau, Christine; Kairy, Dahlia; Mazer, Barbara; Guindon, Andréanne; Le Dorze, Guylaine

2018-04-01

After rehabilitation, it is not clear the extent to which persons living with a disability return to their former activities in the community, such as going to shopping malls. Rehabilitation professionals are faced with the challenge to adequately prepare their clients to resume community participation. The purpose of this study was to identify rehabilitation strategies aimed at preparing clients to engage in activities in shopping malls. Twenty-two participants including 16 rehabilitation clinicians and 6 persons living with a disability participated in four nominal group sessions. Participants were questioned on current or potential rehabilitation strategies carried out to enhance participation in shopping malls for persons living with a disability. Discussions were audio-recorded and qualitative content analysis was conducted. Participants mentioned strategies that were either carried out by the clinician, or in collaboration with other parties. The latter type of strategies was either carried out with the collaboration of the client, the interdisciplinary team, the relatives, or community organizations. Rehabilitation clinicians have a role to play in preparing persons living with a disability to resume activities in a shopping mall. Additionally, therapeutic interventions in community settings may enhance the participation of rehabilitation clients in their everyday activities. Implications for rehabilitation Many strategies are currently used in rehabilitation to prepare persons living with a disability to resume shopping activities. Clinicians could implement shopping-oriented rehabilitation strategies with the client and/or with other rehabilitation partners. Involving clients in activities related to shopping might enhance their participation in shopping malls after rehabilitation. Rehabilitation clinicians can be facilitators for people living with a disability to reach optimal participation.

Cross-sectional TEM specimen preparation for W/B{sub 4}C multilayer sample using FIB

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mondal, Puspen, E-mail: puspen@rrcat.gov.in; Pradhan, P. C.; Tiwari, Pragya

2016-05-23

A recent emergence of a cross-beam scanning electron microscopy (SEM)/focused-ion-beam (FIB) system have given choice to fabricate cross-sectional transmission electron microscopy (TEM) specimen of thin film multilayer sample. A 300 layer pair thin film multilayer sample of W/B{sub 4}C was used to demonstrate the specimen lift-out technique in very short time as compared to conventional cross-sectional sample preparation technique. To get large area electron transparent sample, sample prepared by FIB is followed by Ar{sup +} ion polishing at 2 kV with grazing incident. The prepared cross-sectional sample was characterized by transmission electron microscope.

System for autonomous monitoring of bioagents

DOEpatents

Langlois, Richard G.; Milanovich, Fred P.; Colston, Jr, Billy W.; Brown, Steve B.; Masquelier, Don A.; Mariella, Jr., Raymond P.; Venkateswaran, Kodomudi

2015-06-09

An autonomous monitoring system for monitoring for bioagents. A collector gathers the air, water, soil, or substance being monitored. A sample preparation means for preparing a sample is operatively connected to the collector. A detector for detecting the bioagents in the sample is operatively connected to the sample preparation means. One embodiment of the present invention includes confirmation means for confirming the bioagents in the sample.

Metal-Organic Coordination Polymer to Prepare Density Controllable and High Nitrogen-Doped Content Carbon/Graphene for High Performance Supercapacitors.

PubMed

Luo, Jinwei; Zhong, Wenbin; Zou, Yubo; Xiong, Changlun; Yang, Wantai

2017-01-11

Design and preparation of carbon-based electrode material with high nitrogen-doping ratio and appropriate density attract much interest for supercapacitors in practical application. Herein, three porous carbon/graphene (NCG Cu , NCG Fe , and NCG Zn ) with high doping ratio of nitrogen have been prepared via directly pyrolysis of graphene oxide (GO)/metal-organic coordination polymer (MOCP) composites, which were formed by reacting 4,4'-bipyridine (BPD) with CuCl 2 , FeCl 3 , and ZnCl 2 , respectively. As-prepared NCG Cu , NCG Fe and NCG Zn showed high nitrogen doping ratio of 10.68, 12.99, and 11.21 at. %; and high density of 1.52, 0.84, and 1.15 g cm -3 , respectively. When as-prepared samples were used as supercapacitor electrodes, NCG Cu , NCG Fe and NCG Zn exhibited high gravimetric specific capacitances of 369, 298.5, 309.5 F g -1 , corresponding to high volumetric specific capacitances of 560.9, 250.7, 355.9 F cm -3 at a current density of 0.5 A g -1 , as well as good cycling stability, nearly 100% of the capacitance retained after 1000 cycles even at a large current density of 10 A g -1 . It is expected that the provided novel strategy can be used to develop electrode materials in high performance energy conversion/storage devices.

Development of an enrichment method for endogenous phosphopeptide characterization in human serum.

PubMed

La Barbera, Giorgia; Capriotti, Anna Laura; Cavaliere, Chiara; Ferraris, Francesca; Laus, Michele; Piovesana, Susy; Sparnacci, Katia; Laganà, Aldo

2018-01-01

The work describes the development of an enrichment method for the analysis of endogenous phosphopeptides in serum. Endogenous peptides can play significant biological roles, and some of them could be exploited as future biomarkers. In this context, blood is one of the most useful biofluids for screening, but a systematic investigation of the endogenous peptides, especially phosphorylated ones, is still lacking, mainly due to the lack of suitable analytical methods. Thus, in this paper, different phosphopeptide enrichment strategies were pursued, based either on metal oxide affinity chromatography (MOAC, in the form of commercial TiO 2 spin columns or magnetic graphitized carbon black-TiO 2 composite), or on immobilized metal ion affinity chromatography (IMAC, in the form of Ti 4+ -IMAC magnetic material or commercial Fe 3+ -IMAC spin columns). While MOAC strategies proved completely unsuccessful, probably due to interfering phospholipids displacing phosphopeptides, the IMAC materials performed very well. Different sample preparation strategies were tested, comprising direct dilution with the loading buffer, organic solvent precipitation, and lipid removal from the matrix, as well as the addition of phosphatase inhibitors during sample handling for maximized endogenous phosphopeptide enrichment. All data were acquired by a shotgun peptidomics approach, in which peptide samples were separated by reversed-phase nanoHPLC hyphenated with high-resolution tandem mass spectrometry. The devised method allowed the identification of 176 endogenous phosphopeptides in fresh serum added with inhibitors by the direct dilution protocol and the Ti 4+ -IMAC magnetic material enrichment, but good results could also be obtained from the commercial Fe 3+ -IMAC spin column adapted to the batch enrichment protocol.

Sample Preparation for Mass Spectrometry Imaging of Plant Tissues: A Review

PubMed Central

Dong, Yonghui; Li, Bin; Malitsky, Sergey; Rogachev, Ilana; Aharoni, Asaph; Kaftan, Filip; Svatoš, Aleš; Franceschi, Pietro

2016-01-01

Mass spectrometry imaging (MSI) is a mass spectrometry based molecular ion imaging technique. It provides the means for ascertaining the spatial distribution of a large variety of analytes directly on tissue sample surfaces without any labeling or staining agents. These advantages make it an attractive molecular histology tool in medical, pharmaceutical, and biological research. Likewise, MSI has started gaining popularity in plant sciences; yet, information regarding sample preparation methods for plant tissues is still limited. Sample preparation is a crucial step that is directly associated with the quality and authenticity of the imaging results, it therefore demands in-depth studies based on the characteristics of plant samples. In this review, a sample preparation pipeline is discussed in detail and illustrated through selected practical examples. In particular, special concerns regarding sample preparation for plant imaging are critically evaluated. Finally, the applications of MSI techniques in plants are reviewed according to different classes of plant metabolites. PMID:26904042

Involving children in meal preparation. Effects on food intake.

PubMed

van der Horst, Klazine; Ferrage, Aurore; Rytz, Andreas

2014-08-01

The question of how to promote healthy eating habits in children is relevant because most children do not meet the recommended vegetable intake. Involving children in food preparation could be an opportunity to develop healthy eating behaviors and to increase vegetable consumption. The purpose of this study was to examine the effect of children's involvement in meal preparation on their food and vegetable intake. A between-subject experiment was conducted with 47 children aged 6 to 10 years. In condition 1 (n = 25), children prepared a lunch meal (pasta, breaded chicken, cauliflower, and salad) with the assistance of a parent. In condition 2 (n = 22), the meal was prepared by the parent alone. Independent samples t-tests were conducted to compare intake in the "child cooks" and "parent cooks" conditions. Children in the child cooks condition ate significantly more salad 41.7 g (76.1%), more chicken 21.8 g (27.0%), and more calories 84.6 kcal (24.4%) than children in the parent cooks condition. Between before cooking and directly after cooking the meal, children in the child cooks condition reported significantly increased feelings of valence (feeling positive) and dominance (feeling in control). This study confirms that involving children in meal preparation can increase vegetable intake. Because of the potential effect on energy intake, parents need to be made aware of appropriate portion sizes for their children. Taking this into account, encouraging parents to involve their children in the preparation of healthy and balanced meals could be a valuable intervention strategy to improve the diets and vegetable intake of children. Copyright © 2014 Elsevier Ltd. All rights reserved.

Preparing Pediatric Healthcare Professionals for End-of-Life Care Discussions: An Exploratory Study.

PubMed

Henderson, Amanda; Young, Jeanine; Herbert, Anthony; Bradford, Natalie; Pedersen, Lee-Anne

2017-06-01

Preparedness to initiate end-of-life (EoL) discussions is a confronting and daunting task for all healthcare professionals. We conducted a group interview to explore healthcare professionals' experiences of preparing for EoL discussions with the patient and their family in a pediatric context. To identify what pediatric healthcare professionals consider important when preparing for an EoL discussion. A qualitative design using a group interview. Two open-ended questions were asked: (1) How could preparedness to initiate EoL care discussions between healthcare professionals and the patient and family be enhanced? (2) What education resources/strategies could be developed to support preparation for EoL care discussions? Healthcare professionals, including medical, nursing, and allied health professionals working in pediatric palliative care settings across Queensland, Australia. These settings included major tertiary hospitals, general practice, community, and nongovernment organizations. A convenience sample of 36 healthcare professionals consented to participate in the study. An analysis of the data identified seven themes that had relevance for preparing for an EoL discussion: communication, healthcare professional perspectives, interdisciplinary team role, patient and family perspectives, practical issues, addressing mistakes, and healthcare professional education. Pediatric healthcare professionals confirmed that gaps exist in preparing for an EoL discussion. The findings support a need for further research in two areas. First, a systematic review of interdisciplinary resources that are available to support healthcare professionals in preparing for EoL discussions is recommended. Second, evidence-based interdisciplinary interventions to support pediatric EoL discussions need to be developed and evaluated.

Pigment and Binder Concentrations in Modern Paint Samples Determined by IR and Raman Spectroscopy.

PubMed

Wiesinger, Rita; Pagnin, Laura; Anghelone, Marta; Moretto, Ligia M; Orsega, Emilio F; Schreiner, Manfred

2018-06-18

Knowledge of the techniques employed by artists, such as the composition of the paints, colour palette, and painting style, is of crucial importance not only to attribute works of art to the workshop or artist but also to develop strategies and measures for the conservation and restoration of the art. While much research has been devoted to investigating the composition of an artist's materials from a qualitative point of view, little effort has been made in terms of quantitative analyses. This study aims to quantify the relative concentrations of binders (acrylic and alkyd) and inorganic pigments in different paint samples by IR and Raman spectroscopies. To perform this quantitative evaluation, reference samples of known concentrations were prepared to obtain calibration plots. In a further step, the quantification method was verified by additional test samples and commercially available paint tubes. The results obtained confirm that the quantitative method developed for IR and Raman spectroscopy is able to efficiently determine different pigment and binder concentrations of paint samples with high accuracy. © 2018 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

Final LDRD report : development of sample preparation methods for ChIPMA-based imaging mass spectrometry of tissue samples.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maharrey, Sean P.; Highley, Aaron M.; Behrens, Richard, Jr.

2007-12-01

The objective of this short-term LDRD project was to acquire the tools needed to use our chemical imaging precision mass analyzer (ChIPMA) instrument to analyze tissue samples. This effort was an outgrowth of discussions with oncologists on the need to find the cellular origin of signals in mass spectra of serum samples, which provide biomarkers for ovarian cancer. The ultimate goal would be to collect chemical images of biopsy samples allowing the chemical images of diseased and nondiseased sections of a sample to be compared. The equipment needed to prepare tissue samples have been acquired and built. This equipment includesmore » an cyro-ultramicrotome for preparing thin sections of samples and a coating unit. The coating unit uses an electrospray system to deposit small droplets of a UV-photo absorbing compound on the surface of the tissue samples. Both units are operational. The tissue sample must be coated with the organic compound to enable matrix assisted laser desorption/ionization (MALDI) and matrix enhanced secondary ion mass spectrometry (ME-SIMS) measurements with the ChIPMA instrument Initial plans to test the sample preparation using human tissue samples required development of administrative procedures beyond the scope of this LDRD. Hence, it was decided to make two types of measurements: (1) Testing the spatial resolution of ME-SIMS by preparing a substrate coated with a mixture of an organic matrix and a bio standard and etching a defined pattern in the coating using a liquid metal ion beam, and (2) preparing and imaging C. elegans worms. Difficulties arose in sectioning the C. elegans for analysis and funds and time to overcome these difficulties were not available in this project. The facilities are now available for preparing biological samples for analysis with the ChIPMA instrument. Some further investment of time and resources in sample preparation should make this a useful tool for chemical imaging applications.« less

Perspectives of Australian nursing directors regarding educational preparation for mental health nursing practice.

PubMed

Happell, Brenda; McAllister, Margaret

2014-11-01

There is an ongoing global shortage of mental health nurses. Within Australia, the principal strategy of offering a postgraduate education programme with various incentives to encourage nurses back to study has not been successful. This has led to the consideration of radical alternatives, including the return to pre-registration specialisation in mental health. The successful introduction of this strategy would require the full support of industry partners. To date, the voice of industry has not been heard in relation to this issue. The aim of this paper is to present the views of an Australian sample of mental health nursing directors regarding the resources and other factors required, should undergraduate specialist programmes in mental health be developed, to ensure they are relevant and likely to be successful. A qualitative exploratory research project was undertaken to explore the perspectives and opinions of industry partners. In-depth interviews were conducted with nursing directors (n = 12) in Queensland Australia. Five main themes were identified: relationships with universities; clinical placement preparation and support; workplace culture; facilitators and preceptors; and practical student learning. Genuine collaboration between the two organisations was considered crucial for delivering a quality programme and providing the required support for students. Transformative leadership could inform this collaboration by promoting acknowledgement of and respect for differences.

Surface functionalized SiO2 nanoparticles with cationic polymers via the combination of mussel inspired chemistry and surface initiated atom transfer radical polymerization: Characterization and enhanced removal of organic dye.

PubMed

Huang, Qiang; Liu, Meiying; Mao, Liucheng; Xu, Dazhuang; Zeng, Guangjian; Huang, Hongye; Jiang, Ruming; Deng, Fengjie; Zhang, Xiaoyong; Wei, Yen

2017-08-01

Monodispersed SiO 2 particles functionalized with cationic polymers poly-((3-acrylamidopropyl)trimethylammonium chloride) (PAPTCl) were prepared using mussel inspired surface modification strategy and surface initiated atom transfer radical polymerization (SI-ATRP). Fourier transform infrared spectroscopy, transmission electron microscope, thermogravimetric analysis, X-ray photoelectron spectroscopy, and zeta potential were employed to characterize these SiO 2 samples. The adsorption performance of the functionalized SiO 2 (donated as SiO 2 -PDA-PAPTCl) towards anionic organic dye Congo red (CR) was investigated to evaluate their potential environmental applications. We demonstrated that the surface of SiO 2 particles can be successfully functionalized with cationic PAPTCl. The adsorption capability of as-prepared SiO 2 was found to increases from 28.70 and 106.65mg/g after surface grafted with cationic polymers. The significant enhancement in the adsorption capability of SiO 2 -PDA-PAPTCl is mainly attributed to the introduction of cationic polymers. More importantly, this strategy is expected to be promising for fabrication of many other functional polymer nanocomposites for environmental applications due to the universality of mussel inspired chemistry and well designability and good monomer adaptability of SI-ATRP. Copyright © 2017 Elsevier Inc. All rights reserved.

Generalized Synthesis of Ternary Sulfide Hollow Structures with Enhanced Photocatalytic Performance for Degradation and Hydrogen Evolution.

PubMed

Ding, Shuoping; Liu, Xiufan; Shi, Yiqiu; Liu, Ye; Zhou, Tengfei; Guo, Zaiping; Hu, Juncheng

2018-05-17

A series of ternary sulfide hollow structures have been successfully prepared by a facile glutathione (GSH)-assisted one-step hydrothermal route, where GSH acts as the source of sulfur and bubble template. We demonstrate the feasibility and versatility of this in situ gas-bubble template strategy by the fabrication of novel hollow structures of MIn 2 S 4 (M = Cd, Zn, Ca, Mg, and Mn). Interestingly, with the reaction time varying, the hierarchical CdIn 2 S 4 microspheres with controlled internal structures can be regulated from yolk-shell, smaller yolk-shell (yolk-shell with shrunk yolk), hollow, to solid. Under visible-light irradiation, all of our prepared CdIn 2 S 4 samples with different morphologies were photoactivated. In virtue of the appealing hierarchical hollow structure, the yolk-shell-structured CdIn 2 S 4 microspheres exhibited the optimal photocatalytic activity and excellent durability for both the X 3 B degradation and H 2 evolution, which can be ascribed to the synergy-promoting effect of the small crystallite size together with the unique structural advantages of the yolk-shell structure. Thus, we hypothesize that this proof-of-concept strategy paves an example of rational design of hollow structured ternary or multinary sulfides with superior photochemical performance, holding great potential for future multifunctional applications.

[Comparison of the Conventional Centrifuged and Filtrated Preparations in Urine Cytology].

PubMed

Sekita, Nobuyuki; Shimosakai, Hirofumi; Nishikawa, Rika; Sato, Hiroaki; Kouno, Hiroyoshi; Fujimura, Masaaki; Mikami, Kazuo

2016-03-01

The urine cytology test is one of the most important tools for the diagnosis of malignant urinary tract tumors. This test is also of great value for predicting malignancy. However, the sensitivity of this test is not high enough to screen for malignant cells. In our laboratory, we were able to attain a high sensitivity of urine cytology tests after changing the preparation method of urine samples. The differences in the cytodiagnosis between the two methods are discussed here. From January 2012 to June 2013, 2,031 urine samples were prepared using the conventional centrifuge method (C method) ; and from September 2013 to March 2015, 2,453 urine samples were prepared using the filtration method (F method) for the cytology test. When the samples included in category 4 or 5, were defined as cytological positive, the sensitivities of this test with samples prepared using the F method were significantly high compared with samples prepared using the C method (72% vs 28%, p＜0.001). The number of cells on the glass slides prepared by the F method was significantly higher than that of the samples prepared by the C method (p＜0.001). After introduction of the F method, the number of f alse negative cases was decreased in the urine cytology test because a larger number of cells was seen and easily detected as atypical or malignant epithelial cells. Therefore, this method has a higher sensitivity than the conventional C method as the sensitivity of urine cytology tests relies partially on the number of cells visualized in the prepared samples.

Direct synthesis of nitrogen-doped graphene on platinum wire as a new fiber coating method for the solid-phase microextraction of BXes in water samples: Comparison of headspace and cold-fiber headspace modes.

PubMed

Memarian, Elham; Hosseiny Davarani, Saied Saeed; Nojavan, Saeed; Movahed, Siyavash Kazemi

2016-09-07

In this work, a new solid-phase microextraction fiber was prepared based on nitrogen-doped graphene (N-doped G). Moreover, a new strategy was proposed to solve problems dealt in direct coating of N-doped G. For this purpose, first, Graphene oxide (GO) was coated on Pt wire by electrophoretic deposition method. Then, chemical reduction of coated GO to N-doped G was accomplished by hydrazine and NH3. The prepared fiber showed good mechanical and thermal stabilities. The obtained fiber was used in two different modes (conventional headspace solid-phase microextraction and cold-fiber headspace solid-phase microextraction (CF-HS-SPME)). Both modes were optimized and applied for the extraction of benzene and xylenes from different aqueous samples. All effective parameters including extraction time, salt content, stirring rate, and desorption time were optimized. The optimized CF-HS-SPME combined with GC-FID showed good limit of detections (LODs) (0.3-2.3 μg/L), limit of quantifications (LOQs) (1.0-7.0 μg/L) and linear ranges (1.0-5000 μg/L). The developed method was applied for the analysis of benzene and xylenes in rainwater and some wastewater samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Systematic Assessment of Seven Solvent and Solid-Phase Extraction Methods for Metabolomics Analysis of Human Plasma by LC-MS

NASA Astrophysics Data System (ADS)

Sitnikov, Dmitri G.; Monnin, Cian S.; Vuckovic, Dajana

2016-12-01

The comparison of extraction methods for global metabolomics is usually executed in biofluids only and focuses on metabolite coverage and method repeatability. This limits our detailed understanding of extraction parameters such as recovery and matrix effects and prevents side-by-side comparison of different sample preparation strategies. To address this gap in knowledge, seven solvent-based and solid-phase extraction methods were systematically evaluated using standard analytes spiked into both buffer and human plasma. We compared recovery, coverage, repeatability, matrix effects, selectivity and orthogonality of all methods tested for non-lipid metabolome in combination with reversed-phased and mixed-mode liquid chromatography mass spectrometry analysis (LC-MS). Our results confirmed wide selectivity and excellent precision of solvent precipitations, but revealed their high susceptibility to matrix effects. The use of all seven methods showed high overlap and redundancy which resulted in metabolite coverage increases of 34-80% depending on LC-MS method employed as compared to the best single extraction protocol (methanol/ethanol precipitation) despite 7x increase in MS analysis time and sample consumption. The most orthogonal methods to methanol-based precipitation were ion-exchange solid-phase extraction and liquid-liquid extraction using methyl-tertbutyl ether. Our results help facilitate rational design and selection of sample preparation methods and internal standards for global metabolomics.

Systematic Assessment of Seven Solvent and Solid-Phase Extraction Methods for Metabolomics Analysis of Human Plasma by LC-MS

PubMed Central

Sitnikov, Dmitri G.; Monnin, Cian S.; Vuckovic, Dajana

2016-01-01

The comparison of extraction methods for global metabolomics is usually executed in biofluids only and focuses on metabolite coverage and method repeatability. This limits our detailed understanding of extraction parameters such as recovery and matrix effects and prevents side-by-side comparison of different sample preparation strategies. To address this gap in knowledge, seven solvent-based and solid-phase extraction methods were systematically evaluated using standard analytes spiked into both buffer and human plasma. We compared recovery, coverage, repeatability, matrix effects, selectivity and orthogonality of all methods tested for non-lipid metabolome in combination with reversed-phased and mixed-mode liquid chromatography mass spectrometry analysis (LC-MS). Our results confirmed wide selectivity and excellent precision of solvent precipitations, but revealed their high susceptibility to matrix effects. The use of all seven methods showed high overlap and redundancy which resulted in metabolite coverage increases of 34–80% depending on LC-MS method employed as compared to the best single extraction protocol (methanol/ethanol precipitation) despite 7x increase in MS analysis time and sample consumption. The most orthogonal methods to methanol-based precipitation were ion-exchange solid-phase extraction and liquid-liquid extraction using methyl-tertbutyl ether. Our results help facilitate rational design and selection of sample preparation methods and internal standards for global metabolomics. PMID:28000704

Effect of Genetic Database Comprehensiveness on Fractional Proteomics of Escherichia coli O157:H7

DTIC Science & Technology

2014-01-01

proteins would be observed in the extracellular fraction. 15. SUBJECT TERMS Escherichia coli O157:H7 Liquid chromatography Mass spectrometry...Preparation ...............1 2.2 Liquid Chromatography /Mass Spectrometry Sample Preparation ....................2 2.3 Liquid Chromatography /Mass... Chromatography /Mass Spectrometry Sample Preparation. Samples were prepared for liquid chromatography tandem mass spectrometry (LC-MS/MS) in a similar

Emergency preparedness in a sample of persons with disabilities.

PubMed

Gershon, Robyn R M; Kraus, Lewis E; Raveis, Victoria H; Sherman, Martin F; Kailes, June I

2013-01-01

The objective of this study was to characterize emergency preparedness in this vulnerable population, and to ascertain the role of the personal assistant (PA) and the potential impact of prior emergency experience on preparedness efforts. Cross-sectional Internet-based survey conducted in 2011. Convenience sample. Two-hundred fifty-three community residents with cognitive and /or physical disabilities, all receiving personal assistance services. Emergency preparedness, operationalized as responses to a seven-item scale. The mean score for the emergency preparedness scale was 2.32 (SD = 2.74), range 0-7. Even though 62.8 percent (n = 159) of the participants had previously experienced one or more large-scale emergencies, only 47.4 percent (n = 120) of the entire sample and 55.3 percent (n = 88) of those with actual emergency experience reported preparing an emergency plan. Sixty-three percent (n = 76) of those reporting a plan had involved their PA in its development. Participants who reported such involvement were significantly more likely to have higher scores on the emergency preparedness scale (p < 0.001). Participants who had experienced a prior emergency were also more likely to score higher on the emergency preparedness scale (p < 0.001). In general, participants reported limited attention to other basic preparedness recommendations: only 28 percent (n = 70) had prepared a "go-bag" with necessary supplies, 29 percent (n = 74) had developed a strategy for communicating with their PA during emergencies, and 32 percent (n = 81) had stockpiled emergency supplies. Of particular importance, only 26 percent (n = 66) had made alternative back-up plans for personal assistance. Involving the PA in the planning process and experiencing an emergency were both significantly associated with higher emergency preparedness scores in this sample of people living with disabilities. However, critical deficiencies in preparedness were noted, such as lack of back-up plans for replacing their PA. Despite a concerted national effort to improve preparedness in the population of people living with disabilities, important preparedness gaps remain. These findings highlight the need for additional study on emergency preparedness barriers in people living with disabilities so that effective strategies to reduce vulnerabilities can be identified.

Utility of Cytospin and Cell block Technology in Evaluation of Body Fluids and Urine Samples: A Comparative Study.

PubMed

Qamar, Irmeen; Rehman, Suhailur; Mehdi, Ghazala; Maheshwari, Veena; Ansari, Hena A; Chauhan, Sunanda

2018-01-01

Cytologic examination of body fluids commonly involves the use of direct or sediment smears, cytocentrifuge preparations, membrane filter preparations, or cell block sections. Cytospin and cell block techniques are extremely useful in improving cell yield of thin serous effusions and urine samples, and ensure high diagnostic efficacy. We studied cytospin preparations and cell block sections prepared from 180 samples of body fluids and urine samples to compare the relative efficiency of cell retrieval, preservation of cell morphology, ease of application of special stains, and diagnostic efficacy. Samples were collected and processed to prepare cytospin smears and cell block sections. We observed that overall, cell yield and preservation of individual cell morphology were better in cytospin preparations as compared to cell blocks, while preservation of architectural pattern was better in cell block sections. The number of suspicious cases also decreased on cell block sections, with increased detection of malignancy. It was difficult to prepare cell blocks from urine samples due to low cellularity. Cytospin technology is a quick, efficient, and cost-effective method of increasing cell yield in hypocellular samples, with better preservation of cell morphology. Cell blocks are better prepared from high cellularity fluids; however, tissue architecture is better studied, with improved rate of diagnosis and decrease in ambiguous results. Numerous sections can be prepared from a small amount of material. Special stains and immunochemical stains can be easily applied to cell blocks. It also provides a source of archival material.

An optical fusion gate for W-states

NASA Astrophysics Data System (ADS)

Özdemir, Ş. K.; Matsunaga, E.; Tashima, T.; Yamamoto, T.; Koashi, M.; Imoto, N.

2011-10-01

We introduce a simple optical gate to fuse arbitrary-size polarization entangled W-states to prepare larger W-states. The gate requires a polarizing beam splitter (PBS), a half-wave plate (HWP) and two photon detectors. We study, numerically and analytically, the necessary resource consumption for preparing larger W-states by fusing smaller ones with the proposed fusion gate. We show analytically that resource requirement scales at most sub-exponentially with the increasing size of the state to be prepared. We numerically determine the resource cost for fusion without recycling where W-states of arbitrary size can be optimally prepared. Moreover, we introduce another strategy that is based on recycling and outperforms the optimal strategy for the non-recycling case.

Facile synthesis of upconversion nanoparticles with high purity using lanthanide oleate compounds

NASA Astrophysics Data System (ADS)

Kang, Ning; Ai, Chao-Chao; Zhou, Ya-Ming; Wang, Zuo; Ren, Lei

2018-02-01

A novel strategy for preparing highly pure NaYF4-based upconversion nanoparticles (UCNPs) was developed using lanthanide oleate compounds [Ln(OA)3] as the precursor, denoted as the Ln-OA preparation method. Compared to the conventional solvothermal method for synthesizing UCNPs using lanthanide chloride compounds (LnCl3) as the precursor (denoted as the Ln-Cl method), the Ln-OA strategy exhibited the merits of high purity, reduced purification process and a uniform size in preparing core and core-shell UCNPs excited by a 980 or 808 nm near infrared (NIR) laser. This work sheds new insight on the preparation of UCNPs and promotes their application in biomedical fields.

Extending the solvent-free MALDI sample preparation method.

PubMed

Hanton, Scott D; Parees, David M

2005-01-01

Matrix-assisted laser desorption/ionization (MALDI) mass spectrometry is an important technique to characterize many different materials, including synthetic polymers. MALDI mass spectral data can be used to determine the polymer average molecular weights, repeat units, and end groups. One of the key issues in traditional MALDI sample preparation is making good solutions of the analyte and the matrix. Solvent-free sample preparation methods have been developed to address these issues. Previous results of solvent-free or dry prepared samples show some advantages over traditional wet sample preparation methods. Although the results of the published solvent-free sample preparation methods produced excellent mass spectra, we found the method to be very time-consuming, with significant tool cleaning, which presents a significant possibility of cross contamination. To address these issues, we developed an extension of the solvent-free method that replaces the mortar and pestle grinding with ball milling the sample in a glass vial with two small steel balls. This new method generates mass spectra with equal quality of the previous methods, but has significant advantages in productivity, eliminates cross contamination, and is applicable to liquid and soft or waxy analytes.

Investigating Peer Review as an Intentional Learning Strategy to Foster Collaborative Knowledge-Building in Students of Instructional Design

ERIC Educational Resources Information Center

Brill, Jennifer M.; Hodges, Charles B.

2011-01-01

Peer review has been advocated for as an intentional strategy to support the knowledge and skill attainment of adult learners preparing for professional practice, including those students preparing for instructional design and technology practice. The purposes of this article are to discuss the practical application of peer review as an…

Collaborative testing as a learning strategy in nursing education.

PubMed

Sandahl, Sheryl S

2010-01-01

A primary goal of nursing education is to prepare nurses to work collaboratively as members of interprofessional health care teams on behalf of patients. Collaborative testing is a collaborative learning strategy used to foster knowledge development, critical thinking in decision making, and group processing skills. This study incorporated a quasi-experimental design with a comparison group to examine the effect of collaborative testing as a learning strategy on student learning and retention of course content as well as group process skills and student perceptions of their learning and anxiety. The setting was a baccalaureate nursing program; the sample consisted of two groups of senior students enrolled in Medical-Surgical Nursing II. Student learning, as measured by unit examination scores, was greater for students taking examinations collaboratively compared to individually. Retention of course content, as measured by final examination scores, was not greater for students taking examinations collaboratively compared to individually. Student perceptions were overwhelmingly positive, with students reporting increased learning as a result of the collaborative testing experiences. Despite the lack of data to support increased retention, collaborative testing may be a learning strategy worth implementing in nursing education. Students reported more positive interactions and collaboration with their peers, skills required by the professional nurse.

Optimizing exosomal RNA isolation for RNA-Seq analyses of archival sera specimens.

PubMed

Prendergast, Emily N; de Souza Fonseca, Marcos Abraão; Dezem, Felipe Segato; Lester, Jenny; Karlan, Beth Y; Noushmehr, Houtan; Lin, Xianzhi; Lawrenson, Kate

2018-01-01

Exosomes are endosome-derived membrane vesicles that contain proteins, lipids, and nucleic acids. The exosomal transcriptome mediates intercellular communication, and represents an understudied reservoir of novel biomarkers for human diseases. Next-generation sequencing enables complex quantitative characterization of exosomal RNAs from diverse sources. However, detailed protocols describing exosome purification for preparation of exosomal RNA-sequence (RNA-Seq) libraries are lacking. Here we compared methods for isolation of exosomes and extraction of exosomal RNA from human cell-free serum, as well as strategies for attaining equal representation of samples within pooled RNA-Seq libraries. We compared commercial precipitation with ultracentrifugation for exosome purification and confirmed the presence of exosomes via both transmission electron microscopy and immunoblotting. Exosomal RNA extraction was compared using four different RNA purification methods. We determined the minimal starting volume of serum required for exosome preparation and showed that high quality exosomal RNA can be isolated from sera stored for over a decade. Finally, RNA-Seq libraries were successfully prepared with exosomal RNAs extracted from human cell-free serum, cataloguing both coding and non-coding exosomal transcripts. This method provides researchers with strategic options to prepare RNA-Seq libraries and compare RNA-Seq data quantitatively from minimal volumes of fresh and archival human cell-free serum for disease biomarker discovery.

Antifouling membranes for sustainable water purification: strategies and mechanisms.

PubMed

Zhang, Runnan; Liu, Yanan; He, Mingrui; Su, Yanlei; Zhao, Xueting; Elimelech, Menachem; Jiang, Zhongyi

2016-10-24

One of the greatest challenges to the sustainability of modern society is an inadequate supply of clean water. Due to its energy-saving and cost-effective features, membrane technology has become an indispensable platform technology for water purification, including seawater and brackish water desalination as well as municipal or industrial wastewater treatment. However, membrane fouling, which arises from the nonspecific interaction between membrane surface and foulants, significantly impedes the efficient application of membrane technology. Preparing antifouling membranes is a fundamental strategy to deal with pervasive fouling problems from a variety of foulants. In recent years, major advancements have been made in membrane preparation techniques and in elucidating the antifouling mechanisms of membrane processes, including ultrafiltration, nanofiltration, reverse osmosis and forward osmosis. This review will first introduce the major foulants and the principal mechanisms of membrane fouling, and then highlight the development, current status and future prospects of antifouling membranes, including antifouling strategies, preparation techniques and practical applications. In particular, the strategies and mechanisms for antifouling membranes, including passive fouling resistance and fouling release, active off-surface and on-surface strategies, will be proposed and discussed extensively.

Sample Preparation for Electron Probe Microanalysis—Pushing the Limits

PubMed Central

Geller, Joseph D.; Engle, Paul D.

2002-01-01

There are two fundamental considerations in preparing samples for electron probe microanalysis (EPMA). The first one may seem obvious, but we often find it is overlooked. That is, the sample analyzed should be representative of the population from which it comes. The second is a direct result of the assumptions in the calculations used to convert x-ray intensity ratios, between the sample and standard, to concentrations. Samples originate from a wide range of sources. During their journey to being excited under the electron beam for the production of x rays there are many possibilities for sample alteration. Handling can contaminate samples by adding extraneous matter. In preparation, the various abrasives used in sizing the sample by sawing, grinding and polishing can embed themselves. The most accurate composition of a contaminated sample is, at best, not representative of the original sample; it is misleading. Our laboratory performs EPMA analysis on customer submitted samples and prepares over 250 different calibration standards including pure elements, compounds, alloys, glasses and minerals. This large variety of samples does not lend itself to mass production techniques, including automatic polishing. Our manual preparation techniques are designed individually for each sample. The use of automated preparation equipment does not lend itself to this environment, and is not included in this manuscript. The final step in quantitative electron probe microanalysis is the conversion of x-ray intensities ratios, known as the “k-ratios,” to composition (in mass fraction or atomic percent) and/or film thickness. Of the many assumptions made in the ZAF (where these letters stand for atomic number, absorption and fluorescence) corrections the localized geometry between the sample and electron beam, or takeoff angle, must be accurately known. Small angular errors can lead to significant errors in the final results. The sample preparation technique then becomes very important, and, under certain conditions, may even be the limiting factor in the analytical uncertainty budget. This paper considers preparing samples to get known geometries. It will not address the analysis of samples with irregular, unprepared surfaces or unknown geometries. PMID:27446757

Expert opinion regarding the preparation of entry-level physiotherapists for primary healthcare practice, examined using Biggs 3P's model of teaching learning.

PubMed

McMahon, Sinead; O'Donoghue, Grainne; Doody, Catherine; O'Neill, Geraldine; Cusack, Tara

2016-05-01

The scope of contemporary physiotherapy practice is a critical factor in determining the appropriate educational preparation for physiotherapists now and into the future. The world-wide shift from secondary to primary healthcare has, and is, continuing to result in new and different ways of working. It is crucial that curricular changes reflect these developments. In this study a qualitative approach using Biggs 3P's - Pressage, Process and Product model to discuss curriculum design. The aim of the study was to explore the perspectives of both national and international physiotherapy educators/practitioners in primary healthcare, on the key elements required in physiotherapy education programmes to prepare future primary healthcare practitioners. Snowball sampling was used to identify experts in education and/or primary healthcare practice. Semi-structured interviews were conducted using an interview guide based on the Biggs 3P's model. Twelve participants were recruited from Ireland (n = 2), the UK (n = 4), Canada (n = 3), New Zealand (n = 2) and Australia (n = 1) using snowball sampling. Interviews were analysed using thematic analysis. Themes identified included; understanding the philosophy of physiotherapy practice, cultural competence, inter-disciplinary team working and communication skills. Contextual factors and teaching and learning strategies were discussed. There is an urgent need for physiotherapy education programmes to adopt the concept of primary healthcare as the basis for the physiotherapy curriculum and illuminate key components for consideration.

Facile formation of Ag{sub 2}WO{sub 4}/AgX (X = Cl, Br, I) hybrid nanorods with enhanced visible-light-driven photoelectrochemical properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Jingjing; Yu, Caiyun; Zheng, Changcheng

2015-01-15

Highlights: • Ag{sub 2}WO{sub 4}/AgX hybrid nanorods were prepared by a facile in-situ anion exchange reaction. • Ag{sub 2}WO{sub 4} nanorods and different X{sup −} ions were reacted in water at room temperature. • The hybrids possess significantly enhanced photoelectrochemical properties. • Ag{sub 2}WO{sub 4}/AgBr hybrids exhibit the highest photocatalytic activity among three samples. • The active species tests were also investigated to confirm photocatalytic mechanism. - Abstract: In this work, we demonstrated a general strategy for the preparation of a series of uniform Ag{sub 2}WO{sub 4}/AgX (X = Cl, Br, I) hybrid nanorods by a facile in-situ anion exchangemore » reaction occurring at room temperature between pregrown Ag{sub 2}WO{sub 4} nanorods and different X{sup −} ions in water. Compared with Ag{sub 2}WO{sub 4} nanorods, further investigation has revealed that the as-prepared hybrid nanorods possess significantly enhanced photocurrent response and photocatalytic activity in degrading methyl orange (MO) under visible-light irradiation. In particular, the Ag{sub 2}WO{sub 4}/AgBr hybrid nanorods exhibit the highest photocatalytic activity among the three kinds of samples. The active species tests indicate that superoxide anion radicals and photogenerated holes are responsible for the enhanced photocatalytic performance.« less

Strategy to combat obesity and to promote physical activity in Arab countries.

PubMed

Musaiger, Abdulrahman O; Al Hazzaa, Hazzaa M; Al-Qahtani, Aayed; Elati, Jalila; Ramadan, Jasem; Aboulella, Nebal A; Mokhtar, Najat; Kilani, Hashem A

2011-01-01

Obesity has become a major public health problem in the Arab countries, creating a health and economic burden on these countries' government services. There is an urgent need to develop a strategy for prevention and control of obesity. The third Arab Conference on Obesity and Physical Activity was held in Bahrain in January 2010, and proposed the Strategy to Combat Obesity and Promote Physical Activity in Arab Countries. This strategy provides useful guidelines for each Arab country to prepare its own strategy or plan of action to prevent and control obesity. The strategy focused on expected outcomes, objectives, indicators to measure the objectives, and action needs for 9 target areas: child-care centers for preschool children, schools, primary health care, secondary care, food companies, food preparation institutes, media, public benefit organizations, and the workplace. Follow-up and future developments of this strategy were also included.

Strategy to combat obesity and to promote physical activity in Arab countries

PubMed Central

Musaiger, Abdulrahman O; Al Hazzaa, Hazzaa M; Al-Qahtani, Aayed; Elati, Jalila; Ramadan, Jasem; AboulElla, Nebal A; Mokhtar, Najat; Kilani, Hashem A

2011-01-01

Obesity has become a major public health problem in the Arab countries, creating a health and economic burden on these countries’ government services. There is an urgent need to develop a strategy for prevention and control of obesity. The third Arab Conference on Obesity and Physical Activity was held in Bahrain in January 2010, and proposed the Strategy to Combat Obesity and Promote Physical Activity in Arab Countries. This strategy provides useful guidelines for each Arab country to prepare its own strategy or plan of action to prevent and control obesity. The strategy focused on expected outcomes, objectives, indicators to measure the objectives, and action needs for 9 target areas: child-care centers for preschool children, schools, primary health care, secondary care, food companies, food preparation institutes, media, public benefit organizations, and the workplace. Follow-up and future developments of this strategy were also included. PMID:21660292

Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation

NASA Technical Reports Server (NTRS)

Sarrazin, P.; Chipera, S.; Bish, D.; Blake, D.; Feldman, S.; Vaniman, D.; Bryson, C.

2004-01-01

Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.

Chromatography in Industry

NASA Astrophysics Data System (ADS)

Schoenmakers, Peter

2009-07-01

This review focuses on the chromatography research that has been carried out within industry or in close cooperation with industry and that has been reported in the scientific literature between 2006 and mid-2008. Companies in the health care sector, such as pharmaceutical and biotechnology companies, are the largest contributors. Industrial research seems to take place in an open environment in cooperation with academia, peer companies, and institutions. Industry appears ready to embrace new technologies as they emerge, but they focus strongly on making chromatography work robustly, reliably, rapidly, and automatically. “Hyphenated” systems that incorporate on-line sample-preparation techniques and mass-spectrometric detection are the rule rather than the exception. Various multidimensional separation methods are finding numerous applications. Strategies aimed at speeding up the development of new chromatographic methods remain the focus of attention. Also, there is a clear trend toward exploring chromatographic methods for parallel processing along with other strategies for high-throughput analysis.

Sampling hazelnuts for aflatoxin: uncertainty associated with sampling, sample preparation, and analysis.

PubMed

Ozay, Guner; Seyhan, Ferda; Yilmaz, Aysun; Whitaker, Thomas B; Slate, Andrew B; Giesbrecht, Francis

2006-01-01

The variability associated with the aflatoxin test procedure used to estimate aflatoxin levels in bulk shipments of hazelnuts was investigated. Sixteen 10 kg samples of shelled hazelnuts were taken from each of 20 lots that were suspected of aflatoxin contamination. The total variance associated with testing shelled hazelnuts was estimated and partitioned into sampling, sample preparation, and analytical variance components. Each variance component increased as aflatoxin concentration (either B1 or total) increased. With the use of regression analysis, mathematical expressions were developed to model the relationship between aflatoxin concentration and the total, sampling, sample preparation, and analytical variances. The expressions for these relationships were used to estimate the variance for any sample size, subsample size, and number of analyses for a specific aflatoxin concentration. The sampling, sample preparation, and analytical variances associated with estimating aflatoxin in a hazelnut lot at a total aflatoxin level of 10 ng/g and using a 10 kg sample, a 50 g subsample, dry comminution with a Robot Coupe mill, and a high-performance liquid chromatographic analytical method are 174.40, 0.74, and 0.27, respectively. The sampling, sample preparation, and analytical steps of the aflatoxin test procedure accounted for 99.4, 0.4, and 0.2% of the total variability, respectively.

Analytical tools for the analysis of β-carotene and its degradation products

PubMed Central

Stutz, H.; Bresgen, N.; Eckl, P. M.

2015-01-01

Abstract β-Carotene, the precursor of vitamin A, possesses pronounced radical scavenging properties. This has centered the attention on β-carotene dietary supplementation in healthcare as well as in the therapy of degenerative disorders and several cancer types. However, two intervention trials with β-carotene have revealed adverse effects on two proband groups, that is, cigarette smokers and asbestos-exposed workers. Beside other causative reasons, the detrimental effects observed have been related to the oxidation products of β-carotene. Their generation originates in the polyene structure of β-carotene that is beneficial for radical scavenging, but is also prone to oxidation. Depending on the dominant degradation mechanism, bond cleavage might occur either randomly or at defined positions of the conjugated electron system, resulting in a diversity of cleavage products (CPs). Due to their instability and hydrophobicity, the handling of standards and real samples containing β-carotene and related CPs requires preventive measures during specimen preparation, analyte extraction, and final analysis, to avoid artificial degradation and to preserve the initial analyte portfolio. This review critically discusses different preparation strategies of standards and treatment solutions, and also addresses their protection from oxidation. Additionally, in vitro oxidation strategies for the generation of oxidative model compounds are surveyed. Extraction methods are discussed for volatile and non-volatile CPs individually. Gas chromatography (GC), (ultra)high performance liquid chromatography (U)HPLC, and capillary electrochromatography (CEC) are reviewed as analytical tools for final analyte analysis. For identity confirmation of analytes, mass spectrometry (MS) is indispensable, and the appropriate ionization principles are comprehensively discussed. The final sections cover analysis of real samples and aspects of quality assurance, namely matrix effects and method validation. PMID:25867077

Dissolution enhancement of Deflazacort using hollow crystals prepared by antisolvent crystallization process.

PubMed

Paulino, A S; Rauber, G; Campos, C E M; Maurício, M H P; de Avillez, R R; Capobianco, G; Cardoso, S G; Cuffini, S L

2013-05-13

Deflazacort (DFZ), a derivate of prednisolone, is a poorly soluble drug which has been proposed to have major advantages over other corticosteroids. Poorly soluble drugs present limited bioavailability due to their low solubility and dissolution rate and several strategies have been developed in order to find ways to improve them. In general, pharmaceutical laboratories use a micronized process to reduce the particle size in order to increase the dissolution of the drugs. However, this process causes changes such as polymorphic transitions, particle agglomeration and a reduction in fluidity and wettability. These solid-state properties affect the dissolution behavior and stability performance of drugs. Crystallization techniques are widely used in the pharmaceutical industry and antisolvent crystallization has been used to obtain ultrafine particles. In this study, DFZ was investigated in terms of its antisolvent crystallization in different solvents and under various preparation conditions (methanol/water ratio, stirring and evaporation rate, etc.), in order to compare the physicochemical properties between crystallized samples and raw materials available on the Brazilian market with and without micronization. Crystalline structure, morphology, and particle size, and their correlation with the Intrinsic Dissolution Rate (IDR) and dissolution profile as relevant biopharmaceutical properties were studied. Crystallization conditions were achieved which provided crystalline samples of hollow-shaped crystals with internal channels, which increased the dissolution rate of DFZ. The antisolvent crystallization process allowed the formation of hollow crystals, which demonstrated a better dissolution profile than the raw material (crystalline and micronized), making this a promising technique as a crystallization strategy for improving the dissolution and thus the bioavailability of poorly soluble drugs. Copyright © 2013 Elsevier B.V. All rights reserved.

Hotspots engineering by grafting Au@Ag core-shell nanoparticles on the Au film over slightly etched nanoparticles substrate for on-site paraquat sensing.

PubMed

Wang, Chaoguang; Wu, Xuezhong; Dong, Peitao; Chen, Jian; Xiao, Rui

2016-12-15

Paraquat (PQ) pollutions are ultra-toxic to human beings and hard to be decomposed in the environment, thus requiring an on-site detection strategy. Herein, we developed a robust and rapid PQ sensing strategy based on the surface-enhanced Raman scattering (SERS) technique. A hybrid SERS substrate was prepared by grafting the Au@Ag core-shell nanoparticles (NPs) on the Au film over slightly etched nanoparticles (Au FOSEN). Hotspots were engineered at the junctions as indicated by the finite difference time domain calculation. SERS performance of the hybrid substrate was explored using p-ATP as the Raman probe. The hybrid substrate gives higher enhancement factor comparing to either the Au FOSEN substrate or the Au@Ag core-shell NPs, and exhibits excellent reproducibility, homogeneity and stability. The proposed SERS substrates were prepared in batches for the practical PQ sensing. The total analysis time for a single sample, including the pre-treatment and measurement, was less than 5min with a PQ detection limit of 10nM. Peak intensities of the SERS signal were plotted as a function of the PQ concentrations to calibrate the sensitivity by fitting the Hill's equation. The plotted calibration curve showed a good log-log linearity with the coefficient of determination of 0.98. The selectivity of the sensing proposal was based on the "finger print" Raman spectra of the analyte. The proposed substrate exhibited good recovery when it applied to real water samples, including lab tap water, bottled water, and commercially obtained apple juice and grape juice. This SERS-based PQ detection method is simple, rapid, sensitive and selective, which shows great potential in pesticide residue and additives abuse monitoring. Copyright © 2016 Elsevier B.V. All rights reserved.

7 CFR 61.34 - Drawing and preparation of sample.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 3 2010-01-01 2010-01-01 false Drawing and preparation of sample. 61.34 Section 61.34 Agriculture Regulations of the Department of Agriculture (Continued) AGRICULTURAL MARKETING SERVICE (Standards... Cottonseed Samplers § 61.34 Drawing and preparation of sample. Each licensed cottonseed sampler shall draw...

CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING AIR SAMPLES FOR ANALYSIS OF POLAR PERSISTENT ORGANIC POLLUTANTS (SOP-5.13)

EPA Science Inventory

The method for extracting and preparing indoor and outdoor air samples for analysis of polar persistent organic pollutants is summarized in this SOP. It covers the preparation of samples that are to be analyzed by gas chromatography/mass spectrometry.

40 CFR 761.392 - Preparing validation study samples.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Preparing validation study samples..., AND USE PROHIBITIONS Comparison Study for Validating a New Performance-Based Decontamination Solvent Under § 761.79(d)(4) § 761.392 Preparing validation study samples. (a)(1) To validate a procedure to...

40 CFR 761.392 - Preparing validation study samples.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 31 2011-07-01 2011-07-01 false Preparing validation study samples..., AND USE PROHIBITIONS Comparison Study for Validating a New Performance-Based Decontamination Solvent Under § 761.79(d)(4) § 761.392 Preparing validation study samples. (a)(1) To validate a procedure to...

7 CFR 27.89 - Expenses; inspection; sampling.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 2 2011-01-01 2011-01-01 false Expenses; inspection; sampling. 27.89 Section 27.89... Micronaire § 27.89 Expenses; inspection; sampling. Expense of inspection and sampling, the preparation of the... Office, the expense of inspection, sampling, preparation of samples, and delivery of the samples to the...

7 CFR 27.89 - Expenses; inspection; sampling.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 2 2010-01-01 2010-01-01 false Expenses; inspection; sampling. 27.89 Section 27.89... Micronaire § 27.89 Expenses; inspection; sampling. Expense of inspection and sampling, the preparation of the... Office, the expense of inspection, sampling, preparation of samples, and delivery of the samples to the...

Imaging Gallium Nitride High Electron Mobility Transistors to Identify Point Defects

DTIC Science & Technology

2014-03-01

streamline the sample preparation procedure to maximize the yield of successful samples to be analyzed chemically in an energy dispersive spectrometry...transmission electron microscope (STEM), sample preparation 15. NUMBER OF PAGES 103 16. PRICE CODE 17. SECURITY CLASSIFICATION OF REPORT...Computer Engineering iii THIS PAGE INTENTIONALLY LEFT BLANK iv ABSTRACT The purpose of this thesis is to streamline the sample preparation

Pulsed-voltage atom probe tomography of low conductivity and insulator materials by application of ultrathin metallic coating on nanoscale specimen geometry.

PubMed

Adineh, Vahid R; Marceau, Ross K W; Chen, Yu; Si, Kae J; Velkov, Tony; Cheng, Wenlong; Li, Jian; Fu, Jing

2017-10-01

We present a novel approach for analysis of low-conductivity and insulating materials with conventional pulsed-voltage atom probe tomography (APT), by incorporating an ultrathin metallic coating on focused ion beam prepared needle-shaped specimens. Finite element electrostatic simulations of coated atom probe specimens were performed, which suggest remarkable improvement in uniform voltage distribution and subsequent field evaporation of the insulated samples with a metallic coating of approximately 10nm thickness. Using design of experiment technique, an experimental investigation was performed to study physical vapor deposition coating of needle specimens with end tip radii less than 100nm. The final geometries of the coated APT specimens were characterized with high-resolution scanning electron microscopy and transmission electron microscopy, and an empirical model was proposed to determine the optimal coating thickness for a given specimen size. The optimal coating strategy was applied to APT specimens of resin embedded Au nanospheres. Results demonstrate that the optimal coating strategy allows unique pulsed-voltage atom probe analysis and 3D imaging of biological and insulated samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Technology assessment and strategy for development of a Rapid Field Water Microbiology Test Kit. Technical report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Preston, D.R.; Schaub, S.A.

1991-09-01

A literature and market search of existing technology for the detection, identification, and quantification of microorganisms in water was conducted. Based upon the availability of technologies and their configurations, an assessment of the appropriate strategies to pursue for the near and long term development plans in development of the Rapid Field Bacteriology Test Kit was performed. Near term technologies to improve the Army's capability to detect microorganisms would appear to be essentially improvements in versatility and measurement of coliform indicator organisms. New chromogenic and fluorogenic indicator substances associated with new substrates appear to be best suited for test kit developmentmore » either for quantitative membrane filter tests or presence/absence and multiple fermentation tests. Test times, incubator requirements, and operator involvement appear to be similar to older technologies. Long term development would appear to favor such technologies as genetic probes with amplification of the hydridized nucleic acid materials of positive samples, and some immunological based systems such as enzyme linked, immuno-sorbent assays. In both cases, the major problems would appear to be sample preparation and development of signal strengths from the reactions which would allow the user to see results in 1 hour.« less

Utility of Cytospin and Cell block Technology in Evaluation of Body Fluids and Urine Samples: A Comparative Study

PubMed Central

Qamar, Irmeen; Rehman, Suhailur; Mehdi, Ghazala; Maheshwari, Veena; Ansari, Hena A.; Chauhan, Sunanda

2018-01-01

Background: Cytologic examination of body fluids commonly involves the use of direct or sediment smears, cytocentrifuge preparations, membrane filter preparations, or cell block sections. Cytospin and cell block techniques are extremely useful in improving cell yield of thin serous effusions and urine samples, and ensure high diagnostic efficacy. Materials and Methods: We studied cytospin preparations and cell block sections prepared from 180 samples of body fluids and urine samples to compare the relative efficiency of cell retrieval, preservation of cell morphology, ease of application of special stains, and diagnostic efficacy. Samples were collected and processed to prepare cytospin smears and cell block sections. Results: We observed that overall, cell yield and preservation of individual cell morphology were better in cytospin preparations as compared to cell blocks, while preservation of architectural pattern was better in cell block sections. The number of suspicious cases also decreased on cell block sections, with increased detection of malignancy. It was difficult to prepare cell blocks from urine samples due to low cellularity. Conclusions: Cytospin technology is a quick, efficient, and cost-effective method of increasing cell yield in hypocellular samples, with better preservation of cell morphology. Cell blocks are better prepared from high cellularity fluids; however, tissue architecture is better studied, with improved rate of diagnosis and decrease in ambiguous results. Numerous sections can be prepared from a small amount of material. Special stains and immunochemical stains can be easily applied to cell blocks. It also provides a source of archival material. PMID:29643653

Steps Leading to an Ethnographic Analysis of Mothers Preparing Children for a Memory Test.

ERIC Educational Resources Information Center

Rogoff, Barbara; Gardner, William P.

In this study four research strategies used in previous studies of the socialization of cognitive skills were first contrasted and then assessed in terms of five criteria. (The data base for this study was 32 videotapes of mothers preparing their 7- or 9-year-old children to take a memory test.) The four strategies (frequency coding, fine-grained…

High-throughput automated microfluidic sample preparation for accurate microbial genomics

PubMed Central

Kim, Soohong; De Jonghe, Joachim; Kulesa, Anthony B.; Feldman, David; Vatanen, Tommi; Bhattacharyya, Roby P.; Berdy, Brittany; Gomez, James; Nolan, Jill; Epstein, Slava; Blainey, Paul C.

2017-01-01

Low-cost shotgun DNA sequencing is transforming the microbial sciences. Sequencing instruments are so effective that sample preparation is now the key limiting factor. Here, we introduce a microfluidic sample preparation platform that integrates the key steps in cells to sequence library sample preparation for up to 96 samples and reduces DNA input requirements 100-fold while maintaining or improving data quality. The general-purpose microarchitecture we demonstrate supports workflows with arbitrary numbers of reaction and clean-up or capture steps. By reducing the sample quantity requirements, we enabled low-input (∼10,000 cells) whole-genome shotgun (WGS) sequencing of Mycobacterium tuberculosis and soil micro-colonies with superior results. We also leveraged the enhanced throughput to sequence ∼400 clinical Pseudomonas aeruginosa libraries and demonstrate excellent single-nucleotide polymorphism detection performance that explained phenotypically observed antibiotic resistance. Fully-integrated lab-on-chip sample preparation overcomes technical barriers to enable broader deployment of genomics across many basic research and translational applications. PMID:28128213

Behavior of Aluminum in Solid Propellant Combustion

DTIC Science & Technology

1982-06-01

dry pressing 30% Valley Met H- 30 aluminum, 7% carnauba wax , and 63% 100 P AP. One sample was prepared using as received H-30, a second sample used pre...34propellant" formulations. The formulations included dry pressed AP/AI, and AP/AI/ Wax samples. Sandwiches were also prepared consisting of an aluminum...Binder flame instead of by aluminum exposure during accumulate break-up. Combustion of AP/AI/ Wax Samples A set of propellant samples were prepared by

Carbon dots based dual-emission silica nanoparticles as ratiometric fluorescent probe for nitrite determination in food samples.

PubMed

Xiang, Guoqiang; Wang, Yule; Zhang, Heng; Fan, Huanhuan; Fan, Lu; He, Lijun; Jiang, Xiuming; Zhao, Wenjie

2018-09-15

In this work, a simple and effective strategy for designing a ratiometric fluorescent nanosensor was described. A carbon dots (CDs) based dual-emission nanosensor for nitrite was prepared by coating the CDs on to dye-doped silica nanoparticles. Dual-emission silica nanoparticles fluorescence was quenched in sulfuric acid using potassium bromate (KBrO 3 ). The nitrite present catalyzed the KBrO 3 oxidation, resulting in ratiometric fluorescence response of the dual-emission silica nanoparticles. Several important parameters affecting the performance of the nanosensor were investigated. Under optimized conditions, the limit of detection was 1.0 ng mL -1 and the linear range 10-160 ng mL -1 . Furthermore, the sensor was suitable for nitrite determination in different food samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

Comparison of three officinal species of Callicarpa based on a biochemome profiling strategy with UHPLC-IT-MS and chemometrics analysis.

PubMed

Chen, Meng-Lu; Chang, Wen-Qi; Zhou, Jian-Liang; Yin, Ying-Hao; Xia, Wen-Rui; Liu, Jian-Qun; Liu, Li-Fang; Xin, Gui-Zhong

2017-10-25

Traditional Chinese medicine (TCM) materials with closely related species are frequently fungible in clinical use. Therefore, holistic comparison of the composition in bioactive compounds is essential to evaluate whether they are equivalent in efficacy. Taking three officinal species of Callicarpa as a case, we proposed and validated a standardized strategy for the discrimination of closely related TCM materials, which focused on the extraction, profiling and multivariate statistical analysis of their biochemome. Firstly, serial liquid-liquid extractions were utilized to prepare different batches of Callicarpa biochemome, and the preparation yields were utilized for the normalization of sampling quantity prior to UHPLC-IT-MS analysis. Secondly, 34 compounds, including 19 phenylethanoid glycosides, 10 flavonoids and 5 terpenoids, were identified based on an untargeted UHPLC-IT-MS method. Thirdly, method validation of linearity, precision and stability showed that the UHPLC-IT-MS system was qualified (R 2 >0.995, RSD<15%) for subsequent biochemome profiling. After PCA and PLS-DA analysis, 30 marker compounds were screened and demonstrated to be of good predictability using genetic algorithm optimized support vector machines. Finally, a heatmap visualization was employed for clarifying the distribution of marker compounds, which could be helpful to determine whether the three Callicarpa species are, in fact, equivalent substitutes. This study provides a standardized biochemome profiling strategy for systemic comparison analysis of closely related TCM materials, which shows promising perspectives in tracking the supply chain of pharmaceutical suppliers. Copyright © 2017 Elsevier B.V. All rights reserved.

Strategies for Reforming Workforce Preparation Programs in Europe

ERIC Educational Resources Information Center

Stenstrom, Marja-Leena; Lasonen, Johanna

2004-01-01

The Post-16 Strategies project coordinated by Dr. Johanna Lasonen from 1996 to 1998 was chiefly concerned with four post-16 education strategies: (1) "vocational enhancement"; (2) "mutual enrichment"; (3) "linkages;" and (4) "unification." These four strategies to promote parity of esteem between vocational…

Sampling and Homogenization Strategies Significantly Influence the Detection of Foodborne Pathogens in Meat.

PubMed

Rohde, Alexander; Hammerl, Jens Andre; Appel, Bernd; Dieckmann, Ralf; Al Dahouk, Sascha

2015-01-01

Efficient preparation of food samples, comprising sampling and homogenization, for microbiological testing is an essential, yet largely neglected, component of foodstuff control. Salmonella enterica spiked chicken breasts were used as a surface contamination model whereas salami and meat paste acted as models of inner-matrix contamination. A systematic comparison of different homogenization approaches, namely, stomaching, sonication, and milling by FastPrep-24 or SpeedMill, revealed that for surface contamination a broad range of sample pretreatment steps is applicable and loss of culturability due to the homogenization procedure is marginal. In contrast, for inner-matrix contamination long treatments up to 8 min are required and only FastPrep-24 as a large-volume milling device produced consistently good recovery rates. In addition, sampling of different regions of the spiked sausages showed that pathogens are not necessarily homogenously distributed throughout the entire matrix. Instead, in meat paste the core region contained considerably more pathogens compared to the rim, whereas in the salamis the distribution was more even with an increased concentration within the intermediate region of the sausages. Our results indicate that sampling and homogenization as integral parts of food microbiology and monitoring deserve more attention to further improve food safety.

Sampling and Homogenization Strategies Significantly Influence the Detection of Foodborne Pathogens in Meat

PubMed Central

Rohde, Alexander; Hammerl, Jens Andre; Appel, Bernd; Dieckmann, Ralf; Al Dahouk, Sascha

2015-01-01

Efficient preparation of food samples, comprising sampling and homogenization, for microbiological testing is an essential, yet largely neglected, component of foodstuff control. Salmonella enterica spiked chicken breasts were used as a surface contamination model whereas salami and meat paste acted as models of inner-matrix contamination. A systematic comparison of different homogenization approaches, namely, stomaching, sonication, and milling by FastPrep-24 or SpeedMill, revealed that for surface contamination a broad range of sample pretreatment steps is applicable and loss of culturability due to the homogenization procedure is marginal. In contrast, for inner-matrix contamination long treatments up to 8 min are required and only FastPrep-24 as a large-volume milling device produced consistently good recovery rates. In addition, sampling of different regions of the spiked sausages showed that pathogens are not necessarily homogenously distributed throughout the entire matrix. Instead, in meat paste the core region contained considerably more pathogens compared to the rim, whereas in the salamis the distribution was more even with an increased concentration within the intermediate region of the sausages. Our results indicate that sampling and homogenization as integral parts of food microbiology and monitoring deserve more attention to further improve food safety. PMID:26539462

Estimation of affinities of ligands in mixtures via magnetic recovery of target-ligand complexes and chromatographic analyses: chemometrics and an experimental model

PubMed Central

2011-01-01

Abstract Background The combinatorial library strategy of using multiple candidate ligands in mixtures as library members is ideal in terms of cost and efficiency, but needs special screening methods to estimate the affinities of candidate ligands in such mixtures. Herein, a new method to screen candidate ligands present in unknown molar quantities in mixtures was investigated. Results The proposed method involves preparing a processed-mixture-for-screening (PMFS) with each mixture sample and an exogenous reference ligand, initiating competitive binding among ligands from the PMFS to a target immobilized on magnetic particles, recovering target-ligand complexes in equilibrium by magnetic force, extracting and concentrating bound ligands, and analyzing ligands in the PMFS and the concentrated extract by chromatography. The relative affinity of each candidate ligand to its reference ligand is estimated via an approximation equation assuming (a) the candidate ligand and its reference ligand bind to the same site(s) on the target, (b) their chromatographic peak areas are over five times their intercepts of linear response but within their linear ranges, (c) their binding ratios are below 10%. These prerequisites are met by optimizing primarily the quantity of the target used and the PMFS composition ratio. The new method was tested using the competitive binding of biotin derivatives from mixtures to streptavidin immobilized on magnetic particles as a model. Each mixture sample containing a limited number of candidate biotin derivatives with moderate differences in their molar quantities were prepared via parallel-combinatorial-synthesis (PCS) without purification, or via the pooling of individual compounds. Some purified biotin derivatives were used as reference ligands. This method showed resistance to variations in chromatographic quantification sensitivity and concentration ratios; optimized conditions to validate the approximation equation could be applied to different mixture samples. Relative affinities of candidate biotin derivatives with unknown molar quantities in each mixture sample were consistent with those estimated by a homogenous method using their purified counterparts as samples. Conclusions This new method is robust and effective for each mixture possessing a limited number of candidate ligands whose molar quantities have moderate differences, and its integration with PCS has promise to routinely practice the mixture-based library strategy. PMID:21545719

Preparation of Chemical Samples On Relevant Surfaces Using Inkjet Technology

DTIC Science & Technology

2013-04-01

PREPARATION OF CHEMICAL SAMPLES ON RELEVANT SURFACES USING INKJET TECHNOLOGY...2012 4. TITLE AND SUBTITLE 5a. CONTRACT NUMBER Preparation of Chemical Samples on Relevant Surfaces Using Inkjet Technology 5b. GRANT NUMBER...SUBJECT TERMS Surface detection Inkjet Simulant deposition 16. SECURITY CLASSIFICATION OF: 17. LIMITATION OF ABSTRACT 18. NUMBER OF

Improved LC-MS/MS method for the quantification of hepcidin-25 in clinical samples.

PubMed

Abbas, Ioana M; Hoffmann, Holger; Montes-Bayón, María; Weller, Michael G

2018-06-01

Mass spectrometry-based methods play a crucial role in the quantification of the main iron metabolism regulator hepcidin by singling out the bioactive 25-residue peptide from the other naturally occurring N-truncated isoforms (hepcidin-20, -22, -24), which seem to be inactive in iron homeostasis. However, several difficulties arise in the MS analysis of hepcidin due to the "sticky" character of the peptide and the lack of suitable standards. Here, we propose the use of amino- and fluoro-silanized autosampler vials to reduce hepcidin interaction to laboratory glassware surfaces after testing several types of vials for the preparation of stock solutions and serum samples for isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS). Furthermore, we have investigated two sample preparation strategies and two chromatographic separation conditions with the aim of developing a LC-MS/MS method for the sensitive and reliable quantification of hepcidin-25 in serum samples. A chromatographic separation based on usual acidic mobile phases was compared with a novel approach involving the separation of hepcidin-25 with solvents at high pH containing 0.1% of ammonia. Both methods were applied to clinical samples in an intra-laboratory comparison of two LC-MS/MS methods using the same hepcidin-25 calibrators with good correlation of the results. Finally, we recommend a LC-MS/MS-based quantification method with a dynamic range of 0.5-40 μg/L for the assessment of hepcidin-25 in human serum that uses TFA-based mobile phases and silanized glass vials. Graphical abstract Structure of hepcidin-25 (Protein Data Bank, PDB ID 2KEF).

Humidity-controlled preparation of frozen-hydrated biological samples for cryogenic coherent x-ray diffraction microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Takayama, Yuki; Nakasako, Masayoshi; RIKEN Harima Institute/SPring-8, 1-1-1 Kouto, Mikaduki, Sayo, Hyogo 679-5148

2012-05-15

Coherent x-ray diffraction microscopy (CXDM) has the potential to visualize the structures of micro- to sub-micrometer-sized biological particles, such as cells and organelles, at high resolution. Toward advancing structural studies on the functional states of such particles, here, we developed a system for the preparation of frozen-hydrated biological samples for cryogenic CXDM experiments. The system, which comprised a moist air generator, microscope, micro-injector mounted on a micromanipulator, custom-made sample preparation chamber, and flash-cooling device, allowed for the manipulation of sample particles in the relative humidity range of 20%-94%rh at 293 K to maintain their hydrated and functional states. Here, wemore » report the details of the system and the operation procedure, including its application to the preparation of a frozen-hydrated chloroplast sample. Sample quality was evaluated through a cryogenic CXDM experiment conducted at BL29XUL of SPring-8. Taking the performance of the system and the quality of the sample, the system was suitable to prepare frozen-hydrated biological samples for cryogenic CXDM experiments.« less

Preparation of bone samples in the Gliwice Radiocarbon Laboratory for AMS radiocarbon dating.

PubMed

Piotrowska, N; Goslar, T

2002-12-01

In the Gliwice Radiocarbon Laboratory, a system for preparation of samples for AMS dating has been built. At first it was used to produce graphite targets from plant macrofossils and sediments. In this study we extended its capabilities with the preparation of bones. We dealt with 3 methods; the first was the classical Longin method of collagen extraction, the second one included additional treatment of powdered bone in alkali solution, while in the third one carboxyl carbon was separated from amino acids obtained after hydrolysis of protein. The suitability of the methods was tested on 2 bone samples. Most of our samples gave ages > 40 kyr BP, suggesting good performance of the adapted methods, except for one sample prepared with simple Longin method. For routine preparation of bones we chose the Longin method with additional alkali treatment.

Effect Of Neodymium Substitution In Structural Characteristics Of Magnesium Ferrite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thankachan, Smitha; Binu, P. J.; Xavier, Sheena

2011-10-20

The effect of Nd{sup 3+} substitution on the structural properties of Magnesium ferrite was studied in the series MgNd{sub x}Fe{sub 2-x}O{sub 4}, where x = 0 to 0.3 in steps of 0.05. The series was prepared by sol-gel technique which is one of the novel technique to prepare nanosized samples. Structural characterization was done using X-ray diffractometer and Fourier Transform Infrared Spectrometer. XRD analysis reveals the prepared samples are single phasic till x = 0.2. From x0 = .25, a secondary phase of iron neodymium oxide appears along with the spinel phase. Particle size calculation shows the prepared samples aremore » in the 9nm to 11 nm regime. Lattice parameter was found to increase with concentration of Nd. XRD and FTIR analysis confirmed spinel structure of the prepared samples. XRF result shows the expected composition of prepared samples. The frequency dependence of the dielectric constant in the range 100 Hz--120MHz was also studied« less

A novel strategy for pharmaceutical cocrystal generation without knowledge of stoichiometric ratio: myricetin cocrystals and a ternary phase diagram.

PubMed

Hong, Chao; Xie, Yan; Yao, Yashu; Li, Guowen; Yuan, Xiurong; Shen, Hongyi

2015-01-01

To develop a streamlined strategy for pharmaceutical cocrystal preparation without knowledge of the stoichiometric ratio by preparing and characterizing the cocrystals of myricetin (MYR) with four cocrystal coformers (CCF). An approach based on the phase solubility diagram (PSD) was used for MYR cocrystals preparation and the solid-state properties were characterized by differential scanning calorimetry (DSC), fourier transform-infrared spectroscopy (FT-IR), powder X-ray diffraction (PXRD), and scanning electron microscopy (SEM). The ternary phase diagram (TPD) was constructed by combining the PSD and nuclear magnetic resonance (NMR) data. After that, the TPD was verified by traditional methods. The dissolution of MYR in the four cocrystals and pure MYR within three different media were also evaluated. A simple research method for MYR cocrystal preparation was obtained as follows: first, the PSD of MYR and CCF was constructed and analyzed; second, by transforming the curve in the PSD to a TPD, a region of pure cocrystals formation was exhibited, and then MYR cocrystals were prepared and identified by DSC, FT-IR, PXRD, and SEM; third, with the composition of the prepared cocrystal from NMR, the TPD of the MYR-CCF-Solvent system was constructed. The powder dissolution data showed that the solubility and dissolution rate of MYR was significantly enhanced by the cocrystals. A novel strategy for pharmaceutical cocrystals preparation without knowledge of the stoichiometric ratio based on the TPD was established and MYR cocrystals were successfully prepared. The present study provides a systematic approach for pharmaceutical cocrystal generation, which benefits the development and application of cocrystal technology in drug delivery.

A 96-well screen filter plate for high-throughput biological sample preparation and LC-MS/MS analysis.

PubMed

Peng, Sean X; Cousineau, Martin; Juzwin, Stephen J; Ritchie, David M

2006-01-01

A novel 96-well screen filter plate (patent pending) has been invented to eliminate a time-consuming and labor-intensive step in preparation of in vivo study samples--to remove blood or plasma clots. These clots plug the pipet tips during a manual or automated sample-transfer step causing inaccurate pipetting or total pipetting failure. Traditionally, these blood and plasma clots are removed by picking them out manually one by one from each sample tube before any sample transfer can be made. This has significantly slowed the sample preparation process and has become a bottleneck for automated high-throughput sample preparation using robotic liquid handlers. Our novel screen filter plate was developed to solve this problem. The 96-well screen filter plate consists of 96 stainless steel wire-mesh screen tubes connected to the 96 openings of a top plate so that the screen filter plate can be readily inserted into a 96-well sample storage plate. Upon insertion, the blood and plasma clots are excluded from entering the screen tube while clear sample solutions flow freely into it. In this way, sample transfer can be easily completed by either manual or automated pipetting methods. In this report, three structurally diverse compounds were selected to evaluate and validate the use of the screen filter plate. The plasma samples of these compounds were transferred and processed in the presence and absence of the screen filter plate and then analyzed by LC-MS/MS methods. Our results showed a good agreement between the samples prepared with and without the screen filter plate, demonstrating the utility and efficiency of this novel device for preparation of blood and plasma samples. The device is simple, easy to use, and reusable. It can be employed for sample preparation of other biological fluids that contain floating particulates or aggregates.

Recent advances of mesoporous materials in sample preparation.

PubMed

Zhao, Liang; Qin, Hongqiang; Wu, Ren'an; Zou, Hanfa

2012-03-09

Sample preparation has been playing an important role in the analysis of complex samples. Mesoporous materials as the promising adsorbents have gained increasing research interest in sample preparation due to their desirable characteristics of high surface area, large pore volume, tunable mesoporous channels with well defined pore-size distribution, controllable wall composition, as well as modifiable surface properties. The aim of this paper is to review the recent advances of mesoporous materials in sample preparation with emphases on extraction of metal ions, adsorption of organic compounds, size selective enrichment of peptides/proteins, specific capture of post-translational peptides/proteins and enzymatic reactor for protein digestion. Copyright © 2011 Elsevier B.V. All rights reserved.

Sample types applied for molecular diagnosis of therapeutic management of advanced non-small cell lung cancer in the precision medicine.

PubMed

Han, Yanxi; Li, Jinming

2017-10-26

In this era of precision medicine, molecular biology is becoming increasingly significant for the diagnosis and therapeutic management of non-small cell lung cancer. The specimen as the primary element of the whole testing flow is particularly important for maintaining the accuracy of gene alteration testing. Presently, the main sample types applied in routine diagnosis are tissue and cytology biopsies. Liquid biopsies are considered as the most promising alternatives when tissue and cytology samples are not available. Each sample type possesses its own strengths and weaknesses, pertaining to the disparity of sampling, preparation and preservation procedures, the heterogeneity of inter- or intratumors, the tumor cellularity (percentage and number of tumor cells) of specimens, etc., and none of them can individually be a "one size to fit all". Therefore, in this review, we summarized the strengths and weaknesses of different sample types that are widely used in clinical practice, offered solutions to reduce the negative impact of the samples and proposed an optimized strategy for choice of samples during the entire diagnostic course. We hope to provide valuable information to laboratories for choosing optimal clinical specimens to achieve comprehensive functional genomic landscapes and formulate individually tailored treatment plans for NSCLC patients that are in advanced stages.

Nuclear Magnetic Resonance Spectroscopy-Based Identification of Yeast.

PubMed

Himmelreich, Uwe; Sorrell, Tania C; Daniel, Heide-Marie

2017-01-01

Rapid and robust high-throughput identification of environmental, industrial, or clinical yeast isolates is important whenever relatively large numbers of samples need to be processed in a cost-efficient way. Nuclear magnetic resonance (NMR) spectroscopy generates complex data based on metabolite profiles, chemical composition and possibly on medium consumption, which can not only be used for the assessment of metabolic pathways but also for accurate identification of yeast down to the subspecies level. Initial results on NMR based yeast identification where comparable with conventional and DNA-based identification. Potential advantages of NMR spectroscopy in mycological laboratories include not only accurate identification but also the potential of automated sample delivery, automated analysis using computer-based methods, rapid turnaround time, high throughput, and low running costs.We describe here the sample preparation, data acquisition and analysis for NMR-based yeast identification. In addition, a roadmap for the development of classification strategies is given that will result in the acquisition of a database and analysis algorithms for yeast identification in different environments.

Sample Preparation and Mounting of Drosophila Embryos for Multiview Light Sheet Microscopy.

PubMed

Schmied, Christopher; Tomancak, Pavel

2016-01-01

Light sheet fluorescent microscopy (LSFM), and in particular its most widespread flavor Selective Plane Illumination Microscopy (SPIM), promises to provide unprecedented insights into developmental dynamics of entire living systems. By combining minimal photo-damage with high imaging speed and sample mounting tailored toward the needs of the specimen, it enables in toto imaging of embryogenesis with high spatial and temporal resolution. Drosophila embryos are particularly well suited for SPIM imaging because the volume of the embryo does not change from the single cell embryo to the hatching larva. SPIM microscopes can therefore image Drosophila embryos embedded in rigid media, such as agarose, from multiple angles every few minutes from the blastoderm stage until hatching. Here, we describe sample mounting strategies to achieve such a recording. We also provide detailed protocols to realize multiview, long-term, time-lapse recording of Drosophila embryos expressing fluorescent markers on the commercially available Zeiss Lightsheet Z.1 microscope and the OpenSPIM.

Selective isolation of gonyautoxins 1,4 from the dinoflagellate Alexandrium minutum based on molecularly imprinted solid-phase extraction.

PubMed

Lian, Ziru; Wang, Jiangtao

2017-09-15

Gonyautoxins 1,4 (GTX1,4) from Alexandrium minutum samples were isolated selectively and recognized specifically by an innovative and effective extraction procedure based on molecular imprinting technology. Novel molecularly imprinted polymer microspheres (MIPMs) were prepared by double-templated imprinting strategy using caffeine and pentoxifylline as dummy templates. The synthesized polymers displayed good affinity to GTX1,4 and were applied as sorbents. Further, an off-line molecularly imprinted solid-phase extraction (MISPE) protocol was optimized and an effective approach based on the MISPE coupled with HPLC-FLD was developed for selective isolation of GTX1,4 from the cultured A. minutum samples. The separation method showed good extraction efficiency (73.2-81.5%) for GTX1,4 and efficient removal of interferences matrices was also achieved after the MISPE process for the microalgal samples. The outcome demonstrated the superiority and great potential of the MISPE procedure for direct separation of GTX1,4 from marine microalgal extracts. Copyright © 2017. Published by Elsevier Ltd.

Practicable group testing method to evaluate weight/weight GMO content in maize grains.

PubMed

Mano, Junichi; Yanaka, Yuka; Ikezu, Yoko; Onishi, Mari; Futo, Satoshi; Minegishi, Yasutaka; Ninomiya, Kenji; Yotsuyanagi, Yuichi; Spiegelhalter, Frank; Akiyama, Hiroshi; Teshima, Reiko; Hino, Akihiro; Naito, Shigehiro; Koiwa, Tomohiro; Takabatake, Reona; Furui, Satoshi; Kitta, Kazumi

2011-07-13

Because of the increasing use of maize hybrids with genetically modified (GM) stacked events, the established and commonly used bulk sample methods for PCR quantification of GM maize in non-GM maize are prone to overestimate the GM organism (GMO) content, compared to the actual weight/weight percentage of GM maize in the grain sample. As an alternative method, we designed and assessed a group testing strategy in which the GMO content is statistically evaluated based on qualitative analyses of multiple small pools, consisting of 20 maize kernels each. This approach enables the GMO content evaluation on a weight/weight basis, irrespective of the presence of stacked-event kernels. To enhance the method's user-friendliness in routine application, we devised an easy-to-use PCR-based qualitative analytical method comprising a sample preparation step in which 20 maize kernels are ground in a lysis buffer and a subsequent PCR assay in which the lysate is directly used as a DNA template. This method was validated in a multilaboratory collaborative trial.

40 CFR 761.323 - Sample preparation.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 761.323 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL... Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a minimum of 10 samples weighing at least 300 grams each. Samples of PCB remediation waste used in the...

40 CFR 761.323 - Sample preparation.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 761.323 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL... Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a minimum of 10 samples weighing at least 300 grams each. Samples of PCB remediation waste used in the...

40 CFR 761.323 - Sample preparation.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 761.323 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL... Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a minimum of 10 samples weighing at least 300 grams each. Samples of PCB remediation waste used in the...

14C sample preparation for AMS microdosing studies at Lund University using online combustion and septa-sealed vials

NASA Astrophysics Data System (ADS)

Sydoff, Marie; Stenström, Kristina

2010-04-01

The Department of Physics at Lund University is participating in a European Union project called EUMAPP (European Union Microdose AMS Partnership Programme), in which sample preparation and accelerator mass spectrometry (AMS) measurements of biological samples from microdosing studies have been made. This paper describes a simplified method of converting biological samples to solid graphite for 14C analysis with AMS. The method is based on online combustion of the samples, and reduction of CO 2 in septa-sealed vials. The septa-sealed vials and disposable materials are used to eliminate sample cross-contamination. Measurements of ANU and Ox I standards show deviations of 2% and 3%, respectively, relative to reference values. This level of accuracy is sufficient for biological samples from microdosing studies. Since the method has very few handling steps from sample to graphite, the risk of failure during the sample preparation process is minimized, making the method easy to use in routine preparation of samples.

BASS Experiment Imagery

NASA Image and Video Library

2013-04-09

ISS035-E-015952 (10 April 2013) --- This is one of a series of close-up images photographed during a run of the Burning and Suppression of Solids (BASS) experiment onboard the Earth-orbiting International Space Station. Following a series of preparations, on April 5 NASA astronaut Chris Cassidy (out of frame) conducted several runs of the experiment, which examines the burning and extinction characteristics of a wide variety of fuel samples in microgravity. The experiment is planned for guiding strategies for extinguishing fires in microgravity. BASS results contribute to the combustion computational models used in the design of fire detection and suppression systems in microgravity and on Earth.

Single-hole hollow molecularly imprinted polymer embedded carbon dot for fast detection of tetracycline in honey.

PubMed

Li, Huiyu; Zhao, Li; Xu, Yuan; Zhou, Tianyu; Liu, Haochi; Huang, Ning; Ding, Jie; Li, Yi; Ding, Lan

2018-08-01

It is difficult to detect tetracycline (TC) in honey sample by using carbon dots (CDs) because the autofluorescence of the matrix of honey sample overlaps with the fluorescence emission spectrum of the large majority of CDs. Herein, single-hole hollow molecularly imprinted polymers embedded carbon dots (HMIP@CD) was prepared via microwave-assisted method. TC in diluted honey sample was adsorbed by the HMIP@CD within 3 min, after which the HMIP@CD absorbed with TC was separated by centrifugation from honey sample and redispersed into phosphate buffer solution. The autofluorescence of honey that interferes with the fluorescence signal of HMIP@CD was avoided. The method exhibited an excellent linearity within 10-200 μg L -1 and a low detection limit of 3.1 μg L -1 . At three spiking levels of TC, the recoveries ranged from 93% to 105% with precisions below 1.6%. This method provides an effective strategy for detecting analyte in complex matrix with autofluorescence interference. Copyright © 2018. Published by Elsevier B.V.

46 CFR 164.009-15 - Test procedure.

Code of Federal Regulations, 2010 CFR

2010-10-01

... material, is less than 47 mm, the specimens prepared consist of layers of the sample. (3) If the sample is a composite material and has a height that is not 50 ±3mm, the layers of the specimen prepared are proportional in thickness to the layers of the sample. (4) The top and bottom faces of each specimen prepared...

9 CFR 147.8 - Procedures for preparing egg yolk samples for diagnostic tests.

Code of Federal Regulations, 2014 CFR

2014-01-01

... 9 Animals and Animal Products 1 2014-01-01 2014-01-01 false Procedures for preparing egg yolk samples for diagnostic tests. 147.8 Section 147.8 Animals and Animal Products ANIMAL AND PLANT HEALTH... IMPROVEMENT PLAN Blood Testing Procedures § 147.8 Procedures for preparing egg yolk samples for diagnostic...

9 CFR 147.8 - Procedures for preparing egg yolk samples for diagnostic tests.

Code of Federal Regulations, 2013 CFR

2013-01-01

... 9 Animals and Animal Products 1 2013-01-01 2013-01-01 false Procedures for preparing egg yolk samples for diagnostic tests. 147.8 Section 147.8 Animals and Animal Products ANIMAL AND PLANT HEALTH... IMPROVEMENT PLAN Blood Testing Procedures § 147.8 Procedures for preparing egg yolk samples for diagnostic...

9 CFR 147.8 - Procedures for preparing egg yolk samples for diagnostic tests.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 9 Animals and Animal Products 1 2012-01-01 2012-01-01 false Procedures for preparing egg yolk samples for diagnostic tests. 147.8 Section 147.8 Animals and Animal Products ANIMAL AND PLANT HEALTH... IMPROVEMENT PLAN Blood Testing Procedures § 147.8 Procedures for preparing egg yolk samples for diagnostic...

9 CFR 147.8 - Procedures for preparing egg yolk samples for diagnostic tests.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 9 Animals and Animal Products 1 2011-01-01 2011-01-01 false Procedures for preparing egg yolk samples for diagnostic tests. 147.8 Section 147.8 Animals and Animal Products ANIMAL AND PLANT HEALTH... IMPROVEMENT PLAN Blood Testing Procedures § 147.8 Procedures for preparing egg yolk samples for diagnostic...

Extending the spectrum of DNA sequences retrieved from ancient bones and teeth

PubMed Central

Glocke, Isabelle; Meyer, Matthias

2017-01-01

The number of DNA fragments surviving in ancient bones and teeth is known to decrease with fragment length. Recent genetic analyses of Middle Pleistocene remains have shown that the recovery of extremely short fragments can prove critical for successful retrieval of sequence information from particularly degraded ancient biological material. Current sample preparation techniques, however, are not optimized to recover DNA sequences from fragments shorter than ∼35 base pairs (bp). Here, we show that much shorter DNA fragments are present in ancient skeletal remains but lost during DNA extraction. We present a refined silica-based DNA extraction method that not only enables efficient recovery of molecules as short as 25 bp but also doubles the yield of sequences from longer fragments due to improved recovery of molecules with single-strand breaks. Furthermore, we present strategies for monitoring inefficiencies in library preparation that may result from co-extraction of inhibitory substances during DNA extraction. The combination of DNA extraction and library preparation techniques described here substantially increases the yield of DNA sequences from ancient remains and provides access to a yet unexploited source of highly degraded DNA fragments. Our work may thus open the door for genetic analyses on even older material. PMID:28408382

Chirality-Controlled Synthesis and Applications of Single-Wall Carbon Nanotubes.

PubMed

Liu, Bilu; Wu, Fanqi; Gui, Hui; Zheng, Ming; Zhou, Chongwu

2017-01-24

Preparation of chirality-defined single-wall carbon nanotubes (SWCNTs) is the top challenge in the nanotube field. In recent years, great progress has been made toward preparing single-chirality SWCNTs through both direct controlled synthesis and postsynthesis separation approaches. Accordingly, the uses of single-chirality-dominated SWCNTs for various applications have emerged as a new front in nanotube research. In this Review, we review recent progress made in the chirality-controlled synthesis of SWCNTs, including metal-catalyst-free SWCNT cloning by vapor-phase epitaxy elongation of purified single-chirality nanotube seeds, chirality-specific growth of SWCNTs on bimetallic solid alloy catalysts, chirality-controlled synthesis of SWCNTs using bottom-up synthetic strategy from carbonaceous molecular end-cap precursors, etc. Recent major progresses in postsynthesis separation of single-chirality SWCNT species, as well as methods for chirality characterization of SWCNTs, are also highlighted. Moreover, we discuss some examples where single-chirality SWCNTs have shown clear advantages over SWCNTs with broad chirality distributions. We hope this review could inspire more research on the chirality-controlled preparation of SWCNTs and equally important inspire the use of single-chirality SWCNT samples for more fundamental studies and practical applications.

Strategies for Reducing Public Speaking Anxiety in Japan.

ERIC Educational Resources Information Center

Kondo, David Shinji

1994-01-01

Develops a typology of strategies people use to cope with public speaking anxiety. Assesses the influences of anxiety level on strategy use. Finds 65 basic tactics in 6 strategy types (Relaxation, Preparation, Positive Thinking, Audience Depreciation, Concentration, and Resignation). Finds high anxious persons more likely to report Relaxation and…

La 2-xSr xCuO 4-δ superconducting samples prepared by the wet-chemical method

NASA Astrophysics Data System (ADS)

Loose, A.; Gonzalez, J. L.; Lopez, A.; Borges, H. A.; Baggio-Saitovitch, E.

2009-10-01

In this work, we report on the physical properties of good-quality polycrystalline superconducting samples of La 2-xSr xCu 1-yZn yO 4-δ ( y=0, 0.02) prepared by a wet-chemical method, focusing on the temperature dependence of the critical current. Using the wet-chemical method, we were able to produce samples with improved homogeneity compared to the solid-state method. A complete set of samples with several carrier concentrations, ranging from the underdoped (strontium concentration x≈0.05) to the highly overdoped ( x≈0.25) region, were prepared and investigated. The X-ray diffraction analysis, zero-field cooling magnetization and electrical resistivity measurements were reported on earlier. The structural parameters of the prepared samples seem to be slightly modified by the preparation method and their critical temperatures were lower than reported in the literature. The temperature dependence of the critical current was explained by a theoretical model which took the granular structure of the samples into account.

Automated SEM and TEM sample preparation applied to copper/low k materials

NASA Astrophysics Data System (ADS)

Reyes, R.; Shaapur, F.; Griffiths, D.; Diebold, A. C.; Foran, B.; Raz, E.

2001-01-01

We describe the use of automated microcleaving for preparation of both SEM and TEM samples as done by SELA's new MC500 and TEMstation tools. The MC500 is an automated microcleaving tool that is capable of producing cleaves with 0.25 μm accuracy resulting in SEM-ready samples. The TEMstation is capable of taking a sample output from the MC500 (or from SELA's earlier MC200 tool) and producing a FIB ready slice of 25±5 μm, mounted on a TEM-washer and ready for FIB thinning to electron transparency for TEM analysis. The materials selected for the tool set evaluation mainly included the Cu/TaN/HOSP low-k system. The paper is divided into three sections, experimental approach, SEM preparation and analysis of HOSP low-k, and TEM preparation and analysis of Cu/TaN/HOSP low-k samples. For the samples discussed, data is presented to show the quality of preparation provided by these new automated tools.

The minimum information required for a glycomics experiment (MIRAGE) project: sample preparation guidelines for reliable reporting of glycomics datasets.

PubMed

Struwe, Weston B; Agravat, Sanjay; Aoki-Kinoshita, Kiyoko F; Campbell, Matthew P; Costello, Catherine E; Dell, Anne; Ten Feizi; Haslam, Stuart M; Karlsson, Niclas G; Khoo, Kay-Hooi; Kolarich, Daniel; Liu, Yan; McBride, Ryan; Novotny, Milos V; Packer, Nicolle H; Paulson, James C; Rapp, Erdmann; Ranzinger, Rene; Rudd, Pauline M; Smith, David F; Tiemeyer, Michael; Wells, Lance; York, William S; Zaia, Joseph; Kettner, Carsten

2016-09-01

The minimum information required for a glycomics experiment (MIRAGE) project was established in 2011 to provide guidelines to aid in data reporting from all types of experiments in glycomics research including mass spectrometry (MS), liquid chromatography, glycan arrays, data handling and sample preparation. MIRAGE is a concerted effort of the wider glycomics community that considers the adaptation of reporting guidelines as an important step towards critical evaluation and dissemination of datasets as well as broadening of experimental techniques worldwide. The MIRAGE Commission published reporting guidelines for MS data and here we outline guidelines for sample preparation. The sample preparation guidelines include all aspects of sample generation, purification and modification from biological and/or synthetic carbohydrate material. The application of MIRAGE sample preparation guidelines will lead to improved recording of experimental protocols and reporting of understandable and reproducible glycomics datasets. © The Author 2016. Published by Oxford University Press. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

[Recent advances in sample preparation methods of plant hormones].

PubMed

Wu, Qian; Wang, Lus; Wu, Dapeng; Duan, Chunfeng; Guan, Yafeng

2014-04-01

Plant hormones are a group of naturally occurring trace substances which play a crucial role in controlling the plant development, growth and environment response. With the development of the chromatography and mass spectroscopy technique, chromatographic analytical method has become a widely used way for plant hormone analysis. Among the steps of chromatographic analysis, sample preparation is undoubtedly the most vital one. Thus, a highly selective and efficient sample preparation method is critical for accurate identification and quantification of phytohormones. For the three major kinds of plant hormones including acidic plant hormones & basic plant hormones, brassinosteroids and plant polypeptides, the sample preparation methods are reviewed in sequence especially the recently developed methods. The review includes novel methods, devices, extractive materials and derivative reagents for sample preparation of phytohormones analysis. Especially, some related works of our group are included. At last, the future developments in this field are also prospected.

Transportation energy strategy: Project {number_sign}5 of the Hawaii Energy Strategy Development Program

DOE Office of Scientific and Technical Information (OSTI.GOV)

NONE

1995-08-01

This study was prepared for the State Department of Business, Economic Development and Tourism (DBEDT) as part of the Hawaii Energy Strategy program. Authority and responsibility for energy planning activities, such as the Hawaii Energy Strategy, rests with the State Energy Resources Coordinator, who is the Director of DBEDT. Hawaii Energy Strategy Study No. 5, Transportation Energy Strategy Development, was prepared to: collect and synthesize information on the present and future use of energy in Hawaii`s transportation sector, examine the potential of energy conservation to affect future energy demand; analyze the possibility of satisfying a portion of the state`s futuremore » transportation energy demand through alternative fuels; and recommend a program targeting energy use in the state`s transportation sector to help achieve state goals. The analyses and conclusions of this report should be assessed in relation to the other Hawaii Energy Strategy Studies in developing a comprehensive state energy program. 56 figs., 87 tabs.« less

Inverse supercritical fluid extraction as a sample preparation method for the analysis of the nanoparticle content in sunscreen agents.

PubMed

Müller, David; Cattaneo, Stefano; Meier, Florian; Welz, Roland; de Vries, Tjerk; Portugal-Cohen, Meital; Antonio, Diana C; Cascio, Claudia; Calzolai, Luigi; Gilliland, Douglas; de Mello, Andrew

2016-04-01

We demonstrate the use of inverse supercritical carbon dioxide (scCO2) extraction as a novel method of sample preparation for the analysis of complex nanoparticle-containing samples, in our case a model sunscreen agent with titanium dioxide nanoparticles. The sample was prepared for analysis in a simplified process using a lab scale supercritical fluid extraction system. The residual material was easily dispersed in an aqueous solution and analyzed by Asymmetrical Flow Field-Flow Fractionation (AF4) hyphenated with UV- and Multi-Angle Light Scattering detection. The obtained results allowed an unambiguous determination of the presence of nanoparticles within the sample, with almost no background from the matrix itself, and showed that the size distribution of the nanoparticles is essentially maintained. These results are especially relevant in view of recently introduced regulatory requirements concerning the labeling of nanoparticle-containing products. The novel sample preparation method is potentially applicable to commercial sunscreens or other emulsion-based cosmetic products and has important ecological advantages over currently used sample preparation techniques involving organic solvents. Copyright © 2016 Elsevier B.V. All rights reserved.

Sample preparation techniques for the determination of trace residues and contaminants in foods.

PubMed

Ridgway, Kathy; Lalljie, Sam P D; Smith, Roger M

2007-06-15

The determination of trace residues and contaminants in complex matrices, such as food, often requires extensive sample extraction and preparation prior to instrumental analysis. Sample preparation is often the bottleneck in analysis and there is a need to minimise the number of steps to reduce both time and sources of error. There is also a move towards more environmentally friendly techniques, which use less solvent and smaller sample sizes. Smaller sample size becomes important when dealing with real life problems, such as consumer complaints and alleged chemical contamination. Optimal sample preparation can reduce analysis time, sources of error, enhance sensitivity and enable unequivocal identification, confirmation and quantification. This review considers all aspects of sample preparation, covering general extraction techniques, such as Soxhlet and pressurised liquid extraction, microextraction techniques such as liquid phase microextraction (LPME) and more selective techniques, such as solid phase extraction (SPE), solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). The applicability of each technique in food analysis, particularly for the determination of trace organic contaminants in foods is discussed.

40 CFR 51.116 - Data availability.

Code of Federal Regulations, 2011 CFR

2011-07-01

... FOR PREPARATION, ADOPTION, AND SUBMITTAL OF IMPLEMENTATION PLANS Control Strategy § 51.116 Data availability. (a) The State must retain all detailed data and calculations used in the preparation of each plan... Administrator at his request. (b) The detailed data and calculations used in the preparation of plan revisions...

40 CFR 51.116 - Data availability.

Code of Federal Regulations, 2010 CFR

2010-07-01

... FOR PREPARATION, ADOPTION, AND SUBMITTAL OF IMPLEMENTATION PLANS Control Strategy § 51.116 Data availability. (a) The State must retain all detailed data and calculations used in the preparation of each plan... Administrator at his request. (b) The detailed data and calculations used in the preparation of plan revisions...

Sample Preparation Techniques for Grain Boundary Characterization of Annealed TRISO-Coated Particles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dunzik-Gougar, M. L.; van Rooyen, I. J.; Hill, C. M.

Crystallographic information about chemical vapor deposition layers of silicon carbide (SiC) is essential to understanding layer performance, especially when the layers are in non planar geometries, such as spherical. We performed electron Back Scatter Diffraction (EBSD) analysis of spherical SiC layers using a different approach to sample focus ion beam milling technique to avoid the negative impacts of traditional sample polishing and to address the need of very small samples of irradiated materials for analysis. Mechanical and chemical grinding and polishing of sample surfaces can introduce lattice strains and result in unequal removal of SiC and surrounding layers of differentmore » material due to the hardness differences of these materials. The nature of layer interfaces is thought to play a key role in performance of the SiC; therefore, analysis of representative samples at these interfacial areas is crucial. In work reported here, a focused ion beam (FIB) was employed in a novel manner to prepare a more representative sample for EBSD analysis from TRISO layers free of effects introduced by mechanical and chemical preparation methods. In addition, the difficulty of handling neutron irradiated microscopic samples such as those analyzed in this work has been simplified with pre tilted mounting stages. Our study showed that although the average grain size of samples may be similar, the grain boundary characteristics may differ significantly. It was also found that low angle grain boundaries, comprises 25% in the FIB-prepared sample vs only 1-2% in the polished sample measured in the same particle. From this study it was determined that results of FIB prepared sample will provide more repeatable results, as the role of sample preparation is eliminated.« less

Sample Preparation Techniques for Grain Boundary Characterization of Annealed TRISO-Coated Particles

DOE PAGES

Dunzik-Gougar, M. L.; van Rooyen, I. J.; Hill, C. M.; ...

2016-08-25

Crystallographic information about chemical vapor deposition layers of silicon carbide (SiC) is essential to understanding layer performance, especially when the layers are in non planar geometries, such as spherical. We performed electron Back Scatter Diffraction (EBSD) analysis of spherical SiC layers using a different approach to sample focus ion beam milling technique to avoid the negative impacts of traditional sample polishing and to address the need of very small samples of irradiated materials for analysis. Mechanical and chemical grinding and polishing of sample surfaces can introduce lattice strains and result in unequal removal of SiC and surrounding layers of differentmore » material due to the hardness differences of these materials. The nature of layer interfaces is thought to play a key role in performance of the SiC; therefore, analysis of representative samples at these interfacial areas is crucial. In work reported here, a focused ion beam (FIB) was employed in a novel manner to prepare a more representative sample for EBSD analysis from TRISO layers free of effects introduced by mechanical and chemical preparation methods. In addition, the difficulty of handling neutron irradiated microscopic samples such as those analyzed in this work has been simplified with pre tilted mounting stages. Our study showed that although the average grain size of samples may be similar, the grain boundary characteristics may differ significantly. It was also found that low angle grain boundaries, comprises 25% in the FIB-prepared sample vs only 1-2% in the polished sample measured in the same particle. From this study it was determined that results of FIB prepared sample will provide more repeatable results, as the role of sample preparation is eliminated.« less

Advantages and Disadvantages of using a Focused Ion Beam to Prepare TEM Samples From Irradiated U-10Mo Monolithic Nuclear Fuel

DOE Office of Scientific and Technical Information (OSTI.GOV)

B. D. Miller; J. Gan; J. Madden

2012-05-01

Transmission electron microscopy (TEM), scanning electron microscopy (SEM), and focused ion beam (FIB) milling were performed on an irradiated U-10Mo monolithic fuel to understand its irradiation microstructure. This is the first reported TEM work of irradiated fuel sample prepared using a FIB. Advantages and disadvantages of using the FIB to create TEM samples from this irradiated fuel will be presented along with some results from the work. Sample preparation techniques used to create SEM and FIB samples from the brittle irradiated monolithic sample will also be discussed.

Synthetic Strategies in the Preparation of Polymer/Inorganic Hybrid Nanoparticles

PubMed Central

Hood, Matthew A.; Mari, Margherita; Muñoz-Espí, Rafael

2014-01-01

This article reviews the recent advances and challenges in the preparation of polymer/inorganic hybrid nanoparticles. We mainly focus on synthetic strategies, basing our classification on whether the inorganic and the polymer components have been formed in situ or ex situ, of the hybrid material. Accordingly, four types of strategies are identified and described, referring to recent examples: (i) ex situ formation of the components and subsequent attachment or integration, either by covalent or noncovalent bonding; (ii) in situ polymerization in the presence of ex situ formed inorganic nanoparticles; (iii) in situ precipitation of the inorganic components on or in polymer structures; and (iv) strategies in which both polymer and inorganic component are simultaneously formed in situ. PMID:28788665

Should We Extend Teacher Preparation?

ERIC Educational Resources Information Center

Hawley, Willis D.

1989-01-01

Discusses the implications of five-year teacher preparation programs. Argues that different strategies and curricula should be tested and evaluated before mandating major system-wide changes in teacher certification requirements. (FMW)

40 CFR 761.323 - Sample preparation.

Code of Federal Regulations, 2010 CFR

2010-07-01

... Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a minimum of 10 samples weighing at least 300 grams each. Samples of PCB remediation waste used in the... PCB remediation waste at the cleanup site, or must be the same kind of material as that waste. For...

Racial Differences in Test Preparation Strategies: A Commentary on "Shadow Education, American Style: Test Preparation, the SAT and College Enrollment"

ERIC Educational Resources Information Center

Alon, Sigal

2010-01-01

Claudia Buchmann, Dennis Condron and Vincent Roscigno's study, titled "Shadow Education, American Style: Test Preparation, the SAT and College Enrollment," demonstrates that vigorous use of expensive test preparation tools, such as private classes and tutors, significantly boosts scores on standardized exams such as the SAT or ACT. This…

Sustainable synthesis of metals-doped ZnO nanoparticles from zinc-bearing dust for photodegradation of phenol.

PubMed

Wu, Zhao-Jin; Huang, Wei; Cui, Ke-Ke; Gao, Zhi-Fang; Wang, Ping

2014-08-15

A novel strategy of waste-cleaning-waste is proposed in the present work. A metals-doped ZnO (M-ZnO, M = Fe, Mg, Ca and Al) nanomaterial has been prepared from a metallurgical zinc-containing solid waste "fabric filter dust" by combining sulfolysis and co-precipitation processes, and is found to be a favorable photocatalyst for photodegradation of organic substances in wastewater under visible light irradiation. All the zinc and dopants (Fe, Mg, Ca and Al) for preparing M-ZnO are recovered from the fabric filter dust, without any addition of chemical as elemental source. The dust-derived M-ZnO samples deliver single phase indexed as the hexagonal ZnO crystal, with controllable dopants species. The photocatalytic activity of the dust-derived M-ZnO samples is characterized by photodegradation of phenol aqueous solution under visible light irradiation, giving more prominent photocatalytic behaviors than undoped ZnO. Such enhancements may be attributed to incorporation of the dust-derived metal elements (Fe, Mg, Ca and Al) into ZnO structure, which lead to the modification of band gap and refinement of grain size. The results show a feasibility to utilize the industrial waste as a resource of photodegradating organic substances in wastewater treatments. Copyright © 2014 Elsevier B.V. All rights reserved.

Rapid detection of potyviruses from crude plant extracts.

PubMed

Silva, Gonçalo; Oyekanmi, Joshua; Nkere, Chukwuemeka K; Bömer, Moritz; Kumar, P Lava; Seal, Susan E

2018-04-01

Potyviruses (genus Potyvirus; family Potyviridae) are widely distributed and represent one of the most economically important genera of plant viruses. Therefore, their accurate detection is a key factor in developing efficient control strategies. However, this can sometimes be problematic particularly in plant species containing high amounts of polysaccharides and polyphenols such as yam (Dioscorea spp.). Here, we report the development of a reliable, rapid and cost-effective detection method for the two most important potyviruses infecting yam based on reverse transcription-recombinase polymerase amplification (RT-RPA). The developed method, named 'Direct RT-RPA', detects each target virus directly from plant leaf extracts prepared with a simple and inexpensive extraction method avoiding laborious extraction of high-quality RNA. Direct RT-RPA enables the detection of virus-positive samples in under 30 min at a single low operation temperature (37 °C) without the need for any expensive instrumentation. The Direct RT-RPA tests constitute robust, accurate, sensitive and quick methods for detection of potyviruses from recalcitrant plant species. The minimal sample preparation requirements and the possibility of storing RPA reagents without cold chain storage, allow Direct RT-RPA to be adopted in minimally equipped laboratories and with potential use in plant clinic laboratories and seed certification facilities worldwide. Copyright © 2018 The Authors. Published by Elsevier Inc. All rights reserved.

Soil sampling strategies: evaluation of different approaches.

PubMed

de Zorzi, Paolo; Barbizzi, Sabrina; Belli, Maria; Mufato, Renzo; Sartori, Giuseppe; Stocchero, Giulia

2008-11-01

The National Environmental Protection Agency of Italy (APAT) performed a soil sampling intercomparison, inviting 14 regional agencies to test their own soil sampling strategies. The intercomparison was carried out at a reference site, previously characterised for metal mass fraction distribution. A wide range of sampling strategies, in terms of sampling patterns, type and number of samples collected, were used to assess the mean mass fraction values of some selected elements. The different strategies led in general to acceptable bias values (D) less than 2sigma, calculated according to ISO 13258. Sampling on arable land was relatively easy, with comparable results between different sampling strategies.

Modular microfluidic system for biological sample preparation

DOEpatents

Rose, Klint A.; Mariella, Jr., Raymond P.; Bailey, Christopher G.; Ness, Kevin Dean

2015-09-29

A reconfigurable modular microfluidic system for preparation of a biological sample including a series of reconfigurable modules for automated sample preparation adapted to selectively include a) a microfluidic acoustic focusing filter module, b) a dielectrophoresis bacteria filter module, c) a dielectrophoresis virus filter module, d) an isotachophoresis nucleic acid filter module, e) a lyses module, and f) an isotachophoresis-based nucleic acid filter.

Critical evaluation of sample pretreatment techniques.

PubMed

Hyötyläinen, Tuulia

2009-06-01

Sample preparation before chromatographic separation is the most time-consuming and error-prone part of the analytical procedure. Therefore, selecting and optimizing an appropriate sample preparation scheme is a key factor in the final success of the analysis, and the judicious choice of an appropriate procedure greatly influences the reliability and accuracy of a given analysis. The main objective of this review is to critically evaluate the applicability, disadvantages, and advantages of various sample preparation techniques. Particular emphasis is placed on extraction techniques suitable for both liquid and solid samples.

[Economic impact of strategies using ephedrine prefilled syringes].

PubMed

Crégut-Corbaton, J; Malbranche, C; Guignard, M-H; Fagnoni, P

2013-11-01

Ephedrine is an emergency drug available in ampules and syringes need to be prepared in advance according to one of two strategies in our establishment: strategy 1 (S1: 1 ampule per patient) and strategy 2 (S2: 1 ampule per operating room). There are also prefilled syringes. Because of their high cost and conflicting results in the literature, we assessed the economic interest of using prefilled syringes compared with strategies S1 and S2. This was a prospective observational study. The consumption of ephedrine was recorded over two periods of 14 days: P1 with syringes prepared in advance according to S1 or S2 and P2 with the on-demand use of prefilled syringes. The cost of a syringe of ephedrine prepared in advance (nurse time preparation included) was evaluated at €1.65 vs. €3.57 for a prefilled syringe. In operating rooms using S1, the use of prefilled syringes reduced overall the cost per patient about €1.22 and global annual costs by 72% (€2830), while the decrease was about €0.32 for the cost per patient and about 47% (€2760) for global annual costs for operating rooms using S2. The interest of our study is that we investigated different supply strategies for ephedrine within a large number of operating rooms. In our establishment, it was decided to use prefilled syringes in operating rooms that used S1. As well as the economic interest, prefilled syringes contributed to improved safety and saved nursing time. Copyright © 2013 Société française d’anesthésie et de réanimation (Sfar). Published by Elsevier SAS. All rights reserved.

Preparation of protein samples for mass spectrometry and N-terminal sequencing.

PubMed

Glenn, Gary

2014-01-01

The preparation of protein samples for mass spectrometry and N-terminal sequencing is a key step in successfully identifying proteins. Mass spectrometry is a very sensitive technique, and as such, samples must be prepared carefully since they can be subject to contamination of the sample (e.g., due to incomplete subcellular fractionation or purification of a multiprotein complex), overwhelming of the sample by highly abundant proteins, and contamination from skin or hair (keratin can be a very common hit). One goal of sample preparation for mass spec is to reduce the complexity of the sample - in the example presented here, mitochondria are purified, solubilized, and fractionated by sucrose density gradient sedimentation prior to preparative 1D SDS-PAGE. It is important to verify the purity and integrity of the sample so that you can have confidence in the hits obtained. More protein is needed for N-terminal sequencing and ideally it should be purified to a single band when run on an SDS-polyacrylamide gel. The example presented here involves stably expressing a tagged protein in HEK293 cells and then isolating the protein by affinity purification and SDS-PAGE. © 2014 Elsevier Inc. All rights reserved.

Tangible resources for preparing patients for antiviral therapy for chronic hepatitis C.

PubMed

Bonner, Jason E; Barritt, A Sidney; Fried, Michael W; Evon, Donna M

2012-06-01

Chronic hepatitis C (HCV) infected patients with coexisting mental health and/or substance abuse issues face significant barriers to treatment and are often deferred. This paper sought to highlight critical pre-treatment strategies and provide tangible resources for HCV clinicians to facilitate preparation and successful treatment of these patients. Guided by the clinical experience of our liver center, a large, tertiary academic medical center, and informed by the extant literature, we summarize pre-treatment strategies and specific resources and recommendations for HCV providers. Four key pre-treatment strategies include: 1) screening for mental health/substance abuse issues using brief, reliable and validated instruments; 2) locating and establishing collaborative care with mental health and substance abuse specialists; 3) using a motivational interviewing communication style; and 4) addressing adherence-related issues. HCV clinicians are in a unique position to prepare patients with coexisting mental health and/or substance abuse issues for antiviral therapy.

Preparation and characterizations of activated carbon monolith from rubber wood and its effect on supercapacitor performances

NASA Astrophysics Data System (ADS)

Taer, E.; Taslim, R.; Deraman, M.

2016-02-01

Preparation of activated carbon monolith (ACM) from rubber wood was investigated. Two kind of preparation method were carried out by pre-carbonized of rubber wood saw dust and rubber wood material as it is naturally. The samples were prepared with pelletizing method and small cutting of rubber wood in cross sectional method. Both of samples were characterized by physical and electrochemical technique. The physical properties such as morphology and porosity were investigated. The electrochemical properties of both samples such as equivalent series resistances (ESR) and specific capacitances were also compared. In conclusion, this study showed that both of different preparation method would propose a simple method of ACM electrode preparation technique for supercapacitor applications.

The preparation of high quality alumina defective photonic crystals and their application of photoluminescence enhancement

NASA Astrophysics Data System (ADS)

An, Yu-Ying; Wang, Jian; Zhou, Wen-Ming; Jin, Hong-Xia; Li, Jian-Feng; Wang, Cheng-Wei

2018-07-01

The high quality anodic aluminum oxide (AAO) defective photonic crystals (DPCs) have been successfully prepared by using a modified periodic pulse anodization technique including an effective voltage compensating strategy. The test results confirmed that the AAO DPCs were with a perfect regular layered-structure and had a narrow defective photonic band gap (DPBG) with a high quality defective mode. When the rhodamine B (rhB) was absorbed onto the pore walls of the AAO DPCs, it was found that the DPBG blue edge and localized defective mode inside could significantly enhance the photoluminescence (PL) intensity of rhodamine B (rhB), while they were carefully regulated to match with the emission peak position of rhB respectively. Even more intriguing was that the localized defective peak in DPBG had more notable effect on rhB's photoluminescence, 3.1 times higher than that of the control samples under the same conditions. The corresponding mechanism for photoluminescence enhancement was also discussed in detail.

Peptide-membrane Interactions by Spin-labeling EPR

PubMed Central

Smirnova, Tatyana I.; Smirnov, Alex I.

2016-01-01

Site-directed spin labeling (SDSL) in combination with Electron Paramagnetic Resonance (EPR) spectroscopy is a well-established method that has recently grown in popularity as an experimental technique, with multiple applications in protein and peptide science. The growth is driven by development of labeling strategies, as well as by considerable technical advances in the field, that are paralleled by an increased availability of EPR instrumentation. While the method requires an introduction of a paramagnetic probe at a well-defined position in a peptide sequence, it has been shown to be minimally destructive to the peptide structure and energetics of the peptide-membrane interactions. In this chapter, we describe basic approaches for using SDSL EPR spectroscopy to study interactions between small peptides and biological membranes or membrane mimetic systems. We focus on experimental approaches to quantify peptide-membrane binding, topology of bound peptides, and characterize peptide aggregation. Sample preparation protocols including spin-labeling methods and preparation of membrane mimetic systems are also described. PMID:26477253

A high-throughput robotic sample preparation system and HPLC-MS/MS for measuring urinary anatabine, anabasine, nicotine and major nicotine metabolites.

PubMed

Wei, Binnian; Feng, June; Rehmani, Imran J; Miller, Sharyn; McGuffey, James E; Blount, Benjamin C; Wang, Lanqing

2014-09-25

Most sample preparation methods characteristically involve intensive and repetitive labor, which is inefficient when preparing large numbers of samples from population-scale studies. This study presents a robotic system designed to meet the sampling requirements for large population-scale studies. Using this robotic system, we developed and validated a method to simultaneously measure urinary anatabine, anabasine, nicotine and seven major nicotine metabolites: 4-Hydroxy-4-(3-pyridyl)butanoic acid, cotinine-N-oxide, nicotine-N-oxide, trans-3'-hydroxycotinine, norcotinine, cotinine and nornicotine. We analyzed robotically prepared samples using high-performance liquid chromatography (HPLC) coupled with triple quadrupole mass spectrometry in positive electrospray ionization mode using scheduled multiple reaction monitoring (sMRM) with a total runtime of 8.5 min. The optimized procedure was able to deliver linear analyte responses over a broad range of concentrations. Responses of urine-based calibrators delivered coefficients of determination (R(2)) of >0.995. Sample preparation recovery was generally higher than 80%. The robotic system was able to prepare four 96-well plate (384 urine samples) per day, and the overall method afforded an accuracy range of 92-115%, and an imprecision of <15.0% on average. The validation results demonstrate that the method is accurate, precise, sensitive, robust, and most significantly labor-saving for sample preparation, making it efficient and practical for routine measurements in large population-scale studies such as the National Health and Nutrition Examination Survey (NHANES) and the Population Assessment of Tobacco and Health (PATH) study. Published by Elsevier B.V.

College Preparation for Students with Learning Disabilities: A Curriculum Approach.

ERIC Educational Resources Information Center

Whinnery, Keith W.

1992-01-01

A college preparation curriculum relevant to the needs of students with learning disabilities is presented, focusing on early planning, instructional modifications, strategy instruction, and support services. (JDD)

Pt NPs and DNAzyme functionalized polymer nanospheres as triple signal amplification strategy for highly sensitive electrochemical immunosensor of tumour marker.

PubMed

Chang, Honghong; Zhang, Haochun; Lv, Jia; Zhang, Bing; Wei, Wenlong; Guo, Jingang

2016-12-15

Highly sensitive determination of tumour markers is the key for early diagnosis of cancer. Herein, triple signal amplification strategy resulting from polymer nanospheres, Pt NPs, and DNAzyme was proposed in the developed electrochemical immunosensor. First, electroactive polymer nanospheres were synthesized by infinite coordination polymerization of ferrocenedicarboxylic acid, which could generate strong electrochemical signals due to plentiful ferrocene molecules. Further, the polymer nanospheres were functionalized by Pt NPs and DNAzyme (hemin/G-quadruplex) with the ability of catalyzing H2O2, which contributes to enhance the electrochemical signals. The prepared conjugations were characterized by transmission electron microscope (TEM) and energy dispersive X-ray spectroscopy (EDX). And the process of preparation was monitored by zeta potential. Based on the sandwich-type immunoassay, the electrochemical immunosensor was constructed employing the conjugations as signal tags. Under optimal conditions, the DPV peak increased with the increasing of alpha fetal protein (AFP) concentration, and the linear range was from 0.1pgmL(-1) to 100ngmL(-1) with low detection limit of 0.086pgmL(-1). Meanwhile, the designed immunosensor exhibited excellent selectivity and anti-interference property, good reproducibility and stability. More importantly, there were no significant differences in analyzing real clinical samples between designed immunosensor and commercial ELISA. Copyright © 2016 Elsevier B.V. All rights reserved.

Studies of tin-transition metal-carbon and tin-cobalt-transition metal-carbon negative electrode materials prepared by mechanical attrition

NASA Astrophysics Data System (ADS)

Ferguson, P. P.; Martine, M. L.; George, A. E.; Dahn, J. R.

Samples of Sn 30TM 30C 40 and of Sn 30Co 15TM 15C 40, with TM = 3d transition metals, were prepared by vertical-axis attritor milling. The structure and performance of these samples were studied by X-ray diffraction (XRD) and by electrochemical testing. The XRD patterns of Sn 30TM 30C 40 show an amorphous-like diffraction pattern only for the sample with TM = Co. The other prepared samples show broadened Bragg peaks of their main starting material, along with an amorphous-like background, even after 32 h of milling. Samples with TM = Co and TM = Ni show stable differential capacity versus potential plots and stable cycling for at least 100 cycles with reversible capacities of 425 and 250 mAh g -1, respectively. All samples prepared with 15 at.% Co show good capacity retention for at least 100 cycles ranging from 270 mAh g -1 for samples with TM = Ni to 500 mAh g -1 for samples with TM = Ti. The differential capacity versus potential plots for all the prepared Sn 30Co 15TM 15C 40 samples show similar structure to that of Sn 30Co 30C 40 except when TM = Cu. This shows the possibility of preparing tin-based negative electrode materials using a combination of cobalt and TM, especially if one looks to reduce the cobalt content.

Non-Contact Conductivity Measurement for Automated Sample Processing Systems

NASA Technical Reports Server (NTRS)

Beegle, Luther W.; Kirby, James P.

2012-01-01

A new method has been developed for monitoring and control of automated sample processing and preparation especially focusing on desalting of samples before analytical analysis (described in more detail in Automated Desalting Apparatus, (NPO-45428), NASA Tech Briefs, Vol. 34, No. 8 (August 2010), page 44). The use of non-contact conductivity probes, one at the inlet and one at the outlet of the solid phase sample preparation media, allows monitoring of the process, and acts as a trigger for the start of the next step in the sequence (see figure). At each step of the muti-step process, the system is flushed with low-conductivity water, which sets the system back to an overall low-conductivity state. This measurement then triggers the next stage of sample processing protocols, and greatly minimizes use of consumables. In the case of amino acid sample preparation for desalting, the conductivity measurement will define three key conditions for the sample preparation process. First, when the system is neutralized (low conductivity, by washing with excess de-ionized water); second, when the system is acidified, by washing with a strong acid (high conductivity); and third, when the system is at a basic condition of high pH (high conductivity). Taken together, this non-contact conductivity measurement for monitoring sample preparation will not only facilitate automation of the sample preparation and processing, but will also act as a way to optimize the operational time and use of consumables

Enhancing the Knowledge Base in Educational Administration. UCEA Monograph Series.

ERIC Educational Resources Information Center

Wendel, Frederick C., Ed.

Effective administrator preparation programs and professional practices are important to enhancing principals' knowledge base. In chapter 1 of this report, "Strategies of Organizing Principal Preparation: A Survey of the Danforth Principal Preparation Program," Gerald C. Ubben and Frances C. Fowler discuss their survey of facilitators of the…

Student-Prepared Games as a Teaching Strategy

ERIC Educational Resources Information Center

Brisk, William J.

1974-01-01

A course on game preparation attended by students from different disciplines involved an exposure to various types of games, leading up to individual and group development of games. Two of the games developed, Senate and Disarmament, described in the article, exemplify the benefit in hard deductive reasoning required by game preparation. (JH)

Aptamer-based polyhedral oligomeric silsesquioxane (POSS)-containing hybrid affinity monolith prepared via a "one-pot" process for selective extraction of ochratoxin A.

PubMed

Chen, Yiqiong; Chen, Maolin; Chi, Jinxin; Yu, Xia; Chen, Yongxuan; Lin, Xucong; Xie, Zenghong

2018-08-17

A novel aptamer-based polyhedral oligomeric silsesquioxane (POSS)-containing hybrid affinity monolith has been prepared with a facile "one-pot" process simultaneously via "free radical polymerization" and "thiol-ene" click reaction, and used for on-line selective extraction and practical analysis to trace ochratoxin A (OTA). By using the ternary porogenic mixture composed of water/DMF/PEG, a homogeneous polymerization mixture with POSS chemicals, acrylate-based monomers and aptamer aqueous solution was obtained, and the copolymerization of POSS chemicals, polymer monomers and aptamer aqueous solution was systematically studied. Characterizations such as the morphology, FT-IR and fluorescence spectra, mechanical stability, dynamic binding capacity, cross-reactivity and selectivity of the resultant affinity monolith were also evaluated. Attributed to the porous monolithic structure and aptamer-based affinity interaction, acceptable selective recognition and recovery yields towards trace OTA were obtained. With a 5-fold volume enrichment, the limit of detection (LOD) and limit of quantitation (LOQ) of OTA in fortified beer samples were gained at 0.025 ng/mL (S/N = 3) and 0.045 ng/mL (S/N = 10), respectively. It could be competent for the sensitive measure of actual OTA residues in real beer samples. In comparison with the previously reported strategies containing common "sol-gel" chemistry, the proposed protocol to fabricating aptamer-modified POSS-containing hybrid affinity monolith showed a simpler preparation with acceptable selectivity and higher recovery to trace OTA. Copyright © 2018 Elsevier B.V. All rights reserved.

Metal chelation dual-template epitope imprinting polymer via distillation-precipitation polymerization for recognition of porcine serum albumin.

PubMed

Qin, Ya-Ping; Wang, Hai-Yan; He, Xi-Wen; Li, Wen-You; Zhang, Yu-Kui

2018-08-01

A novel dual-template epitope imprinting polymer coated on magnetic carbon nanotubes (MCNTs@D-EMIP) was successfully prepared for specific recognition of porcine serum albumin (PSA) via dual-template epitope imprinting, metal chelation imprinting and distillation-precipitation polymerization (DPP). C-terminal peptides and N-terminal peptides of PSA were selected as templates simultaneously, and zinc acrylate and ethylene glycol dimethacrylate (EGDMA) were used as functional monomer and cross-linker, respectively. The epitope templates were immobilized by metal chelation and six-membered ring formed with zinc acrylate. Finally, MCNTs@D-EMIP was synthesized by DPP in only 30 min, which was much shorter than those of other polymerization methods. The prepared MCNTs@D-EMIP displayed specific recognition ability toward PSA and its adsorption amount and imprinting factor were 45.05 mg g -1 and 4.50, which were much higher than those of single template epitope imprinting polymers. Besides, high-performance liquid chromatography (HPLC) analysis of PSA in porcine blood serum real sample indicated that the specificity was not affected by other competitive proteins, which forcefully stated that the MCNTs@D-EMIP had potential to be applied in bio-separation area. In addition, the results of cross-reactivity experiment proved that this strategy had generality to prepare dual-template epitope imprinting polymer for recognition of target protein. In summary, this study provided an efficient protocol to recognize target protein in complex sample via dual-template epitope imprinting approach, metal chelation imprinting and distillation-precipitation polymerization. Copyright © 2018 Elsevier B.V. All rights reserved.

Cost Analysis of Various Low Pathogenic Avian Influenza Surveillance Systems in the Dutch Egg Layer Sector

PubMed Central

Rutten, Niels; Gonzales, José L.; Elbers, Armin R. W.; Velthuis, Annet G. J.

2012-01-01

Background As low pathogenic avian influenza viruses can mutate into high pathogenic viruses the Dutch poultry sector implemented a surveillance system for low pathogenic avian influenza (LPAI) based on blood samples. It has been suggested that egg yolk samples could be sampled instead of blood samples to survey egg layer farms. To support future decision making about AI surveillance economic criteria are important. Therefore a cost analysis is performed on systems that use either blood or eggs as sampled material. Methodology/Principal Findings The effectiveness of surveillance using egg or blood samples was evaluated using scenario tree models. Then an economic model was developed that calculates the total costs for eight surveillance systems that have equal effectiveness. The model considers costs for sampling, sample preparation, sample transport, testing, communication of test results and for the confirmation test on false positive results. The surveillance systems varied in sampled material (eggs or blood), sampling location (farm or packing station) and location of sample preparation (laboratory or packing station). It is shown that a hypothetical system in which eggs are sampled at the packing station and samples prepared in a laboratory had the lowest total costs (i.e. € 273,393) a year. Compared to this a hypothetical system in which eggs are sampled at the farm and samples prepared at a laboratory, and the currently implemented system in which blood is sampled at the farm and samples prepared at a laboratory have 6% and 39% higher costs respectively. Conclusions/Significance This study shows that surveillance for avian influenza on egg yolk samples can be done at lower costs than surveillance based on blood samples. The model can be used in future comparison of surveillance systems for different pathogens and hazards. PMID:22523543

Short-Term Group Psychotherapy: A Clinical Trial of a New Combination of Pretreatment and Treatment Strategies.

ERIC Educational Resources Information Center

Merkel, William T.; Willis, Stephen L.

1985-01-01

The paper discusses a clinical trial of pretreatment and treatment strategies to enhance the effectiveness of short-term groups. Pretreatment strategies included preparing patients and increasing the perceived authority of the therapists. Treatment strategies include delineation of a specific treatment focus and a directive approach by the…

Riding Elvis's Motorcycle: Using Self-Regulated Strategy Development To PLAN and WRITE for a State Writing Exam.

ERIC Educational Resources Information Center

De La Paz, Susan; Owen, Bonnie; Harris, Karen R.; Graham, Steve

2000-01-01

This article describes implementation of the Self-Regulated Strategy Development (SRSD) approach to help students learn a specific essay writing strategy in preparation for a state writing test. It also reviews the theoretical and research bases for using SRSD to teaching writing strategies. (Contains references.) (DB)

Time- and energy-efficient solution combustion synthesis of binary metal tungstate nanoparticles with enhanced photocatalytic activity.

PubMed

Thomas, Abegayl; Janáky, Csaba; Samu, Gergely F; Huda, Muhammad N; Sarker, Pranab; Liu, J Ping; van Nguyen, Vuong; Wang, Evelyn H; Schug, Kevin A; Rajeshwar, Krishnan

2015-05-22

In the search for stable and efficient photocatalysts beyond TiO2 , the tungsten-based oxide semiconductors silver tungstate (Ag2 WO4 ), copper tungstate (CuWO4 ), and zinc tungstate (ZnWO4 ) were prepared using solution combustion synthesis (SCS). The tungsten precursor's influence on the product was of particular relevance to this study, and the most significant effects are highlighted. Each sample's photocatalytic activity towards methyl orange degradation was studied and benchmarked against their respective commercial oxide sample obtained by solid-state ceramic synthesis. Based on the results herein, we conclude that SCS is a time- and energy-efficient method to synthesize crystalline binary tungstate nanomaterials even without additional excessive heat treatment. As many of these photocatalysts possess excellent photocatalytic activity, the discussed synthetic strategy may open sustainable materials chemistry avenues to solar energy conversion and environmental remediation. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Matrix interference from Fc-Fc interactions in immunoassays for detecting human IgG4 therapeutics.

PubMed

Partridge, Michael A; Karayusuf, Elif Kabuloglu; Dhulipala, Gangadhar; Dreyer, Robert; Daly, Thomas; Sumner, Giane; Pyles, Erica; Torri, Albert

2015-01-01

An assay measuring an IgG4 biotherapeutic in human serum used a drug-specific monoclonal antibody (mAb) capture reagent and an antihuman IgG4 mAb as detection reagent. However, serum IgG4 binding to the capture mAb via Fc-interactions was detected by the anti-IgG4 mAb, causing high background. Two approaches were developed to minimize background; incorporating a mild acid sample preparation step or using the Fab of the capture antibody. Either strategy improved signal:noise dramatically, increasing assay sensitivity >20-fold. Biophysical analyses of antibody domains indicated that noncovalent Fc oligomers could inhibit the background. Matrix interference from human IgG4 binding to the capture mAb was reduced with a Fab fragment of the drug-specific capture antibody or by incorporating a mild acid sample treatment into the assay.

Routine single particle CryoEM sample and grid characterization by tomography

PubMed Central

Noble, Alex J; Brasch, Julia; Chase, Jillian; Acharya, Priyamvada; Tan, Yong Zi; Zhang, Zhening; Kim, Laura Y; Scapin, Giovanna; Rapp, Micah; Eng, Edward T; Rice, William J; Cheng, Anchi; Negro, Carl J; Shapiro, Lawrence; Kwong, Peter D; Jeruzalmi, David; des Georges, Amedee; Potter, Clinton S

2018-01-01

Single particle cryo-electron microscopy (cryoEM) is often performed under the assumption that particles are not adsorbed to the air-water interfaces and in thin, vitreous ice. In this study, we performed fiducial-less tomography on over 50 different cryoEM grid/sample preparations to determine the particle distribution within the ice and the overall geometry of the ice in grid holes. Surprisingly, by studying particles in holes in 3D from over 1000 tomograms, we have determined that the vast majority of particles (approximately 90%) are adsorbed to an air-water interface. The implications of this observation are wide-ranging, with potential ramifications regarding protein denaturation, conformational change, and preferred orientation. We also show that fiducial-less cryo-electron tomography on single particle grids may be used to determine ice thickness, optimal single particle collection areas and strategies, particle heterogeneity, and de novo models for template picking and single particle alignment. PMID:29809143

Maneuver Strategy for OSIRIS-REx Proximity Operations

NASA Technical Reports Server (NTRS)

Wibben, Daniel R.; Williams, Kenneth E.; McAdams, James V.; Antreasian, Peter G.; Leonard, Jason M.; Moreau, Michael C.

2017-01-01

The Origins Spectral Interpretation Resource Identification Security Regolith Explorer (OSIRIS-REx) asteroid sample return mission will study and observe asteroid (101955) Bennu (previously known as 1999 RQ36) and subsequently collect and return a sample from the asteroid to Earth for further detailed analysis. After a successful launch in September 2016, the spacecraft will be in cruise phase for two years until arrival at asteroid Bennu in late 2018. At that time, aseries of critical maneuvers will provide an initial characterization of Bennu and the dynamical environment surrounding it, ultimately concluding with a successful capture into orbit about the small asteroid. This paper discusses some of the unique navigation challenges presented by these early operational phases in close proximity to Bennu and shares key observations and results from operational tests that have prepared the operations team and help mitigate the risks posed by these challenges.

Nano-immunoassay with improved performance for detection of cancer biomarkers

DOE PAGES

Krasnoslobodtsev, Alexey V.; Torres, Maria P.; Kaur, Sukhwinder; ...

2015-01-01

Nano-immunoassay utilizing surface-enhanced Raman scattering (SERS) effect is a promising analytical technique for the early detection of cancer. In its current standing the assay is capable of discriminating samples of healthy individuals from samples of pancreatic cancer patients. Further improvements in sensitivity and reproducibility will extend practical applications of the SERS-based detection platforms to wider range of problems. In this report, we discuss several strategies designed to improve performance of the SERS-based detection system. We demonstrate that reproducibility of the platform is enhanced by using atomically smooth mica surface as a template for preparation of capture surface in SERS sandwichmore » immunoassay. Furthermore, the assay's stability and sensitivity can be further improved by using either polymer or graphene monolayer as a thin protective layer applied on top of the assay addresses. The protective layer renders the signal to be more stable against photo-induced damage and carbonaceous contamination.« less

Application of targeted quantitative proteomics analysis in human cerebrospinal fluid using a liquid chromatography matrix-assisted laser desorption/ionization time-of-flight tandem mass spectrometer (LC MALDI TOF/TOF) platform.

PubMed

Pan, Sheng; Rush, John; Peskind, Elaine R; Galasko, Douglas; Chung, Kathryn; Quinn, Joseph; Jankovic, Joseph; Leverenz, James B; Zabetian, Cyrus; Pan, Catherine; Wang, Yan; Oh, Jung Hun; Gao, Jean; Zhang, Jianpeng; Montine, Thomas; Zhang, Jing

2008-02-01

Targeted quantitative proteomics by mass spectrometry aims to selectively detect one or a panel of peptides/proteins in a complex sample and is particularly appealing for novel biomarker verification/validation because it does not require specific antibodies. Here, we demonstrated the application of targeted quantitative proteomics in searching, identifying, and quantifying selected peptides in human cerebrospinal spinal fluid (CSF) using a matrix-assisted laser desorption/ionization time-of-flight tandem mass spectrometer (MALDI TOF/TOF)-based platform. The approach involved two major components: the use of isotopic-labeled synthetic peptides as references for targeted identification and quantification and a highly selective mass spectrometric analysis based on the unique characteristics of the MALDI instrument. The platform provides high confidence for targeted peptide detection in a complex system and can potentially be developed into a high-throughput system. Using the liquid chromatography (LC) MALDI TOF/TOF platform and the complementary identification strategy, we were able to selectively identify and quantify a panel of targeted peptides in the whole proteome of CSF without prior depletion of abundant proteins. The effectiveness and robustness of the approach associated with different sample complexity, sample preparation strategies, as well as mass spectrometric quantification were evaluated. Other issues related to chromatography separation and the feasibility for high-throughput analysis were also discussed. Finally, we applied targeted quantitative proteomics to analyze a subset of previously identified candidate markers in CSF samples of patients with Parkinson's disease (PD) at different stages and Alzheimer's disease (AD) along with normal controls.

MERCURY RESEARCH STRATEGY.

EPA Science Inventory

The USEPA's ORD is pleased to announce the availability of its Mercury Research Strategy. This strategy guides ORD's mercury research program and covers the FY2001-2005 time frame. ORD will use it to prepare a multi-year mercury research implementation plan in 2001. The Mercury R...

One Sample, One Shot - Evaluation of sample preparation protocols for the mass spectrometric proteome analysis of human bile fluid without extensive fractionation.

PubMed

Megger, Dominik A; Padden, Juliet; Rosowski, Kristin; Uszkoreit, Julian; Bracht, Thilo; Eisenacher, Martin; Gerges, Christian; Neuhaus, Horst; Schumacher, Brigitte; Schlaak, Jörg F; Sitek, Barbara

2017-02-10

The proteome analysis of bile fluid represents a promising strategy to identify biomarker candidates for various diseases of the hepatobiliary system. However, to obtain substantive results in biomarker discovery studies large patient cohorts necessarily need to be analyzed. Consequently, this would lead to an unmanageable number of samples to be analyzed if sample preparation protocols with extensive fractionation methods are applied. Hence, the performance of simple workflows allowing for "one sample, one shot" experiments have been evaluated in this study. In detail, sixteen different protocols implying modifications at the stages of desalting, delipidation, deglycosylation and tryptic digestion have been examined. Each method has been individually evaluated regarding various performance criteria and comparative analyses have been conducted to uncover possible complementarities. Here, the best performance in terms of proteome coverage has been assessed for a combination of acetone precipitation with in-gel digestion. Finally, a mapping of all obtained protein identifications with putative biomarkers for hepatocellular carcinoma (HCC) and cholangiocellular carcinoma (CCC) revealed several proteins easily detectable in bile fluid. These results can build the basis for future studies with large and well-defined patient cohorts in a more disease-related context. Human bile fluid is a proximal body fluid and supposed to be a potential source of disease markers. However, due to its biochemical composition, the proteome analysis of bile fluid still represents a challenging task and is therefore mostly conducted using extensive fractionation procedures. This in turn leads to a high number of mass spectrometric measurements for one biological sample. Considering the fact that in order to overcome the biological variability a high number of biological samples needs to be analyzed in biomarker discovery studies, this leads to the dilemma of an unmanageable number of necessary MS-based analyses. Hence, easy sample preparation protocols are demanded representing a compromise between proteome coverage and simplicity. In the presented study, such protocols have been evaluated regarding various technical criteria (e.g. identification rates, missed cleavages, chromatographic separation) uncovering the strengths and weaknesses of various methods. Furthermore, a cumulative bile proteome list has been generated that extends the current bile proteome catalog by 248 proteins. Finally, a mapping with putative biomarkers for hepatocellular carcinoma (HCC) and cholangiocellular carcinoma (CCC) derived from tissue-based studies, revealed several of these proteins being easily and reproducibly detectable in human bile. Therefore, the presented technical work represents a solid base for future disease-related studies. Copyright © 2016 Elsevier B.V. All rights reserved.

Strategies for getting through labor

MedlinePlus

... best ways to prepare is to take a childbirth class to learn what to expect in labor. ... PA: Elsevier Saunders; 2012:chap 51. Minnich ME. Childbirth preparation and nonpharmacologic analgesia. In: Chestnut DH, Wong ...

A high-throughput semi-automated preparation for filtered synaptoneurosomes.

PubMed

Murphy, Kathryn M; Balsor, Justin; Beshara, Simon; Siu, Caitlin; Pinto, Joshua G A

2014-09-30

Synaptoneurosomes have become an important tool for studying synaptic proteins. The filtered synaptoneurosomes preparation originally developed by Hollingsworth et al. (1985) is widely used and is an easy method to prepare synaptoneurosomes. The hand processing steps in that preparation, however, are labor intensive and have become a bottleneck for current proteomic studies using synaptoneurosomes. For this reason, we developed new steps for tissue homogenization and filtration that transform the preparation of synaptoneurosomes to a high-throughput, semi-automated process. We implemented a standardized protocol with easy to follow steps for homogenizing multiple samples simultaneously using a FastPrep tissue homogenizer (MP Biomedicals, LLC) and then filtering all of the samples in centrifugal filter units (EMD Millipore, Corp). The new steps dramatically reduce the time to prepare synaptoneurosomes from hours to minutes, increase sample recovery, and nearly double enrichment for synaptic proteins. These steps are also compatible with biosafety requirements for working with pathogen infected brain tissue. The new high-throughput semi-automated steps to prepare synaptoneurosomes are timely technical advances for studies of low abundance synaptic proteins in valuable tissue samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Thermoluminescence property of nano scale Al{sub 2}O{sub 3}: C by combustion method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bharthasaradhi, R.; Nehru, L. C.

In this study, thermoluminescence dosimetry material of carbon doped aluminium oxide by combustion method using Aluminium nitrate and Glycine. The Structure of the prepared Sample was carried out by XRD. The sample was nano crystalline in nature. Having hexagonal structure with unit cell parameters a=4.75Å, C=12.99Å. The surface morphology of the prepared nanopowder was carried out through (SEM). The morphology of the prepared sample is platelet structure and functional group analysis carried out through FT-IR Spectrum. The prepared sample was irradiated through γ-ray CO{sup 60} (100 Gy) was used as γ-ray source. The thermoluminescence glow curve of the irradiated samplemore » showed an isolated peak at around 200°C. The result suggest the prepared nanopowder is suitable for medical radiation dosimetry.« less

European Approaches to Homeland Security and Counterterrorism

DTIC Science & Technology

2006-07-24

departmental Counterterrorism Strategy (known as CONTEST) centered on the “ 4Ps ” of prevent, pursue, protect, and prepare. Prevention work seeks to address...largely flowed from the “ 4Ps ” of prevent, pursue, protect, and prepare in the UK’s 2004 cross-departmental counterterrorism strategy (CONTEST), which...Homeland Security and Counterterrorism 5a. CONTRACT NUMBER 5b. GRANT NUMBER 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR( S ) 5d. PROJECT NUMBER 5e. TASK NUMBER

Final Report for X-ray Diffraction Sample Preparation Method Development

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ely, T. M.; Meznarich, H. K.; Valero, T.

WRPS-1500790, “X-ray Diffraction Saltcake Sample Preparation Method Development Plan/Procedure,” was originally prepared with the intent of improving the specimen preparation methodology used to generate saltcake specimens suitable for XRD-based solid phase characterization. At the time that this test plan document was originally developed, packed powder in cavity supports with collodion binder was the established XRD specimen preparation method. An alternate specimen preparation method less vulnerable, if not completely invulnerable to preferred orientation effects, was desired as a replacement for the method.

Protocols for the analytical characterization of therapeutic monoclonal antibodies. II - Enzymatic and chemical sample preparation.

PubMed

Bobaly, Balazs; D'Atri, Valentina; Goyon, Alexandre; Colas, Olivier; Beck, Alain; Fekete, Szabolcs; Guillarme, Davy

2017-08-15

The analytical characterization of therapeutic monoclonal antibodies and related proteins usually incorporates various sample preparation methodologies. Indeed, quantitative and qualitative information can be enhanced by simplifying the sample, thanks to the removal of sources of heterogeneity (e.g. N-glycans) and/or by decreasing the molecular size of the tested protein by enzymatic or chemical fragmentation. These approaches make the sample more suitable for chromatographic and mass spectrometric analysis. Structural elucidation and quality control (QC) analysis of biopharmaceutics are usually performed at intact, subunit and peptide levels. In this paper, general sample preparation approaches used to attain peptide, subunit and glycan level analysis are overviewed. Protocols are described to perform tryptic proteolysis, IdeS and papain digestion, reduction as well as deglycosylation by PNGase F and EndoS2 enzymes. Both historical and modern sample preparation methods were compared and evaluated using rituximab and trastuzumab, two reference therapeutic mAb products approved by Food and Drug Administration (FDA) and European Medicines Agency (EMA). The described protocols may help analysts to develop sample preparation methods in the field of therapeutic protein analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Seed-Surface Grafting Precipitation Polymerization for Preparing Microsized Optically Active Helical Polymer Core/Shell Particles and Their Application in Enantioselective Crystallization.

PubMed

Zhao, Biao; Lin, Jiangfeng; Deng, Jianping; Liu, Dong

2018-05-14

Core/shell particles constructed by polymer shell and silica core have constituted a significant category of advanced functional materials. However, constructing microsized optically active helical polymer core/shell particles still remains as a big academic challenge due to the lack of effective and universal preparation methods. In this study, a seed-surface grafting precipitation polymerization (SSGPP) strategy is developed for preparing microsized core/shell particles with SiO 2 as core on which helically substituted polyacetylene is covalently bonded as shell. The resulting core/shell particles exhibit fascinating optical activity and efficiently induce enantioselective crystallization of racemic threonine. Taking advantage of the preparation strategy, novel achiral polymeric and hybrid core/shell particles are also expected. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microstructural and mechanical characteristics of porous iron prepared by powder metallurgy.

PubMed

Capek, Jaroslav; Vojtěch, Dalibor

2014-10-01

The demand for porous biodegradable load-bearing implants has been increasing recently. Based on investigations of biodegradable stents, porous iron may be a suitable material for such applications. In this study, we prepared porous iron samples with porosities of 34-51 vol.% by powder metallurgy using ammonium bicarbonate as a space-holder material. We studied sample microstructure (SEM-EDX and XRD), flexural and compressive behaviors (universal loading machine) and hardness HV5 (hardness tester) of the prepared samples. Sample porosity increased with the amount of spacer in the initial mixtures. Only the pore surfaces had insignificant oxidation and no other contamination was observed. Increasing porosity decreased the mechanical properties of the samples; although, the properties were still comparable with human bone and higher than those of porous non-metallic biomaterials and porous magnesium prepared in a similar way. Based on these results, powder metallurgy appears to be a suitable method for the preparation of porous iron for orthopedic applications. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis of SrFe12O19 magnetic nanoparticles by EDTA complex method

NASA Astrophysics Data System (ADS)

Wang, Shifa; Li, Danming; Xiao, Yuhua; Dang, Wenqiang; Feng, Jie

2017-10-01

A modified polyacrylamide gel route was used to prepare SrFe12O19 magnetic nanoparticles; ethylenediaminetetraacetic acid (EDTA) was used as a carboxyl chelating agent. The phase purity, morphology and magnetic properties of as-prepared samples were analyzed via X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometery (VSM). XRD analysis indicates that high-purity SrFe12O19 magnetic nanoparticles can be synthesized at 700°C in air. The characteristic peaks of as-prepared sample at 210, 283, 321, 340, 381, 411, 432, 475, 532, 618, 686, and 726 cm-1 were observed in Raman spectra. SEM and TEM show that the synthesized SrFe12O19 magnetic nanoparticles are uniform with the mean particle size of 60 nm. VSM measurement shows that the maximum magnetic energy product (BH)max of sample prepared using EDTA as a chelating agent is higher than that of sample prepared using citric acid as a chelating agent.

40 CFR 51.112 - Demonstration of adequacy.

Code of Federal Regulations, 2010 CFR

2010-07-01

... REQUIREMENTS FOR PREPARATION, ADOPTION, AND SUBMITTAL OF IMPLEMENTATION PLANS Control Strategy § 51.112... of the control strategy. (2) A presentation of emission levels expected to result from implementation... result from implementation of the overall control strategy presented either in tabular form or as an...

A Universal Strategy To Prepare Sulfur-Containing Polymer Composites with Desired Morphologies for Lithium-Sulfur Batteries.

PubMed

Zeng, Shao-Zhong; Zeng, Xierong; Tu, Wenxuan; Huang, Haitao; Yu, Liang; Yao, Yuechao; Jin, Nengzhi; Zhang, Qi; Zou, Jizhao

2018-06-19

Lithium-sulfur (Li-S) batteries are probably the most promising candidates for the next-generation batteries owing to their high energy density. However, Li-S batteries face severe technical problems where the dissolution of intermediate polysulfides is the biggest problem because it leads to the degradation of the cathode and the lithium anode, and finally the fast capacity decay. Compared with the composites of elemental sulfur and other matrices, sulfur-containing polymers (SCPs) have strong chemical bonds to sulfur and therefore show low dissolution of polysulfides. Unfortunately, most SCPs have very low electron conductivity and their morphologies can hardly be controlled, which undoubtedly depress the battery performances of SCPs. To overcome these two weaknesses of SCPs, a new strategy was developed for preparing SCP composites with enhanced conductivity and desired morphologies. With this strategy, macroporous SCP composites were successfully prepared from hierarchical porous carbon. The composites displayed discharge/charge capacities up to 1218/1139, 949/922, and 796/785 mA h g -1 at the current rates of 5, 10, and 15 C, respectively. Considering the universality of this strategy and the numerous morphologies of carbon materials, this strategy opens many opportunities for making carbon/SCP composites with novel morphologies.

Toward Achievement in the "Knowledge Economy" of the 21st Century: Preparing Students through T-STEM Academies

ERIC Educational Resources Information Center

Gonzales, Alberto

2010-01-01

Schools are constantly engaged in implementing reform strategies to prepare students for post-secondary education leading to their career choices. Challenges here involve education initiatives addressing programs not strategically planned, educators not prepared for transition, and no follow-up support beyond initial implementation stages. This…

Toward Achievement in the "Knowledge Economy" of the 21st Century: Preparing Students through T-STEM Academies

ERIC Educational Resources Information Center

Gonzales, Alberto; Jones, Don; Ruiz, Alberto

2014-01-01

Schools are constantly engaged in implementing reform strategies to prepare students for postsecondary education leading to their career choices. Challenges here involve education initiatives addressing programs not strategically planned, educators not prepared for transition, and no follow-up support beyond initial implementation stages. This…

Cheyenne-Laramie County Economic Development Strategy

DTIC Science & Technology

1986-06-01

Industry SIC 2879 4. Cosmetics and Toilet Preparations Industry SIC 2844 5. Electronic Connectors Industry SIC 3678 6. Mineral Wool Industry SIC 3296...five primary target-industries selected are: Soap and Other Detergents, Toilet Preparations, Agricultural Chemicals, Mineral Wool , and Electronic...Cheyenne include: -- soap and other detergents -- toilet preparation -- agricultural chemicals -- mineral wool -- electronic connectors * downtown

The Impact of Investments in Additional Preparation on Unified State Exam Results

ERIC Educational Resources Information Center

Prakhov, Ilya Arkadyevich

2015-01-01

The paper proposes a model of educational strategies for college entrants that makes it possible to assess the investment efficiency in additional preparation as evidenced by the Unified State Exam [USE] scores. It was found that college entrants still use traditional forms of preparation despite the new institutional admission conditions at…

Enhancing Pre-Service Special Educator Preparation through Combined Use of Virtual Simulation and Instructional Coaching

ERIC Educational Resources Information Center

Peterson-Ahmad, Maria

2018-01-01

To meet the ever-increasing teaching standards, pre-service special educators need extensive and advanced opportunities for pedagogical preparation prior to entering the classroom. Providing opportunities for pre-service special educators to practice such strategies within a virtual simulation environment offers teacher preparation programs a way…

Preparations for ExoMars: Learning Lessons from Curiosity

NASA Astrophysics Data System (ADS)

Edwards, Peter Henry; Hutchinson, Ian; Morgan, Sally; McHugh, Melissa; Malherbe, Cedric; Lerman, Hannah; INGLEY, Richard

2016-10-01

In 2020, the European Space Agency will launch its first Mars rover mission, ExoMars. The rover will use a drill to obtain samples from up to 2m below the Martian surface that will then be analysed using a variety of analytical instruments, including the Raman Laser Spectrometer (RLS), which will be the first Raman spectrometer to be used on a planetary mission.To prepare for ExoMars RLS operations, we report on a series of experiments that have been performed in order to investigate the response of a representative Raman instrument to a number of analogue samples (selected based on the types of material known to be important, following investigations performed by NASA's Mars Science Laboratory, MSL, on the Curiosity rover). Raman spectroscopy will provide molecular and mineralogical information about the samples obtained from the drill cores on ExoMars. MSL acquires similar information using the CheMin XRD instrument which analyses samples acquired from drill holes several centimetres deep. Like Raman spectroscopy, XRD also provides information on the mineralogical makeup of the analysed samples.The samples in our study were selected based on CheMin data obtained from drill sites at Yellowknife Bay, one of the first locations visited by Curiosity (supplemented with additional fine scale elemental information obtained with the ChemCam LIBS laser instrument). Once selected (or produced), the samples were characterised using standard laboratory XRD and XRF instruments (in order to compare with the data obtained by CheMin) and a standard, laboratory based LIBS system (in order to compare with the ChemCam data). This characterisation provides confirmation that the analogue samples are representative of the materials likely to be encountered on Mars by the ExoMars rover.A representative, miniaturised Raman spectrometer was used to analyse the samples, using acquisition strategies and operating modes similar to those expected for the ExoMars instrument. The type of minerals detected are identified and compared to the information typically acquired using other analytical science techniques investigating in order to highlight the benefits and drawbacks of using Raman spectroscopy for planetary science applications.

Differences in Students' Metacognitive Strategy Knowledge, Motivation, and Strategy Use: A Typology of Self-Regulated Learners

ERIC Educational Resources Information Center

Karlen, Yves

2016-01-01

Metacognitive strategy knowledge, motivation, and learning strategies play an important role in self-regulated learning (SRL). However, little is known about different profiles of self-regulated learners in schools that prepare students for the university entrance certificate. The aim of this study was to examine intraindividual differences in the…

Reading Strategies in French Immersion Science Classes: Preparing Our Students for Tomorrow

ERIC Educational Resources Information Center

Rivard, Leonard P.; Cormier, Marianne; Turnbull, Miles

2012-01-01

This article proposes strategies and practices that create rich discursive spaces for learning science in French immersion contexts. These strategies and practices are drawn from a variety of scholarly sources; here we adapt them to reading in the French immersion science classroom. The strategies and practices are designed for use in a…

Purposeful Sampling for Qualitative Data Collection and Analysis in Mixed Method Implementation Research.

PubMed

Palinkas, Lawrence A; Horwitz, Sarah M; Green, Carla A; Wisdom, Jennifer P; Duan, Naihua; Hoagwood, Kimberly

2015-09-01

Purposeful sampling is widely used in qualitative research for the identification and selection of information-rich cases related to the phenomenon of interest. Although there are several different purposeful sampling strategies, criterion sampling appears to be used most commonly in implementation research. However, combining sampling strategies may be more appropriate to the aims of implementation research and more consistent with recent developments in quantitative methods. This paper reviews the principles and practice of purposeful sampling in implementation research, summarizes types and categories of purposeful sampling strategies and provides a set of recommendations for use of single strategy or multistage strategy designs, particularly for state implementation research.

40 CFR 51.110 - Attainment and maintenance of national standards.

Code of Federal Regulations, 2010 CFR

2010-07-01

... PROGRAMS REQUIREMENTS FOR PREPARATION, ADOPTION, AND SUBMITTAL OF IMPLEMENTATION PLANS Control Strategy...) During developing of the plan, EPA encourages States to identify alternative control strategies, as well...

Strategies for the preparation of bifunctional gadolinium(III) chelators

PubMed Central

Frullano, Luca; Caravan, Peter

2012-01-01

The development of gadolinium chelators that can be easily and readily linked to various substrates is of primary importance for the development high relaxation efficiency and/or targeted magnetic resonance imaging (MRI) contrast agents. Over the last 25 years a large number of bifunctional chelators have been prepared. For the most part, these compounds are based on ligands that are already used in clinically approved contrast agents. More recently, new bifunctional chelators have been reported based on complexes that show a more potent relaxation effect, faster complexation kinetics and in some cases simpler synthetic procedures. This review provides an overview of the synthetic strategies used for the preparation of bifunctional chelators for MRI applications. PMID:22375102

Laser capture microdissection of embryonic cells and preparation of RNA for microarray assays.

PubMed

Redmond, Latasha C; Pang, Christopher J; Dumur, Catherine; Haar, Jack L; Lloyd, Joyce A

2014-01-01

In order to compare the global gene expression profiles of different embryonic cell types, it is first necessary to isolate the specific cells of interest. The purpose of this chapter is to provide a step-by-step protocol to perform laser capture microdissection (LCM) on embryo samples and obtain sufficient amounts of high-quality RNA for microarray hybridizations. Using the LCM/microarray strategy on mouse embryo samples has some challenges, because the cells of interest are available in limited quantities. The first step in the protocol is to obtain embryonic tissue, and immediately cryoprotect and freeze it in a cryomold containing Optimal Cutting Temperature freezing media (Sakura Finetek), using a dry ice-isopentane bath. The tissue is then cryosectioned, and the microscope slides are processed to fix, stain, and dehydrate the cells. LCM is employed to isolate specific cell types from the slides, identified under the microscope by virtue of their morphology. Detailed protocols are provided for using the currently available ArcturusXT LCM instrument and CapSure(®) LCM Caps, to which the selected cells adhere upon laser capture. To maintain RNA integrity, upon removing a slide from the final processing step, or attaching the first cells on the LCM cap, LCM is completed within 20 min. The cells are then immediately recovered from the LCM cap using a denaturing solution that stabilizes RNA integrity. RNA is prepared using standard methods, modified for working with small samples. To ensure the validity of the microarray data, the quality of the RNA is assessed using the Agilent bioanalyzer. Only RNA that is of sufficient integrity and quantity is used to perform microarray assays. This chapter provides guidance regarding troubleshooting and optimization to obtain high-quality RNA from cells of limited availability, obtained from embryo samples by LCM.

Laser Capture Microdissection of Embryonic Cells and Preparation of RNA for Microarray Assays

PubMed Central

Redmond, Latasha C.; Pang, Christopher J.; Dumur, Catherine; Haar, Jack L.; Lloyd, Joyce A.

2014-01-01

In order to compare the global gene expression profiles of different embryonic cell types, it is first necessary to isolate the specific cells of interest. The purpose of this chapter is to provide a step-by-step protocol to perform laser capture microdissection (LCM) on embryo samples and obtain sufficient amounts of high-quality RNA for microarray hybridizations. Using the LCM/microarray strategy on mouse embryo samples has some challenges, because the cells of interest are available in limited quantities. The first step in the protocol is to obtain embryonic tissue, and immediately cryoprotect and freeze it in a cryomold containing Optimal Cutting Temperature freezing media (Sakura Finetek), using a dry ice–isopentane bath. The tissue is then cryosectioned, and the microscope slides are processed to fix, stain, and dehydrate the cells. LCM is employed to isolate specific cell types from the slides, identified under the microscope by virtue of their morphology. Detailed protocols are provided for using the currently available ArcturusXT LCM instrument and CapSure® LCM Caps, to which the selected cells adhere upon laser capture. To maintain RNA integrity, upon removing a slide from the final processing step, or attaching the first cells on the LCM cap, LCM is completed within 20 min. The cells are then immediately recovered from the LCM cap using a denaturing solution that stabilizes RNA integrity. RNA is prepared using standard methods, modified for working with small samples. To ensure the validity of the microarray data, the quality of the RNA is assessed using the Agilent bioanalyzer. Only RNA that is of sufficient integrity and quantity is used to perform microarray assays. This chapter provides guidance regarding troubleshooting and optimization to obtain high-quality RNA from cells of limited availability, obtained from embryo samples by LCM. PMID:24318813

A comparative proteomics method for multiple samples based on a 18O-reference strategy and a quantitation and identification-decoupled strategy.

PubMed

Wang, Hongbin; Zhang, Yongqian; Gui, Shuqi; Zhang, Yong; Lu, Fuping; Deng, Yulin

2017-08-15

Comparisons across large numbers of samples are frequently necessary in quantitative proteomics. Many quantitative methods used in proteomics are based on stable isotope labeling, but most of these are only useful for comparing two samples. For up to eight samples, the iTRAQ labeling technique can be used. For greater numbers of samples, the label-free method has been used, but this method was criticized for low reproducibility and accuracy. An ingenious strategy has been introduced, comparing each sample against a 18 O-labeled reference sample that was created by pooling equal amounts of all samples. However, it is necessary to use proportion-known protein mixtures to investigate and evaluate this new strategy. Another problem for comparative proteomics of multiple samples is the poor coincidence and reproducibility in protein identification results across samples. In present study, a method combining 18 O-reference strategy and a quantitation and identification-decoupled strategy was investigated with proportion-known protein mixtures. The results obviously demonstrated that the 18 O-reference strategy had greater accuracy and reliability than other previously used comparison methods based on transferring comparison or label-free strategies. By the decoupling strategy, the quantification data acquired by LC-MS and the identification data acquired by LC-MS/MS are matched and correlated to identify differential expressed proteins, according to retention time and accurate mass. This strategy made protein identification possible for all samples using a single pooled sample, and therefore gave a good reproducibility in protein identification across multiple samples, and allowed for optimizing peptide identification separately so as to identify more proteins. Copyright © 2017 Elsevier B.V. All rights reserved.

Monolithic methacrylate packed 96-tips for high throughput bioanalysis.

PubMed

Altun, Zeki; Skoglund, Christina; Abdel-Rehim, Mohamed

2010-04-16

In the pharmaceutical industry the growing number of samples to be analyzed requires high throughput and fully automated analytical techniques. Commonly used sample-preparation methods are solid-phase extraction (SPE), liquid-liquid extraction (LLE) and protein precipitation. In this paper we will discus a new sample-preparation technique based on SPE for high throughput drug extraction developed and used by our group. This new sample-preparation method is based on monolithic methacrylate polymer as packing sorbent for 96-tip robotic device. Using this device a 96-well plate could be handled in 2-4min. The key aspect of the monolithic phase is that monolithic material can offer both good binding capacity and low back-pressure properties compared to e.g. silica phases. The present paper presents the successful application of monolithic 96-tips and LC-MS/MS by the sample preparation of busulphan, rescovitine, metoprolol, pindolol and local anaesthetics from human plasma samples and cyklophosphamid from mice blood samples. Copyright 2009 Elsevier B.V. All rights reserved.

Electrodeposition as an alternate method for preparation of environmental samples for iodide by AMS

DOE PAGES

Adamic, M. L.; Lister, T. E.; Dufek, E. J.; ...

2015-03-25

This paper presents an evaluation of an alternate method for preparing environmental samples for 129I analysis by accelerator mass spectrometry (AMS) at Idaho National Laboratory. The optimal sample preparation method is characterized by ease of preparation, capability of processing very small quantities of iodide, and ease of loading into a cathode. Electrodeposition of iodide on a silver wire was evaluated using these criteria. This study indicates that the electrochemically-formed silver iodide deposits produce ion currents similar to those from precipitated silver iodide for the same sample mass. Furthermore, precipitated silver iodide samples are usually mixed with niobium or silver powdermore » prior to loading in a cathode. Using electrodeposition, the silver is already mixed with the sample and can simply be picked up with tweezers, placed in the sample die, and pressed into a cathode. The major advantage of this method is that the silver wire/electrodeposited silver iodide is much easier to load into a cathode.« less

(Project 13-5292) Correlating thermal and mechanical coupling based multiphysics behavior of nuclear materials through in-situ measurements

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tomar, Vikas

Irradiations and post characterization experiments were performed first on Zr samples. This step will help understand the effect of the 2.5% alloying elements on the behavior of Zircaloy-4 (PWR cladding material) when compared to pure Zr. Irradiation flux measurements and sample temperature calibrations were performed at different energies prior to the irradiation experiments. Irradiations were performed with two different energy regimes1: non-displacment energies and displacement energies. Time was also dedicated to optimize transmission electron microscopy (TEM) sample preparation conditions via electropolishing technique. This step is crucial to prepare TEM samples for the in-situ TEM/irradiation experiments (Year 2). In addition, Zircaloy-4more » samples are being prepared for irradiation, and a setup is built by one of our collaborators (Dr. Mert Efe) to prepare ultrafine (UF) and nanocrystalline (NC) Zircaloy-4 samples for comparison with the commercial Zircaloy-4 samples.« less

Thiol-functionalization of metal-organic framework by a facile coordination-based postsynthetic strategy and enhanced removal of Hg2+ from water.

PubMed

Ke, Fei; Qiu, Ling-Guang; Yuan, Yu-Peng; Peng, Fu-Min; Jiang, Xia; Xie, An-Jian; Shen, Yu-Hua; Zhu, Jun-Fa

2011-11-30

The presence of coordinatively unsaturated metal centers in metal-organic frameworks (MOFs) provides an accessible way to selectively functionalize MOFs through coordination bonds. In this work, we describe thiol-functionalization of MOFs by choosing a well known three-dimensional (3D) Cu-based MOF, i.e. [Cu(3)(BTC)(2)(H(2)O)(3)](n) (HKUST-1, BTC=benzene-1,3,5-tricarboxylate), by a facile coordination-based postsynthetic strategy, and demonstrate their application for removal of heavy metal ion from water. A series of [Cu(3)(BTC)(2)](n) samples stoichiometrically decorated with thiol groups has been prepared through coordination bonding of coordinatively unsaturated metal centers in HKUST-1 with -SH group in dithioglycol. The obtained thiol-functionalized samples were characterized by powder X-ray diffraction, scanning electron microscope, energy dispersive X-ray spectroscopy, infrared spectroscopy, and N(2) sorption-desorption isothermal. Significantly, the thiol-functionalized [Cu(3)(BTC)(2)](n) exhibited remarkably high adsorption affinity (K(d)=4.73 × 10(5)mL g(-1)) and high adsorption capacity (714.29 mg g(-1)) for Hg(2+) adsorption from water, while the unfunctionalized HKUST-1 showed no adsorption of Hg(2+) under the same condition. Copyright © 2011 Elsevier B.V. All rights reserved.

Analysis of nutrition-relevant trace elements in human blood and serum by means of total reflection X-ray fluorescence (TXRF) spectroscopy

NASA Astrophysics Data System (ADS)

Stosnach, Hagen; Mages, Margarete

2009-04-01

In clinical service laboratories, one of the most common analytical tasks with regard to inorganic traces is the determination of the nutrition-relevant elements Fe, Cu, Zn, and Se. Because of the high numbers of samples and the commercial character of these analyses, a time-consuming sample preparation must be avoided. In this presentation, the results of total reflection X-ray fluorescence measurements with a low-power system and different sample preparation procedures are compared with those derived from analysis with common methods like Atomic Absorption Spectroscopy (AAS) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS). The results of these investigations indicate that the optimal total reflection X-ray fluorescence analysis of the nutrition-relevant elements Fe, Cu, Zn, and Se can be performed by preparing whole blood and serum samples after dilution with ultrapure water and transferring 10 μl of internally standardized sample to an unsiliconized quartz glass sample carrier with subsequent drying in a laboratory oven. Suitable measurement time was found to be 600 s. The enhanced sample preparation by means of microwave or open digestion, in parts combined with cold plasma ashing, led to an improvement of detection limits by a factor of 2 for serum samples while for whole blood samples an improvement was only observed for samples prepared by means of microwave digestion. As the matrix elements P, S, Cl, and for whole blood Fe have a major influence on the detection limits, most probably a further enhancement of analytical quality requires the removal of the organic matrix. However, for the routine analysis of the nutrition-relevant elements, the dilution preparation was found to be sufficient.

Development of an analytical strategy based on liquid chromatography-high resolution mass spectrometry for measuring perfluorinated compounds in human breast milk: application to the generation of preliminary data regarding perinatal exposure in France.

PubMed

Kadar, Hanane; Veyrand, Bruno; Barbarossa, Andrea; Pagliuca, Giampiero; Legrand, Arnaud; Bosher, Cécile; Boquien, Clair-Yves; Durand, Sophie; Monteau, Fabrice; Antignac, Jean-Philippe; Le Bizec, Bruno

2011-10-01

Perfluorinated compounds (PFCs) are man-made chemicals for which endocrine disrupting properties and related possible side effects on human health have been reported, particularly in the case of an exposure during the early stages of development, (notably the perinatal period). Existing analytical methods dedicated to PFCs monitoring in food and/or human fluids are currently based on liquid chromatography coupled to tandem mass spectrometry, and were recently demonstrated to present some limitations in terms of sensitivity and/or specificity. An alternative strategy dedicated to the analysis of fourteen PFCs in human breast milk was proposed, based on an effective sample preparation followed by a liquid chromatography coupled to high resolution mass spectrometry measurement (LC-HRMS). This methodology confirmed the high interest for HRMS after negative ionization for such halogenated substances, and finally permitted to reach detection limits around the pg mL(-1) range with an outstanding signal specificity compared to LC-MS/MS. The proposed method was applied to a first set of 30 breast milk samples from French women. The main PFCs detected in all these samples were PFOS and PFOA with respective median values of 74 (range from 24 to 171) and 57 (range from 18 to 102) pg mL(-1), respectively. These exposure data appeared in the same range as other reported values for European countries. Copyright © 2011 Elsevier Ltd. All rights reserved.

Cross-Cultural Pedagogy: Practical Strategies for a Successful Interprofessional Study Abroad Course

ERIC Educational Resources Information Center

Bai, Jieru; Larimer, Susan; Riner, Mary Beth

2016-01-01

This article discusses some practical strategies for designing and implementing a cross-cultural interprofessional study abroad course, including pre-departure preparation, facilitating small groups with local students, establishing a weekly theme, utilizing role-play and reflective assignments, and implementing meaningful evaluation strategies.…

Sample preparation for thermo-gravimetric determination and thermo-gravimetric characterization of refuse derived fuel.

PubMed

Robinson, T; Bronson, B; Gogolek, P; Mehrani, P

2016-02-01

Thermo-gravimetric analysis (TGA) is a useful method for characterizing fuels. In the past it has been applied to the study of refuse derived fuel (RDF) and related materials. However, the heterogeneity of RDF makes the preparation of small representative samples very difficult and this difficulty has limited the effectiveness of TGA for characterization of RDF. A TGA method was applied to a variety of materials prepared from a commercially available RDF using a variety of procedures. Applicability of TGA method to the determination of the renewable content of RDF was considered. Cryogenic ball milling was found to be an effective means of preparing RDF samples for TGA. When combined with an effective sample preparation, TGA could be used as an alternative method for assessing the renewable content of RDF. Crown Copyright © 2015. Published by Elsevier Ltd. All rights reserved.

FC and ZFC magnetic properties of ferro-spinels (MFe2O4) prepared by solution-combustion method

NASA Astrophysics Data System (ADS)

Aravind, G.; Kumar, R. Vijaya; Nathaniyal, V.; Rambabu, T.; Ravinder, D.

2017-07-01

Magnetic ferro-spinels MFe2O4 (M= Co and Ni) prepared by citrate-gel solution combustion method using metal nitrates with low sintering temperature (500°C). From the XRD and TEM studies confirm that a nano crystalline nature of the prepared samples. Field Cooled (FC) and Zero Field Cooled (ZFC) magnetic studies of the prepared ferro-spinels are measured by using vibrating sample magnetometer (VSM). The resultant magnetization of the prepared samples as a function of an applied magnetic field 10 T was measured at two different temperatures 5 K and 310 K. Field Cooled (FC) and Zero Field Cooled (ZFC) magnetization measurements under an applied field of 100 Oe and 1000 Oe in the temperature range of 5-375 K were carried out, which shows the blocking temperature of these two samples at around 350 K.

Preparation and Loading Process of Single Crystalline Samples into a Gas Environmental Cell Holder for In Situ Atomic Resolution Scanning Transmission Electron Microscopic Observation.

PubMed

Straubinger, Rainer; Beyer, Andreas; Volz, Kerstin

2016-06-01

A reproducible way to transfer a single crystalline sample into a gas environmental cell holder for in situ transmission electron microscopic (TEM) analysis is shown in this study. As in situ holders have only single-tilt capability, it is necessary to prepare the sample precisely along a specific zone axis. This can be achieved by a very accurate focused ion beam lift-out preparation. We show a step-by-step procedure to prepare the sample and transfer it into the gas environmental cell. The sample material is a GaP/Ga(NAsP)/GaP multi-quantum well structure on Si. Scanning TEM observations prove that it is possible to achieve atomic resolution at very high temperatures in a nitrogen environment of 100,000 Pa.

Recent developments in sample preparation and data pre-treatment in metabonomics research.

PubMed

Li, Ning; Song, Yi peng; Tang, Huiru; Wang, Yulan

2016-01-01

Metabonomics is a powerful approach for biomarker discovery and an effective tool for pinpointing endpoint metabolic effects of external stimuli, such as pathogens and disease development. Due to its wide applications, metabonomics is required to deal with various biological samples of different properties. Hence sample preparation and corresponding data pre-treatment become important factors in ensuring validity of an investigation. In this review, we summarize some recent developments in metabonomics sample preparation and data-pretreatment procedures. Copyright © 2015 Elsevier Inc. All rights reserved.

The low temperature synthesis, characterization and properties of ferroelectrics

NASA Astrophysics Data System (ADS)

Xu, Jie

2000-10-01

PZT 50:50 xerogels prepared by two different sol-gel routes crystallized in a similar fashion to give a mixture of tetragonal and rhombohedral at high temperature (1000°C). Both the diffraction and EXAFS data suggest that the compositional inhomogeneity of the samples prepared by the two routes is similar. The crystallization of CZT gels is complicated. Crystalline CaCO 3 was always detected in the dry gels regardless of the sample composition and preparation methods. At intermediate temperatures a fluorite related phase was always formed and it transformed to perovskite at higher temperatures. The EXAFS data suggest that perovskite CZT samples prepared using alkoxide sol-gel chemistry may not be random solid solutions. All the solution processed ZrTiO4 materials crystallized in the range 600--700°C. The KTN samples prepared using a conventional alkoxide sol-gel route crystallized completely to perovskite at lower temperatures than those prepared using prehydrolyzed precursors. The EXAFS data for the KTN samples prepared using a conventional alkoxide sol-gel route are consistent with a random distribution of tantalum and niobium in the solid solution. However, materials prepared using the inhomogeneous sol-gel route and by the direct reaction of mixed oxides were shown to be compositionally inhomogeneous. The heterogeneity could not be removed by regrinding and heating the mixed oxide samples several times. K2Ta4-xNbxO11 (x = 0, 2, 4) samples were prepared using alkoxide sol-gel chemistry and their crystallization was examined by powder X-ray diffraction. A Rietveld structure analysis of the pyrochlore formed from a gel with bulk composition K2Ta 2Nb2O11 indicated that it was rich in potassium relative to the bulk sample. On heating to high temperatures tetragonal tungsten bronzes were formed. A Rietveld analysis was also performed for K2Ta 2Nb2O11 with tetragonal tungsten bronze structure. The defect pyrochlores "AgTaO3" and GaTaO 3 were synthesized by ion-exchange using pyrochlore KTaO3 as a starting material. The structures of the pyrochlores were examined using the Rietveld method. The pyrochlore-to-perovskite transformations were also explored.

Reduced detection by Ziehl-Neelsen method of acid-fast bacilli in sputum samples preserved in cetylpyridinium chloride solution.

PubMed

Selvakumar, N; Sudhamathi, S; Duraipandian, M; Frieden, T R; Narayanan, P R

2004-02-01

Twelve health facilities implementing the DOTS strategy, and the Tuberculosis Research Centre (TRC), Chennai, India. To determine the detection rates using Ziehl-Neelsen (ZN) and auramine-phenol to stain acid-fast bacilli (AFB) in sputum samples stored in cetylpyridinium chloride (CPC) solution. Two smears were prepared from each of 988 sputum samples collected in CPC and randomly allocated, one to ZN and the other to auramine-phenol staining. All samples were processed for culture of Mycobacterium tuberculosis. A significantly higher proportion of samples were negative using the ZN method compared to the auramine-phenol method (74.5% vs. 61.8%, McNamara's paired chi2 test; P < 0.001). Among 377 samples that were positive using auramine-phenol, 44% were negative using ZN. There were more culture-positive, smear-negative samples in ZN (52.7%) than in auramine-phenol (30%); the difference attained statistical significance (McNemar's paired chi2 test; P < 0.00004). Using ZN, of the 104 smears made immediately after collection, 52 were positive for AFB, of which only 35 (67.3%) were positive after storage in CPC; the reduction in the number of positive smears attained statistical significance (McNemar's paired chi2 test; P = 0.004). Detection of AFB in sputum samples preserved in CPC is significantly reduced using ZN staining.

A Strategy for Sensitive, Large Scale Quantitative Metabolomics

PubMed Central

Liu, Xiaojing; Ser, Zheng; Cluntun, Ahmad A.; Mentch, Samantha J.; Locasale, Jason W.

2014-01-01

Metabolite profiling has been a valuable asset in the study of metabolism in health and disease. However, current platforms have different limiting factors, such as labor intensive sample preparations, low detection limits, slow scan speeds, intensive method optimization for each metabolite, and the inability to measure both positively and negatively charged ions in single experiments. Therefore, a novel metabolomics protocol could advance metabolomics studies. Amide-based hydrophilic chromatography enables polar metabolite analysis without any chemical derivatization. High resolution MS using the Q-Exactive (QE-MS) has improved ion optics, increased scan speeds (256 msec at resolution 70,000), and has the capability of carrying out positive/negative switching. Using a cold methanol extraction strategy, and coupling an amide column with QE-MS enables robust detection of 168 targeted polar metabolites and thousands of additional features simultaneously.  Data processing is carried out with commercially available software in a highly efficient way, and unknown features extracted from the mass spectra can be queried in databases. PMID:24894601

Technical aspects of gel-based proteomics designed for elucidating an aryl hydrocarbon receptor complex.

PubMed

Wada, Yoshinao; Nakano, Norihiko

2004-01-01

The identification of proteins by mass spectrometry has revolutionalized the basic method of identifying proteins constituting an intracellular unit or network for certain biological functions. The gel-based strategy following immunoprecipitation was applied to elucidating proteins associated with the aryl hydrocarbon receptor (AhR). Two hundred femtomoles of AhR was recovered from approximately 2 x 10(7) HepG2 cells by immunoprecipitation and was sufficient for identification by peptide mass fingerprinting. Possible candidates for the AhR-associated proteins were also identified. Improvements of the current strategy to increase the overall sensitivity tenfold are required to clarify the AhR complex in full detail. For example, a combination of trypsin and Achromobacter protease I for in-gel digestion allows the number of missed cleavage sites to be set at zero for database searching, thereby reducing random matches and facilitating identification. There is also room for improvement in each step of sample preparation prior to mass spectrometry.

Comparing Simplification Strategies for the Skeletal Muscle Proteome

PubMed Central

Geary, Bethany; Young, Iain S.; Cash, Phillip; Whitfield, Phillip D.; Doherty, Mary K.

2016-01-01

Skeletal muscle is a complex tissue that is dominated by the presence of a few abundant proteins. This wide dynamic range can mask the presence of lower abundance proteins, which can be a confounding factor in large-scale proteomic experiments. In this study, we have investigated a number of pre-fractionation methods, at both the protein and peptide level, for the characterization of the skeletal muscle proteome. The analyses revealed that the use of OFFGEL isoelectric focusing yielded the largest number of protein identifications (>750) compared to alternative gel-based and protein equalization strategies. Further, OFFGEL led to a substantial enrichment of a different sub-population of the proteome. Filter-aided sample preparation (FASP), coupled to peptide-level OFFGEL provided more confidence in the results due to a substantial increase in the number of peptides assigned to each protein. The findings presented here support the use of a multiplexed approach to proteome characterization of skeletal muscle, which has a recognized imbalance in the dynamic range of its protein complement. PMID:28248220

Fluidics platform and method for sample preparation and analysis

DOEpatents

Benner, W. Henry; Dzenitis, John M.; Bennet, William J.; Baker, Brian R.

2014-08-19

Herein provided are fluidics platform and method for sample preparation and analysis. The fluidics platform is capable of analyzing DNA from blood samples using amplification assays such as polymerase-chain-reaction assays and loop-mediated-isothermal-amplification assays. The fluidics platform can also be used for other types of assays and analyzes. In some embodiments, a sample in a sealed tube can be inserted directly. The following isolation, detection, and analyzes can be performed without a user's intervention. The disclosed platform may also comprises a sample preparation system with a magnetic actuator, a heater, and an air-drying mechanism, and fluid manipulation processes for extraction, washing, elution, assay assembly, assay detection, and cleaning after reactions and between samples.

Paper-based tuberculosis diagnostic devices with colorimetric gold nanoparticles

NASA Astrophysics Data System (ADS)

Tsai, Tsung-Ting; Shen, Shu-Wei; Cheng, Chao-Min; Chen, Chien-Fu

2013-08-01

A colorimetric sensing strategy employing gold nanoparticles and a paper assay platform has been developed for tuberculosis diagnosis. Unmodified gold nanoparticles and single-stranded detection oligonucleotides are used to achieve rapid diagnosis without complicated and time-consuming thiolated or other surface-modified probe preparation processes. To eliminate the use of sophisticated equipment for data analysis, the color variance for multiple detection results was simultaneously collected and concentrated on cellulose paper with the data readout transmitted for cloud computing via a smartphone. The results show that the 2.6 nM tuberculosis mycobacterium target sequences extracted from patients can easily be detected, and the turnaround time after the human DNA is extracted from clinical samples was approximately 1 h.

Diagnosis of Plasma Cell Dyscrasias and Monitoring of Minimal Residual Disease by Multiparametric Flow Cytometry

PubMed Central

Soh, Kah Teong; Tario, Joseph D.; Wallace, Paul K.

2018-01-01

Synopsis Plasma cell dyscrasia (PCD) is a heterogeneous disease which has seen a tremendous change in outcomes due to improved therapies. Over the last few decades, multiparametric flow cytometry has played an important role in the detection and monitoring of PCDs. Flow cytometry is a high sensitivity assay for early detection of minimal residual disease (MRD) that correlates well with progression-free survival and overall survival. Before flow cytometry can be effectively implemented in the clinical setting sample preparation, panel configuration, analysis, and gating strategies must be optimized to ensure accurate results. Current consensus methods and reporting guidelines for MRD testing are discussed. PMID:29128071

An REU Project on the Precambrian Rocks of Yellowstone National Park: Some lessons learned

NASA Astrophysics Data System (ADS)

Henry, D.; Mogk, D. W.; Mueller, P. A.; Foster, D. A.

2014-12-01

An NSF-funded REU project (2011-2013), based in Yellowstone National Park (YNP), was designed to characterize the geology, geochemistry and geochronology of Precambrian rocks in northern YNP. Over two field seasons two cadres of 12 students (12 women and 12 men) were chosen from small-to-large state universities and private colleges. REU students participated in three major activities constituting a complete research experience: Field studies involved geologic mapping and sampling of Precambrian basement; formulation of testable research questions by smaller working groups; and mapping and sampling projects to address research questions; Analytical studies, sample preparation immediately followed field work with petrographic analysis at students' home institutions and a week-long visit to analytical laboratories to conduct follow-up studies by small research groups during the academic year (Univ. Florida - geochemistry and geochronology; Univ. Minnesota - EMPA analysis); Communicating results, each working group submitted an abstract and collectively presented 13 posters at the 2011 and 2012 GSA Rocky Mountain sectional meetings. We used directed discovery to engage students in a community of practice in the field and found that a long apprenticeship (2-3 weeks) is optimal for novice-master interactions in exploring natural setting. Initial group hikes were used to normalize methods and language of the discipline. Students developed a sense of ownership of the overall project and assumed personal responsibility for directed research projects. Training was provided to: guide students in selection and appropriate use of tools; develop sampling strategies; discuss communal ethics, values, and expectations; develop efficient work habits; stimulate independent thinking; and engage decision-making. It was important to scaffold the field experience to students' level of development to lead to mastery. Analytical activities were designed from rock to analysis so that each group mastered all preparation steps and instrumental techniques under supervision of graduate mentors and lab managers leading to a clearer understanding of data interpretation. Students were communally engaged in abstract and poster preparation to ensure proper focus, scientific breadth, and style of presentation.

Motives for dish choices during home meal preparation: results from a large sample of the NutriNet-Santé study.

PubMed

Ducrot, Pauline; Méjean, Caroline; Allès, Benjamin; Fassier, Philippine; Hercberg, Serge; Péneau, Sandrine

2015-09-30

Although culinary practices have strongly evolved over time, few data are available on contemporary dish choices during meal preparation. We therefore sought to determine individual motives when choosing dishes to be prepared during weekdays and on weekends. The importance of 27 criteria related to dish choices was assessed in 53,025 participants in the NutriNet-Santé study. Dimensions of dish choice motives were investigated using exploratory factor analysis. Mean ratings of motives during weekdays and on weekends were compared using Student's t-test. Association between socio-demographic and cooking practice characteristics, and dish choice motives were evaluated using logistic regression models. Five dimensions of dish choice motives emerged: healthy diet (explained variance: 48.3%), constraints (19.0%), pleasure (12.1%), specific diets (11.0%) and organization (9.6%). The healthy diet factor was the most important on weekdays (mean rating 3.93) and weekends (3.90). Pleasure (3.61) had a higher score than constraints (3.54) on weekends (p < 0.0001) while the opposite was observed on weekdays (3.42 vs 3.77, respectively) (p < 0.0001). Organization was more important on weekdays (2.89) than on weekends (2.75) (p < 0.0001). Dish choice motives appeared to be significantly associated with socio-demographic and cooking practice characteristics. This study highlighted factors involved in dish choices in meal preparation on weekdays and weekends, as well as individual characteristics which determine motives for dish choices. From a public health perspective, these findings might help to develop appropriate strategies for promoting home meal preparation.

An Improved Thermal Conductivity Polyurethane Composite for a Space Borne 20KV Power Supply

NASA Technical Reports Server (NTRS)

Shapiro, Andrew A.; Haque, Inam

2005-01-01

This effort was designed to find a way to reduce the temperature rise of critical components of a 20KV High Voltage Power Supply (HVPS) by improving the overall thermal conductivity of the encapsulated modules. Three strategies were evaluated by developing complete procedures, preparing samples, and performing tests. The three strategies were: 1. Improve the thermal conductivity of the polyurethane encapsulant through the addition of thermally conductive powder while minimizing impact on other characteristics of the encapsulant. 2. Improve the thermal conductivity of the polyurethane encapsulated assembly by the addition of a slab of thermally conductive, electrically insulating material, which is to act as a heat spreader. 3. Employ a more thermally conductive substrate (Al203) with the existing encapsulation scheme. The materials were chosen based on the following criteria: high dielectric breakdown strength; high thermal conductivity, ease of manufacturing, high compliance, and other standard space qualified materials properties (low out-gassing, etc.). An optimized cure was determined by a statistical design of experiments for both filled and unfilled materials. The materials were characterized for the desired properties and a complete process was developed and tested. The thermal performance was substantially improved and the strategies may be used for space flight.

The effects of sample preparation on measured concentrations of eight elements in edible tissues of fish from streams contaminated by lead mining

USGS Publications Warehouse

Schmitt, Christopher J.; Finger, Susan E.

1987-01-01

The influence of sample preparation on measured concentrations of eight elements in the edible tissues of two black basses (Centrarchidae), two catfishes (Ictaluridae), and the black redhorse,Moxostoma duquesnei (Catostomidae) from two rivers in southeastern Missouri contaminated by mining and related activities was investigated. Concentrations of Pb, Cd, Cu, Zn, Fe, Mn, Ba, and Ca were measured in two skinless, boneless samples of axial muscle from individual fish prepared in a clean room. One sample (normally-processed) was removed from each fish with a knife in a manner typically used by investigators to process fish for elemental analysis and presumedly representative of methods employed by anglers when preparing fish for home consumption. A second sample (clean-processed) was then prepared from each normally-processed sample by cutting away all surface material with acid-cleaned instruments under ultraclean conditions. The samples were analyzed as a single group by atomic absorption spectrophotometry. Of the elements studied, only Pb regularly exceeded current guidelines for elemental contaminants in foods. Concentrations were high in black redhorse from contaminated sites, regardless of preparation method; for the other fishes, whether or not Pb guidelines were exceeded depended on preparation technique. Except for Mn and Ca, concentrations of all elements measured were significantly lower in cleanthan in normally-processed tissue samples. Absolute differences in measured concentrations between clean- and normally-processed samples were most evident for Pb and Ba in bass and catfish and for Cd and Zn in redhorse. Regardless of preparation method, concentrations of Pb, Ca, Mn, and Ba in individual fish were closely correlated; samples that were high or low in one of these four elements were correspondingly high or low in the other three. In contrast, correlations between Zn, Fe, and Cd occurred only in normallyprocessed samples, suggesting that these correlations resulted from high concentrations on the surfaces of some samples. Concentrations of Pb and Ba in edible tissues of fish from contaminated sites were highly correlated with Ca content, which was probably determined largely by the amount of tissue other than muscle in the sample because fish muscle contains relatively little Ca. Accordingly, variation within a group of similar samples can be reduced by normalizing Pb and Ba concentrations to a standard Ca concentration. When sample size (N) is large, this can be accomplished statistically by analysis of covariance; whenN is small, molar ratios of [Pb]/[Ca] and [Ba]/[Ca] can be computed. Without such adjustments, unrealistically large Ns are required to yield statistically reliable estimates of Pb concentrations in edible tissues. Investigators should acknowledge that reported concentrations of certain elements are only estimates, and that regardless of the care exercised during the collection, preparation, and analysis of samples, results should be interpreted with the awareness that contamination from external sources may have occurred.

40 CFR 205.171-2 - Test exhaust system sample selection and preparation.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 26 2013-07-01 2013-07-01 false Test exhaust system sample selection... Systems § 205.171-2 Test exhaust system sample selection and preparation. (a)(1) Exhaust systems comprising the sample which are required to be tested under a test request in accordance with this subpart...

Miniaturized sample preparation needle: a versatile design for the rapid analysis of smoking-related compounds in hair and air samples.

PubMed

Saito, Yoshihiro; Ueta, Ikuo; Ogawa, Mitsuhiro; Hayashida, Makiko; Jinno, Kiyokatsu

2007-05-09

Miniaturized needle extraction device has been developed as a versatile sample preparation device designed for the rapid and simple analysis of smoking-related compounds in smokers' hair samples and environmental tobacco smoke. Packed with polymeric particle, the resulting particle-packed needle was employed as a miniaturized sample preparation device for the analysis of typical volatile organic compounds in tobacco smoke. Introducing a bundle of polymer-coated filaments as the extraction medium, the needle was further applied as a novel sample preparation device containing simultaneous derivatization/extraction process of volatile aldehydes. Formaldehyde (FA) and acetaldehyde (AA) in smoker's breath during the smoking were successfully derivatized with two derivatization reagents in the polymer-coated fiber-packed needle device followed by the separation and determination in gas chromatography (GC). Smokers' hair samples were also packed into the needle, allowing the direct extraction of nicotine from the hair sample in a conventional GC injector. Optimizing the main experimental parameters for each technique, successful determination of several smoking-related compounds with these needle extraction methods has been demonstrated.

Purposeful sampling for qualitative data collection and analysis in mixed method implementation research

PubMed Central

Palinkas, Lawrence A.; Horwitz, Sarah M.; Green, Carla A.; Wisdom, Jennifer P.; Duan, Naihua; Hoagwood, Kimberly

2013-01-01

Purposeful sampling is widely used in qualitative research for the identification and selection of information-rich cases related to the phenomenon of interest. Although there are several different purposeful sampling strategies, criterion sampling appears to be used most commonly in implementation research. However, combining sampling strategies may be more appropriate to the aims of implementation research and more consistent with recent developments in quantitative methods. This paper reviews the principles and practice of purposeful sampling in implementation research, summarizes types and categories of purposeful sampling strategies and provides a set of recommendations for use of single strategy or multistage strategy designs, particularly for state implementation research. PMID:24193818

A multifaceted knowledge translation strategy can increase compliance with guideline recommendations for mechanical bowel preparation.

PubMed

Eskicioglu, Cagla; Pearsall, Emily; Victor, J Charles; Aarts, Mary-Anne; Okrainec, Allan; McLeod, Robin S

2015-01-01

The successful transfer of evidence into clinical practice is a slow and haphazard process. We report the outcome of a 5-year knowledge translation (KT) strategy to increase adherence with a clinical practice guideline (CPG) for mechanical bowel preparation (MBP) for elective colorectal surgery patients. A locally tailored CPG recommending MBP practices was developed. Data on MBP practices were collected at six University of Toronto hospitals before CPG implementation as well as after two separate KT strategies. KT strategy #1 included development of the CPG, education by opinion leaders, reminder cards, and presentations of data. KT strategy #2 included selection of hospital champions, development of communities of practice, education, reminder cards, electronic updates, pre-printed standardized orders, and audit and feedback. A total of 744 patients (400 males, 344 females, mean age 57.0) were included. Compliance increased from 58.6 to 70.4% after KT strategy #1 and to 81.1% after KT strategy #2 (p < 0.001). Using a tailored KT strategy, increased compliance was observed with CPG recommendations over time suggesting that a longitudinal KT strategy is required to increase and sustain compliance with recommendations. Furthermore, different strategies may be required at different times (i.e., educational sessions initially and reminders and standardized orders to maintain adherence).

Thermal Decomposition Behaviors and Burning Characteristics of Composite Propellants Prepared Using Combined Ammonium Perchlorate/Ammonium Nitrate Particles

NASA Astrophysics Data System (ADS)

Kohga, Makoto; Handa, Saori

2018-01-01

The thermal decomposition behaviors and burning characteristics of propellants prepared with combined ammonium perchlorate (AP)/ammonium nitrate (AN) particles greatly depended on the AN content (χ) of the AP/AN sample. The thermal decomposition behaviors of the propellants prepared with the combined samples almost matched those of the propellants prepared by physically mixing AP and AN particles, while their burning characteristics differed. The use of combined AP/AN particles decreased the heterogeneity of the combustion waves of the AP/AN propellants because of the difference in the combustion wave structure. In contrast, the addition of Fe2O3 caused unsteady combustion of the propellants prepared using samples with χ values lower than 8.1%.

A survey of specific individualized instruction strategies in elementary science methods courses in Tennessee teacher education institutions

NASA Astrophysics Data System (ADS)

Hazari, Alan A.

The purpose of the study was to determine the status of individualized science instruction in Tennessee teacher education institutions. Specifically, the study sought to investigate the extent of teaching about and/or use of 31 strategies for individualizing instruction in elementary science teaching methods courses. The individualized instruction frameworks, with strategies for individualizing instruction, were developed by Rowell, et al. in the College of Education at the University of Tennessee, Knoxville. A review of the literature on the preparation of preservice elementary science teachers for individualized instruction in K-8 classrooms revealed very limited research. This investigation sought to identify how the elementary science teacher educators prepared their preservice elementary science teachers to (1) learn about the children they will teach, (2) determine differences among learners, (3) plan for individualized science instruction in the elementary school classroom, and (4) help attend to individual student differences. The researcher prepared and used a 31-item survey to poll elementary science teacher educators in Tennessee. The participants included K-8 educators from 40 state-approved teacher education institutions. The high teacher education institution response rate (72.5%) brought input from institutions of varying sizes, operated privately or publicly across the state of Tennessee. In general, Tennessee elementary science teacher educators reported that they tended to teach about and/or use a fair number of the 31 individualized instruction strategies that involve both learning about K-8 students and their differences. On the other hand, many of these educators provided preservice teachers with quite a bit of the strategies that lead to planning for individualized science instruction and to attending to individual student differences. The two strategies that were the most taught about and/or used in elementary science methods by Tennessee educators were planning for and maintaining an interactive classroom and implementing cooperative learning groups. The two strategies with the lowest rating were using a computer-tracking system to keep student profiles and using commercial tests to determine student placement. Almost 42% of the strategies in the survey were rated high to very high. This indicated that Tennessee educators do regularly include many of these 31 strategies in their elementary science methods courses. Examples include hands-on approach, cooperative learning, thematic and project teaching, learning centers, and the use of the Tennessee Instructional Model. The study also showed that Tennessee science teacher educators in church-related institutions appeared to utilize more of the 31 strategies for individualizing instruction in K-8 classrooms than do the educators in non-church-related institutions. Tennessee K-8 teachers could be better prepared if exposed to as many different and effective pedagogical tools and practices as possible during their education and preparation. A strong science program rich in content and a variety of instructional strategies (including individualized instruction) is needed to help maximize the science learning opportunities for all Tennessee students.

The Flexibility of Self Regulated Strategy Development for Teaching Argumentative Text

ERIC Educational Resources Information Center

Leins, Patricia A.; Cuenca-Carlino, Yojanna; Kiuhara, Sharlene A.; Jacobson, Laura Thompson

2017-01-01

An increasing challenge for many secondary special education teachers is preparing students for the writing demands in postsecondary settings. The self-regulated strategy development (SRSD) model of writing instruction, considered an evidence-based practice, is an effective strategy for enhancing the writing skills of students with disabilities,…

Supporting English Language Learners in Social Studies: Language-Focused Strategies

ERIC Educational Resources Information Center

Zhang, Ying

2017-01-01

With the significant enrollment increase of English Language Learners (ELLs) nationwide, social studies teachers face challenges to educate these students. As a response to the literature of preparing all content teachers to work with ELLs, this article introduces three teacher-friendly language-focused strategies. These strategies help social…

Listening Strategies of L2 Learners with Varied Test Tasks

ERIC Educational Resources Information Center

Chang, Anna Ching-Shyang

2008-01-01

This article investigates the strategies that EFL students used and how they adjusted these strategies in response to various listening test tasks. The test tasks involved four forms of listening support: previewing questions, repeated input, background information preparation, and vocabulary instruction. Twenty-two participants were enlisted and…

Approaches and Strategies in Next Generation Science Learning

ERIC Educational Resources Information Center

Khine, Myint Swe, Ed.; Saleh, Issa M., Ed.

2013-01-01

"Approaches and Strategies in Next Generation Science Learning" examines the challenges involved in the development of modern curriculum models, teaching strategies, and assessments in science education in order to prepare future students in the 21st century economies. This comprehensive collection of research brings together science educators,…

Yukon Training Strategy. Training for the Future.

ERIC Educational Resources Information Center

Yukon Dept. of Education, White Horse.

This document was created as part of "Yukon 2000," a Yukon government initiative for steering social and economic growth. The expressed intent of the training strategy is to direct government efforts toward preparing people for existing and potential employment in the Yukon. In some areas, the strategy confirms program directions already…

Students' Perceptions of Effective Teaching Strategies in a Developmental Writing Course

ERIC Educational Resources Information Center

Dorsey, Carrie S.

2014-01-01

This dissertation explores student perceptions of effective teaching strategies in a developmental writing course and their perspectives of how well the course prepared them for the freshman college composition course. Three research questions guided the study. Research Question 1 asked which teaching strategies developmental writing students…

The Search for Connections across Principal Preparation, Principal Performance, and Student Achievement in an Exemplary Principal Preparation Program

ERIC Educational Resources Information Center

Donmoyer, Robert; Yennie-Donmoyer, June; Galloway, Fred

2012-01-01

Critics complain that the educational leadership researchers have not produced evidence that demonstrates that principal preparation programs affect student achievement. This study addressed this complaint by focusing on the impact of one exemplary program on graduates and the schools they led. The preponderance-of-evidence strategy used in this…

Strategies toward the Inclusion of Environmental Education in Educator Preparation Programs: Results from a National Survey

ERIC Educational Resources Information Center

Crim, Courtney; Moseley, Christine; Desjean-Perrotta, Blanche

2017-01-01

A national study was conducted to investigate the inclusion of environmental education (EE) into educator preparation programs across the United States. Responses from teacher educators in institutions of higher education indicated that the infusion of EE into educator preparation programs is limited and varies greatly across the nation. Findings…

40 CFR 761.323 - Sample preparation.

Code of Federal Regulations, 2011 CFR

2011-07-01

... PROHIBITIONS Self-Implementing Alternative Extraction and Chemical Analysis Procedures for Non-liquid PCB Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a... of use in this chemical extraction and chemical analysis comparison study, a person may adjust PCB...

Preparing Brigade Combat Team Soldiers for Mission Readiness Through Research on Intangible Psychological Constructs and their Applications. Phase 2: Measurement and Learning Methods

DTIC Science & Technology

2014-02-01

10 Cognitive Learning Strategies, Metacognitive Strategies, Scaffolding, and Cognitive Tutoring...culture, technology , and instructional practices. 11 7. Motivational and emotional influences on learning - What and how much is learned is...of learning and intangible skills. These resulting set of theories includes: 12 • Cognitive learning strategies, metacognitive strategies

Strategies for Coping with Language Anxiety: The Case of Students of English in Japan

ERIC Educational Resources Information Center

Kondo, David Shinji; Ying-Ling, Yang

2004-01-01

This study was designed to develop a typology of strategies that students use to cope with the anxiety they experience in English language classrooms. The influence of anxiety level on strategy use was also assessed. Findings suggested 70 basic tactics for coping with language anxiety that cohered into five strategy categories: Preparation (e.g.…

Gas engine heat pump cycle analysis. Volume 1: Model description and generic analysis

NASA Astrophysics Data System (ADS)

Fischer, R. D.

1986-10-01

The task has prepared performance and cost information to assist in evaluating the selection of high voltage alternating current components, values for component design variables, and system configurations and operating strategy. A steady-state computer model for performance simulation of engine-driven and electrically driven heat pumps was prepared and effectively used for parametric and seasonal performance analyses. Parametric analysis showed the effect of variables associated with design of recuperators, brine coils, domestic hot water heat exchanger, compressor size, engine efficiency, insulation on exhaust and brine piping. Seasonal performance data were prepared for residential and commercial units in six cities with system configurations closely related to existing or contemplated hardware of the five GRI engine contractors. Similar data were prepared for an advanced variable-speed electric unit for comparison purposes. The effect of domestic hot water production on operating costs was determined. Four fan-operating strategies and two brine loop configurations were explored.

Exploring nursing students' level of preparedness for disaster response.

PubMed

Schmidt, Cheryl K; Davis, Jennifer M; Sanders, Jenna L; Chapman, Laura A; Cisco, Mary Catherine; Hady, Arlene R

2011-01-01

This descriptive study explores students' perceptions of personal and program preparedness for disasters. Participants in this online survey included 1,348 nursing students from every state plus Guam, Puerto Rico, and theVirgin Islands. The study explored three questions: a) the level of preparedness, including learning about different types of disasters, preparing disaster plans, creating disaster kits, and participating in community disaster response efforts; b) the impact of disasters on nursing students; and c) strategies to assist nursing students during disasters. Results indicated that nursing students throughout the country are generally not well prepared for disasters. Nurse educators need to develop strategies to prepare their students for disasters. The American Red Cross provides templates for organizations, including colleges and universities, to prepare their campuses for emergencies. Faculty need to collaborate with staff and students to develop and implement plans appropriate for their programs.

Teaching/learning strategies for the essentials of baccalaureate nursing education for entry-level community/public health nursing.

PubMed

Callen, Bonnie; Smith, Claudia M; Joyce, Barbara; Lutz, Jayne; Brown-Schott, Nancy; Block, Derryl

2013-01-01

The purpose of this article is to describe teaching/learning strategies for each of the 15 Essentials of Baccalaureate Nursing Education for Entry-Level Community/Public Health Nursing (ACHNE, 2009). Carper's ways of knowing serve as foundations for creating classroom and clinical experiences that focus on clinical action with community as client. Each community/public health essential is defined with relevance to community/public health nursing practice. Five teaching/learning strategies have been delineated for each essential with suggestions of teaching resources and/or target population application. Teaching/learning strategies that focus on community as client, population health, and the essential knowledge and competencies of C/PH nursing will help ensure preparation of baccalaureate prepared nurses with knowledge and skills to improve the health of populations. © 2013 Wiley Periodicals, Inc.

Preparation, certification and interlaboratory analysis of workplace air filters spiked with high-fired beryllium oxide.

PubMed

Oatts, Thomas J; Hicks, Cheryl E; Adams, Amy R; Brisson, Michael J; Youmans-McDonald, Linda D; Hoover, Mark D; Ashley, Kevin

2012-02-01

Occupational sampling and analysis for multiple elements is generally approached using various approved methods from authoritative government sources such as the National Institute for Occupational Safety and Health (NIOSH), the Occupational Safety and Health Administration (OSHA) and the Environmental Protection Agency (EPA), as well as consensus standards bodies such as ASTM International. The constituents of a sample can exist as unidentified compounds requiring sample preparation to be chosen appropriately, as in the case of beryllium in the form of beryllium oxide (BeO). An interlaboratory study was performed to collect analytical data from volunteer laboratories to examine the effectiveness of methods currently in use for preparation and analysis of samples containing calcined BeO powder. NIST SRM(®) 1877 high-fired BeO powder (1100 to 1200 °C calcining temperature; count median primary particle diameter 0.12 μm) was used to spike air filter media as a representative form of beryllium particulate matter present in workplace sampling that is known to be resistant to dissolution. The BeO powder standard reference material was gravimetrically prepared in a suspension and deposited onto 37 mm mixed cellulose ester air filters at five different levels between 0.5 μg and 25 μg of Be (as BeO). Sample sets consisting of five BeO-spiked filters (in duplicate) and two blank filters, for a total of twelve unique air filter samples per set, were submitted as blind samples to each of 27 participating laboratories. Participants were instructed to follow their current process for sample preparation and utilize their normal analytical methods for processing samples containing substances of this nature. Laboratories using more than one sample preparation and analysis method were provided with more than one sample set. Results from 34 data sets ultimately received from the 27 volunteer laboratories were subjected to applicable statistical analyses. The observed performance data show that sample preparations using nitric acid alone, or combinations of nitric and hydrochloric acids, are not effective for complete extraction of Be from the SRM 1877 refractory BeO particulate matter spiked on air filters; but that effective recovery can be achieved by using sample preparation procedures utilizing either sulfuric or hydrofluoric acid, or by using methodologies involving ammonium bifluoride with heating. Laboratories responsible for quantitative determination of Be in workplace samples that may contain high-fired BeO should use quality assurance schemes that include BeO-spiked sampling media, rather than solely media spiked with soluble Be compounds, and should ensure that methods capable of quantitative digestion of Be from the actual material present are used.

Microfluidic Sample Preparation for Diagnostic Cytopathology

PubMed Central

Mach, Albert J.; Adeyiga, Oladunni B.; Di Carlo, Dino

2014-01-01

The cellular components of body fluids are routinely analyzed to identify disease and treatment approaches. While significant focus has been placed on developing cell analysis technologies, tools to automate the preparation of cellular specimens have been more limited, especially for body fluids beyond blood. Preparation steps include separating, concentrating, and exposing cells to reagents. Sample preparation continues to be routinely performed off-chip by technicians, preventing cell-based point-of-care diagnostics, increasing the cost of tests, and reducing the consistency of the final analysis following multiple manually-performed steps. Here, we review the assortment of biofluids for which suspended cells are analyzed, along with their characteristics and diagnostic value. We present an overview of the conventional sample preparation processes for cytological diagnosis. We finally discuss the challenges and opportunities in developing microfluidic devices for the purpose of automating or miniaturizing these processes, with particular emphases on preparing large or small volume samples, working with samples of high cellularity, automating multi-step processes, and obtaining high purity subpopulations of cells. We hope to convey the importance of and help identify new research directions addressing the vast biological and clinical applications in preparing and analyzing the array of available biological fluids. Successfully addressing the challenges described in this review can lead to inexpensive systems to improve diagnostic accuracy while simultaneously reducing overall systemic healthcare costs. PMID:23380972

Structural morphology, upconversion luminescence and optical thermometric sensing behavior of Y2O3:Er(3+)/Yb(3+) nano-crystalline phosphor.

PubMed

Joshi, C; Dwivedi, A; Rai, S B

2014-08-14

Infrared-to-visible upconverting rare earths Er(3+)/Yb(3+) co-doped Y2O3 nano-crystalline phosphor samples have been prepared by solution combustion method followed by post-heat treatment at higher temperatures. A slight increase in average crystallite size has been found on calcinations verified by X-ray analysis. Transmission electron microscopy (TEM) confirms the nano-crystalline nature of the as-prepared and calcinated samples. Fourier transform infrared (FTIR) analysis shows the structural changes in as-prepared and calcinated samples. Upconversion and downconversion emission recorded using 976 and 532 nm laser sources clearly demonstrates a better luminescence properties in the calcinated samples as compared to as-prepared sample. Upconversion emission has been quantified in terms of standard chromaticity diagram (CIE) showing a shift in overall upconversion emission of as-prepared and calcinated samples. Temperature sensing behaviour of this material has also been investigated by measurement of fluorescence intensity ratio (FIR) of various signals in green emission in the temperature range of 315 to 555 K under 976 nm laser excitation. Copyright © 2014 Elsevier B.V. All rights reserved.

Nearly 1000 Protein Identifications from 50 ng of Xenopus laevis Zygote Homogenate Using Online Sample Preparation on a Strong Cation Exchange Monolith Based Microreactor Coupled with Capillary Zone Electrophoresis.

PubMed

Zhang, Zhenbin; Sun, Liangliang; Zhu, Guijie; Cox, Olivia F; Huber, Paul W; Dovichi, Norman J

2016-01-05

A sulfonate-silica hybrid strong cation exchange monolith microreactor was synthesized and coupled to a linear polyacrylamide coated capillary for online sample preparation and capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) bottom-up proteomic analysis. The protein sample was loaded onto the microreactor in an acidic buffer. After online reduction, alkylation, and digestion with trypsin, the digests were eluted with 200 mM ammonium bicarbonate at pH 8.2 for CZE-MS/MS analysis using 1 M acetic acid as the background electrolyte. This combination of basic elution and acidic background electrolytes results in both sample stacking and formation of a dynamic pH junction. 369 protein groups and 1274 peptides were identified from 50 ng of Xenopus laevis zygote homogenate, which is comparable with an offline sample preparation method, but the time required for sample preparation was decreased from over 24 h to less than 40 min. Dramatically improved performance was produced by coupling the reactor to a longer separation capillary (∼100 cm) and a Q Exactive HF mass spectrometer. 975 protein groups and 3749 peptides were identified from 50 ng of Xenopus protein using the online sample preparation method.

An in situ self-assembly template strategy for the preparation of hierarchical-pore metal-organic frameworks

PubMed Central

Huang, Hongliang; Li, Jian-Rong; Wang, Keke; Han, Tongtong; Tong, Minman; Li, Liangsha; Xie, Yabo; Yang, Qingyuan; Liu, Dahuan; Zhong, Chongli

2015-01-01

Metal-organic frameworks (MOFs) have recently emerged as a new type of nanoporous materials with tailorable structures and functions. Usually, MOFs have uniform pores smaller than 2 nm in size, limiting their practical applications in some cases. Although a few approaches have been adopted to prepare MOFs with larger pores, it is still challenging to synthesize hierarchical-pore MOFs (H-MOFs) with high structural controllability and good stability. Here we demonstrate a facile and versatile method, an in situ self-assembly template strategy for fabricating stable H-MOFs, in which multi-scale soluble and/or acid-sensitive metal-organic assembly (MOA) fragments form during the reactions between metal ions and organic ligands (to construct MOFs), and act as removable dynamic chemical templates. This general strategy was successfully used to prepare various H-MOFs that show rich porous properties and potential applications, such as in large molecule adsorption. Notably, the mesopore sizes of the H-MOFs can be tuned by varying the amount of templates. PMID:26548441

Automated storm water sampling on small watersheds

USGS Publications Warehouse

Harmel, R.D.; King, K.W.; Slade, R.M.

2003-01-01

Few guidelines are currently available to assist in designing appropriate automated storm water sampling strategies for small watersheds. Therefore, guidance is needed to develop strategies that achieve an appropriate balance between accurate characterization of storm water quality and loads and limitations of budget, equipment, and personnel. In this article, we explore the important sampling strategy components (minimum flow threshold, sampling interval, and discrete versus composite sampling) and project-specific considerations (sampling goal, sampling and analysis resources, and watershed characteristics) based on personal experiences and pertinent field and analytical studies. These components and considerations are important in achieving the balance between sampling goals and limitations because they determine how and when samples are taken and the potential sampling error. Several general recommendations are made, including: setting low minimum flow thresholds, using flow-interval or variable time-interval sampling, and using composite sampling to limit the number of samples collected. Guidelines are presented to aid in selection of an appropriate sampling strategy based on user's project-specific considerations. Our experiences suggest these recommendations should allow implementation of a successful sampling strategy for most small watershed sampling projects with common sampling goals.

Integrated Sampling Strategy (ISS) Guide

Treesearch

Robert E. Keane; Duncan C. Lutes

2006-01-01

What is an Integrated Sampling Strategy? Simply put, it is the strategy that guides how plots are put on the landscape. FIREMON’s Integrated Sampling Strategy assists fire managers as they design their fire monitoring project by answering questions such as: What statistical approach is appropriate for my sample design? How many plots can I afford? How many plots do I...

Three Dimensional Nitrogen-Doped and Nitrogen, Sulfur-Codoped Graphene Hydrogels for Electrode Materials in Supercapacitors.

PubMed

Yuan, Zhao; Qiao, Fei; Wang, Guiqiang; Zhou, Jin; Cui, Hongyou; Zhuo, Shuping; Xing, Ling-Bao

2018-08-01

In present work, reduced graphene oxide hydrogels (RGOHs) with three-dimensional (3D) porous structure are prepared through chemical reduction method by using aminourea (NRGOHs) and aminothiourea (NSRGOHs) as reductants. The as-prepared RGOHs are considered not only as promising electrode materials for supercapacitors, but also the doping of nitrogen (aminourea, NRGOHs) or nitrogen/sulfur (aminothiourea, NSRGOHs) can improve electrochemical performance through faradaic pseudocapacitance. The optimized samples have been prepared by controlling the mass ratios of graphene oxide (GO) to aminourea or aminothiourea to be 1:1, 1:2 and 1:5, respectively. With adding different amounts of aminourea or aminothiourea, the obtained RGOHs exhibited different electrochemical performance in supercapacitors. With increasing the dosage of the reductants, the RGOHs revealed better specific capacitances. Moreover, NSRGOHs with nitrogen, sulfur-codoping exhibited better capacitance performance than that of NRGOHs with only nitrogen-doping. NSRGOHs showed excellent capacitive performance with a very high specific capacitance up to 232.2, 323.3 and 345.6 F g-1 at 0.2 A g-1, while NRGOHs showed capacitive performance with specific capacitance up to 220.6, 306.5 and 332.7 F g-1 at 0.2 A g-1. This provides a strategy to improve the capacitive properties of RGOHs significantly by controlling different doping the materials.

Novel dual ligand co-functionalized fluorescent gold nanoclusters as a versatile probe for sensitive analysis of Hg(2+) and oxytetracycline.

PubMed

Xu, Shenghao; Li, Xiaolin; Mao, Yaning; Gao, Teng; Feng, Xiuying; Luo, Xiliang

2016-04-01

In this work, we present a direct one-step strategy for rapidly preparing dual ligand co-functionalized fluorescent Au nanoclusters (NCs) by using threonine (Thr) and 11-mercaptoundecanoic acid (MUA) as assorted reductants and capping agents in aqueous solution at room temperature. Fluorescence spectra, high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), dynamic light scattering (DLS), and infrared (IR) spectroscopy were performed to demonstrate the optical properties and chemical composition of the as-prepared AuNCs. They possess many attractive features such as near-infrared emission (λem = 606 nm), a large Stoke's shift (>300 nm), high colloidal stability (pH, temperature, salt, and time stability), and water dispersibility. Subsequently, the as-prepared AuNCs were used as a versatile probe for "turn off" sensing of Hg(2+) based on aggregation-induced fluorescence quenching and for "turn-on" sensing of oxytetracycline (OTC). This assay provided good linearity ranging from 37.5 to 3750 nM for Hg(2+) and from 0.375 to 12.5 μM for OTC, with detection limits of 8.6 nM and 0.15 μM, respectively. Moreover, the practical application of this assay was further validated by detecting OTC in human serum samples.

Flexible automated approach for quantitative liquid handling of complex biological samples.

PubMed

Palandra, Joe; Weller, David; Hudson, Gary; Li, Jeff; Osgood, Sarah; Hudson, Emily; Zhong, Min; Buchholz, Lisa; Cohen, Lucinda H

2007-11-01

A fully automated protein precipitation technique for biological sample preparation has been developed for the quantitation of drugs in various biological matrixes. All liquid handling during sample preparation was automated using a Hamilton MicroLab Star Robotic workstation, which included the preparation of standards and controls from a Watson laboratory information management system generated work list, shaking of 96-well plates, and vacuum application. Processing time is less than 30 s per sample or approximately 45 min per 96-well plate, which is then immediately ready for injection onto an LC-MS/MS system. An overview of the process workflow is discussed, including the software development. Validation data are also provided, including specific liquid class data as well as comparative data of automated vs manual preparation using both quality controls and actual sample data. The efficiencies gained from this automated approach are described.

Sensory profile and acceptability for pitanga (Eugenia uniflora L.) nectar with different sweeteners.

PubMed

Freitas, Mírian Luisa Faria; Dutra, Mariana Borges de Lima; Bolini, Helena Maria André

2016-12-01

The objective of this study was to evaluate the sensory properties and acceptability of pitanga nectar samples prepared with sucrose and different sweeteners (sucralose, aspartame, stevia with 40% rebaudioside A, stevia with 95% rebaudioside A, neotame, and a 2:1 cyclamate/saccharin blend). A total of 13 assessors participated in a quantitative descriptive analysis and evaluated the samples in relation to the descriptor terms. The acceptability test was carried out by 120 fruit juice consumers. The results of the quantitative descriptive analysis of pitanga nectar showed that samples prepared with sucralose, aspartame, and the 2:1 cyclamate/saccharin blend had sensory profiles similar to that of the sample prepared with sucrose. Consumers' most accepted samples were prepared with sucrose, sucralose, aspartame, and neotame. The sweeteners that have the greatest potential to replace sucrose in pitanga nectar are sucralose and aspartame. © The Author(s) 2016.

The occurrence of Salmonella in airline meals.

PubMed

Hatakka, M; Asplund, K

1993-01-01

The occurrence of Salmonella in airline meals was studied in 1989-1992. Samples were collected from flight kitchens in 29 countries. The material consisted of 400 cold dishes and 1,288 hot dishes as well as salads, cheese plates and deserts. Total number of samples was 2211. Salmonella spp. were isolated from 6 samples; 1 contaminated sample was a cold dish prepared in Bangkok, 1 was a hot dish prepared in Mombasa and the remaining 4 contaminated samples were hot dishes prepared within one week in Beijing. The isolated serotypes were S. ohio, S. manchester and S. braenderup. The contaminated cold dish prepared by a flight kitchen in Bangkok was found to be connected with a Salmonella outbreak which occurred in Finland in 1990. Cold airline dishes containing food of animal origin seems to be more risky as a source of Salmonella infections among airline passengers.

Non-invasive determination of glucose directly in raw fruits using a continuous flow system based on microdialysis sampling and amperometric detection at an integrated enzymatic biosensor.

PubMed

Vargas, E; Ruiz, M A; Campuzano, S; Reviejo, A J; Pingarrón, J M

2016-03-31

A non-destructive, rapid and simple to use sensing method for direct determination of glucose in non-processed fruits is described. The strategy involved on-line microdialysis sampling coupled with a continuous flow system with amperometric detection at an enzymatic biosensor. Apart from direct determination of glucose in fruit juices and blended fruits, this work describes for the first time the successful application of an enzymatic biosensor-based electrochemical approach to the non-invasive determination of glucose in raw fruits. The methodology correlates, through previous calibration set-up, the amperometric signal generated from glucose in non-processed fruits with its content in % (w/w). The comparison of the obtained results using the proposed approach in different fruits with those provided by other method involving the same commercial biosensor as amperometric detector in stirred solutions pointed out that there were no significant differences. Moreover, in comparison with other available methodologies, this microdialysis-coupled continuous flow system amperometric biosensor-based procedure features straightforward sample preparation, low cost, reduced assay time (sampling rate of 7 h(-1)) and ease of automation. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of the molecular weight of poly(ethylene glycol) in biological samples by reversed-phase LC-MS with in-source fragmentation.

PubMed

Warrack, Bethanne M; Redding, Brian P; Chen, Guodong; Bolgar, Mark S

2013-05-01

PEGylation has been widely used to improve the biopharmaceutical properties of therapeutic proteins and peptides. Previous studies have used multiple analytical techniques to determine the fate of both the therapeutic molecule and unconjugated poly(ethylene glycol) (PEG) after drug administration. A straightforward strategy utilizing liquid chromatography-mass spectrometry (LC-MS) to characterize high-molecular weight PEG in biologic matrices without a need for complex sample preparation is presented. The method is capable of determining whether high-MW PEG is cleaved in vivo to lower-molecular weight PEG species. Reversed-phase chromatographic separation is used to take advantage of the retention principles of polymeric materials whereby elution order correlates with PEG molecular weight. In-source collision-induced dissociation (CID) combined with selected reaction monitoring (SRM) or selected ion monitoring (SIM) mass spectrometry (MS) is then used to monitor characteristic PEG fragment ions in biological samples. MS provides high sensitivity and specificity for PEG and the observed retention times in reversed-phase LC enable estimation of molecular weight. This method was successfully used to characterize PEG molecular weight in mouse serum samples. No change in molecular weight was observed for 48 h after dosing.

30 CFR 7.48 - Acid resistance test.

Code of Federal Regulations, 2010 CFR

2010-07-01

...) Test procedures. (1) Prepare one sample each of the insulated surfaces of the battery box and of the... for the battery box and cover, only one sample need be prepared and tested. (2) Prepare a 30 percent... insulation plus the battery cover or box material. The insulation thickness shall be representative of that...

30 CFR 7.48 - Acid resistance test.

Code of Federal Regulations, 2014 CFR

2014-07-01

...) Test procedures. (1) Prepare one sample each of the insulated surfaces of the battery box and of the... for the battery box and cover, only one sample need be prepared and tested. (2) Prepare a 30 percent... insulation plus the battery cover or box material. The insulation thickness shall be representative of that...

30 CFR 7.48 - Acid resistance test.

Code of Federal Regulations, 2013 CFR

2013-07-01

...) Test procedures. (1) Prepare one sample each of the insulated surfaces of the battery box and of the... for the battery box and cover, only one sample need be prepared and tested. (2) Prepare a 30 percent... insulation plus the battery cover or box material. The insulation thickness shall be representative of that...

The importance of sample collection when using single cytokine levels and systemic cytokine profiles as biomarkers--a comparative study of serum versus plasma samples.

PubMed

Tvedt, Tor Henrik Anderson; Rye, Kristin Paulsen; Reikvam, Håkon; Brenner, Annette K; Bruserud, Øystein

2015-03-01

Cytokines, soluble adhesion molecules and metalloproteinases can be detected in human serum or plasma samples. Such systemic levels are widely used as biomarkers in epidemiological and clinical studies. We prepared serum samples and three types of plasma samples (EDTA, heparin, citric acid) from 20 healthy individuals. The levels of 31 cytokines, four soluble adhesion molecules and eight matrix metalloproteinases were analyzed by Luminex technology. Most mediators showed detectable levels in both plasma and serum. Several mediators that can be released by platelets showed increased serum levels, especially CCL5 and CD40L, but for the other mediators the serum levels did not correlate with peripheral blood platelet counts and for these last mediators serum and plasma levels often showed strong correlations. The use of bivalirudin for anticoagulation significantly increased and citric acid combined with platelet inhibitors (ticagrelor, acetylsalicylic acid plus prostaglandin E2) did not alter plasma levels of platelet-store mediators compared with citric acid alone. The impact of sample preparation differed between mediators; for many mediators strong correlations were seen between serum and plasma levels even when absolute levels differed. Soluble adhesion molecule levels showed only minor differences between samples. Unsupervised hierarchical clustering suggested that the effect of sampling/preparation was strongest for serum and heparin plasma samples. Careful standardization of sample preparation is usually necessary when analyzing systemic mediator levels, and differences caused by sample preparation should be considered as a possible explanation if studies show conflicting results. Copyright © 2015 Elsevier B.V. All rights reserved.

An Overview of Conventional and Emerging Analytical Methods for the Determination of Mycotoxins

PubMed Central

Cigić, Irena Kralj; Prosen, Helena

2009-01-01

Mycotoxins are a group of compounds produced by various fungi and excreted into the matrices on which they grow, often food intended for human consumption or animal feed. The high toxicity and carcinogenicity of these compounds and their ability to cause various pathological conditions has led to widespread screening of foods and feeds potentially polluted with them. Maximum permissible levels in different matrices have also been established for some toxins. As these are quite low, analytical methods for determination of mycotoxins have to be both sensitive and specific. In addition, an appropriate sample preparation and pre-concentration method is needed to isolate analytes from rather complicated samples. In this article, an overview of methods for analysis and sample preparation published in the last ten years is given for the most often encountered mycotoxins in different samples, mainly in food. Special emphasis is on liquid chromatography with fluorescence and mass spectrometric detection, while in the field of sample preparation various solid-phase extraction approaches are discussed. However, an overview of other analytical and sample preparation methods less often used is also given. Finally, different matrices where mycotoxins have to be determined are discussed with the emphasis on their specific characteristics important for the analysis (human food and beverages, animal feed, biological samples, environmental samples). Various issues important for accurate qualitative and quantitative analyses are critically discussed: sampling and choice of representative sample, sample preparation and possible bias associated with it, specificity of the analytical method and critical evaluation of results. PMID:19333436

Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

NASA Technical Reports Server (NTRS)

Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo

2012-01-01

The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

Microextraction by packed sorbent: an emerging, selective and high-throughput extraction technique in bioanalysis.

PubMed

Pereira, Jorge; Câmara, José S; Colmsjö, Anders; Abdel-Rehim, Mohamed

2014-06-01

Sample preparation is an important analytical step regarding the isolation and concentration of desired components from complex matrices and greatly influences their reliable and accurate analysis and data quality. It is the most labor-intensive and error-prone process in analytical methodology and, therefore, may influence the analytical performance of the target analytes quantification. Many conventional sample preparation methods are relatively complicated, involving time-consuming procedures and requiring large volumes of organic solvents. Recent trends in sample preparation include miniaturization, automation, high-throughput performance, on-line coupling with analytical instruments and low-cost operation through extremely low volume or no solvent consumption. Micro-extraction techniques, such as micro-extraction by packed sorbent (MEPS), have these advantages over the traditional techniques. This paper gives an overview of MEPS technique, including the role of sample preparation in bioanalysis, the MEPS description namely MEPS formats (on- and off-line), sorbents, experimental and protocols, factors that affect the MEPS performance, and the major advantages and limitations of MEPS compared with other sample preparation techniques. We also summarize MEPS recent applications in bioanalysis. Copyright © 2014 John Wiley & Sons, Ltd.

Detection of Acetone Processing of Castor Bean Mash for Forensic Investigation of Ricin Preparation Methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kreuzer-Martin, Helen W.; Wahl, Jon H.; Metoyer, Candace N.

The toxic protein ricin is of concern as a potential biological threat agent (BTA) Recently, several samples of ricin have been seized in connection with biocriminal activity. Analytical methods are needed that enable federal investigators to determine how the samples were prepared, to match seized samples to potential source materials, and to identify samples that may have been prepared by the same method using the same source materials. One commonly described crude ricin preparation method is acetone extraction of crushed castor beans. Here we describe the use of solid-phase microextraction and headspace analysis of crude ricin preparation samples to determinemore » whether they were processed by acetone extraction. In all cases, acetone-extracted bean mash could be distinguished from un-extracted mash or mash extracted with other organic solvents. Statistical analysis showed that storage in closed containers for up to 109 days had no effect on acetone signal intensity. Signal intensity in acetone-extracted mash decreased during storage in open containers, but extracted mash could still be distinguished from un-extracted mash after 94 days.« less

Effect of salt concentrations and drying methods on the quality and formation of histamine in dried milkfish (Chanos chanos).

PubMed

Hwang, Chiu-Chu; Lin, Chia-Min; Kung, Hsien-Feng; Huang, Ya-Ling; Hwang, Deng-Fwu; Su, Yi-Cheng; Tsai, Yung-Hsiang

2012-11-15

The effects of salt concentrations (0-15.0%) and drying methods on the quality of dried milkfish were studied. The results showed that the levels of aerobic plate counts, total coliform, water activity, moisture contents, total volatile basic nitrogen (TVBN) and thiobarbituric acid (TBA) of the dried milkfish samples prepared with the same drying method decreased with increased salt concentrations. The samples prepared with the cold-air drying method had better quality in term of lower TVBN and TBA values than those of samples prepared with other drying methods. The histamine contents in all samples, except two, prepared with various salt concentrations by different drying methods were less than 1.9 mg/100 g. Two unsalted samples prepared with hot-air drying at 35 °C and sun drying methods were found to contain histamine at levels of 249.7 and 67.4 mg/100 g, respectively, which were higher than the potential hazard level of 50 mg/100 g. Copyright © 2012 Elsevier Ltd. All rights reserved.

Optimization of Sample Preparation processes of Bone Material for Raman Spectroscopy.

PubMed

Chikhani, Madelen; Wuhrer, Richard; Green, Hayley

2018-03-30

Raman spectroscopy has recently been investigated for use in the calculation of postmortem interval from skeletal material. The fluorescence generated by samples, which affects the interpretation of Raman data, is a major limitation. This study compares the effectiveness of two sample preparation techniques, chemical bleaching and scraping, in the reduction of fluorescence from bone samples during testing with Raman spectroscopy. Visual assessment of Raman spectra obtained at 1064 nm excitation following the preparation protocols indicates an overall reduction in fluorescence. Results demonstrate that scraping is more effective at resolving fluorescence than chemical bleaching. The scraping of skeletonized remains prior to Raman analysis is a less destructive method and allows for the preservation of a bone sample in a state closest to its original form, which is beneficial in forensic investigations. It is recommended that bone scraping supersedes chemical bleaching as the preferred method for sample preparation prior to Raman spectroscopy. © 2018 American Academy of Forensic Sciences.

Direct Analysis of Samples of Various Origin and Composition Using Specific Types of Mass Spectrometry.

PubMed

Byliński, Hubert; Gębicki, Jacek; Dymerski, Tomasz; Namieśnik, Jacek

2017-07-04

One of the major sources of error that occur during chemical analysis utilizing the more conventional and established analytical techniques is the possibility of losing part of the analytes during the sample preparation stage. Unfortunately, this sample preparation stage is required to improve analytical sensitivity and precision. Direct techniques have helped to shorten or even bypass the sample preparation stage; and in this review, we comment of some of the new direct techniques that are mass-spectrometry based. The study presents information about the measurement techniques using mass spectrometry, which allow direct sample analysis, without sample preparation or limiting some pre-concentration steps. MALDI - MS, PTR - MS, SIFT - MS, DESI - MS techniques are discussed. These solutions have numerous applications in different fields of human activity due to their interesting properties. The advantages and disadvantages of these techniques are presented. The trends in development of direct analysis using the aforementioned techniques are also presented.

MRM validation of targeted nonglycosylated peptides from N-glycoprotein biomarkers using direct trypsin digestion of undepleted human plasma.

PubMed

Lee, Ju Yeon; Kim, Jin Young; Cheon, Mi Hee; Park, Gun Wook; Ahn, Yeong Hee; Moon, Myeong Hee; Yoo, Jong Shin

2014-02-26

A rapid, simple, and reproducible MRM-based validation method for serological glycoprotein biomarkers in clinical use was developed by targeting the nonglycosylated tryptic peptides adjacent to N-glycosylation sites. Since changes in protein glycosylation are known to be associated with a variety of diseases, glycoproteins have been major targets in biomarker discovery. We previously found that nonglycosylated tryptic peptides adjacent to N-glycosylation sites differed in concentration between normal and hepatocellular carcinoma (HCC) plasma due to differences in steric hindrance of the glycan moiety in N-glycoproteins to tryptic digestion (Lee et al., 2011). To increase the feasibility and applicability of clinical validation of biomarker candidates (nonglycosylated tryptic peptides), we developed a method to effectively monitor nonglycosylated tryptic peptides from a large number of plasma samples and to reduce the total analysis time with maximizing the effect of steric hindrance by the glycans during digestion of glycoproteins. The AUC values of targeted nonglycosylated tryptic peptides were excellent (0.955 for GQYCYELDEK, 0.880 for FEDGVLDPDYPR and 0.907 for TEDTIFLR), indicating that these could be effective biomarkers for hepatocellular carcinoma. This method provides the necessary throughput required to validate glycoprotein biomarkers, as well as quantitative accuracy for human plasma analysis, and should be amenable to clinical use. Difficulties in verifying and validating putative protein biomarkers are often caused by complex sample preparation procedures required to determine their concentrations in a large number of plasma samples. To solve the difficulties, we developed MRM-based protein biomarker assays that greatly reduce complex, time-consuming, and less reproducible sample pretreatment steps in plasma for clinical implementation. First, we used undepleted human plasma samples without any enrichment procedures. Using nanoLC/MS/MS, we targeted nonglycosylated tryptic peptides adjacent to N-linked glycosylation sites in N-linked glycoprotein biomarkers, which could be detected in human plasma samples without depleting highly abundant proteins. Second, human plasma proteins were digested with trypsin without reduction and alkylation procedures to minimize sample preparation. Third, trypsin digestion times were shortened so as to obtain reproducible results with maximization of the steric hindrance effect of the glycans during enzyme digestion. Finally, this rapid and simple sample preparation method was applied to validate targeted nonglycosylated tryptic peptides as liver cancer biomarker candidates for diagnosis in 40 normal and 41 hepatocellular carcinoma (HCC) human plasma samples. This strategy provided the necessary throughput required to monitor protein biomarkers, as well as quantitative accuracy in human plasma analysis. From biomarker discovery to clinical implementation, our method will provide a biomarker study platform that is suitable for clinical deployment, and can be applied to high-throughput approaches. Copyright © 2014 Elsevier B.V. All rights reserved.

A study on the use of near-infrared spectroscopy for the rapid quantification of major compounds in Tanreqing injection

NASA Astrophysics Data System (ADS)

Li, Wenlong; Cheng, Zhiwei; Wang, Yuefei; Qu, Haibin

2013-01-01

In this paper we describe the strategy used in the development and validation of a near infrared spectroscopy method for the rapid determination of baicalin, chlorogenic acid, ursodeoxycholic acid (UDCA), chenodeoxycholic acid (CDCA), and the total solid contents (TSCs) in the Tanreqing injection. To increase the representativeness of calibration sample set, a concentrating-diluting method was adopted to artificially prepare samples. Partial least square regression (PLSR) was used to establish calibration models, with which the five quality indicators can be determined with satisfied accuracy and repeatability. In addition, the slope/bias (S/B) method was used for the models transfer between two different types of NIR instruments from the same manufacturer, which is contributing to enlarge the application range of the established models. With the presented method, a great deal of time, effort and money can be saved when large amounts of Tanreqing injection samples need to be analyzed in a relatively short period of time, which is of great significance to the traditional Chinese medicine (TCM) industries.

Integrated electrochemical microsystems for genetic detection of pathogens at the point of care.

PubMed

Hsieh, Kuangwen; Ferguson, B Scott; Eisenstein, Michael; Plaxco, Kevin W; Soh, H Tom

2015-04-21

The capacity to achieve rapid, sensitive, specific, quantitative, and multiplexed genetic detection of pathogens via a robust, portable, point-of-care platform could transform many diagnostic applications. And while contemporary technologies have yet to effectively achieve this goal, the advent of microfluidics provides a potentially viable approach to this end by enabling the integration of sophisticated multistep biochemical assays (e.g., sample preparation, genetic amplification, and quantitative detection) in a monolithic, portable device from relatively small biological samples. Integrated electrochemical sensors offer a particularly promising solution to genetic detection because they do not require optical instrumentation and are readily compatible with both integrated circuit and microfluidic technologies. Nevertheless, the development of generalizable microfluidic electrochemical platforms that integrate sample preparation and amplification as well as quantitative and multiplexed detection remains a challenging and unsolved technical problem. Recognizing this unmet need, we have developed a series of microfluidic electrochemical DNA sensors that have progressively evolved to encompass each of these critical functionalities. For DNA detection, our platforms employ label-free, single-step, and sequence-specific electrochemical DNA (E-DNA) sensors, in which an electrode-bound, redox-reporter-modified DNA "probe" generates a current change after undergoing a hybridization-induced conformational change. After successfully integrating E-DNA sensors into a microfluidic chip format, we subsequently incorporated on-chip genetic amplification techniques including polymerase chain reaction (PCR) and loop-mediated isothermal amplification (LAMP) to enable genetic detection at clinically relevant target concentrations. To maximize the potential point-of-care utility of our platforms, we have further integrated sample preparation via immunomagnetic separation, which allowed the detection of influenza virus directly from throat swabs and developed strategies for the multiplexed detection of related bacterial strains from the blood of septic mice. Finally, we developed an alternative electrochemical detection platform based on real-time LAMP, which not is only capable of detecting across a broad dynamic range of target concentrations, but also greatly simplifies quantitative measurement of nucleic acids. These efforts represent considerable progress toward the development of a true sample-in-answer-out platform for genetic detection of pathogens at the point of care. Given the many advantages of these systems, and the growing interest and innovative contributions from researchers in this field, we are optimistic that iterations of these systems will arrive in clinical settings in the foreseeable future.

Phosphopeptide Enrichment by Covalent Chromatography after Derivatization of Protein Digests Immobilized on Reversed-Phase Supports

PubMed Central

Nika, Heinz; Nieves, Edward; Hawke, David H.; Angeletti, Ruth Hogue

2013-01-01

A rugged sample-preparation method for comprehensive affinity enrichment of phosphopeptides from protein digests has been developed. The method uses a series of chemical reactions to incorporate efficiently and specifically a thiol-functionalized affinity tag into the analyte by barium hydroxide catalyzed β-elimination with Michael addition using 2-aminoethanethiol as nucleophile and subsequent thiolation of the resulting amino group with sulfosuccinimidyl-2-(biotinamido) ethyl-1,3-dithiopropionate. Gentle oxidation of cysteine residues, followed by acetylation of α- and ε-amino groups before these reactions, ensured selectivity of reversible capture of the modified phosphopeptides by covalent chromatography on activated thiol sepharose. The use of C18 reversed-phase supports as a miniaturized reaction bed facilitated optimization of the individual modification steps for throughput and completeness of derivatization. Reagents were exchanged directly on the supports, eliminating sample transfer between the reaction steps and thus, allowing the immobilized analyte to be carried through the multistep reaction scheme with minimal sample loss. The use of this sample-preparation method for phosphopeptide enrichment was demonstrated with low-level amounts of in-gel-digested protein. As applied to tryptic digests of α-S1- and β-casein, the method enabled the enrichment and detection of the phosphorylated peptides contained in the mixture, including the tetraphosphorylated species of β-casein, which has escaped chemical procedures reported previously. The isolates proved highly suitable for mapping the sites of phosphorylation by collisionally induced dissociation. β-Elimination, with consecutive Michael addition, expanded the use of the solid-phase-based enrichment strategy to phosphothreonyl peptides and to phosphoseryl/phosphothreonyl peptides derived from proline-directed kinase substrates and to their O-sulfono- and O-linked β-N-acetylglucosamine (O-GlcNAc)-modified counterparts. Solid-phase enzymatic dephosphorylation proved to be a viable tool to condition O-GlcNAcylated peptide in mixtures with phosphopeptides for selective affinity purification. Acetylation, as an integral step of the sample-preparation method, precluded reduction in recovery of the thiolation substrate caused by intrapeptide lysine-dehydroalanine cross-link formation. The solid-phase analytical platform provides robustness and simplicity of operation using equipment readily available in most biological laboratories and is expected to accommodate additional chemistries to expand the scope of solid-phase serial derivatization for protein structural characterization. PMID:23997662

Influence of the initial surface texture on the resulting surface roughness and waviness for micro-machining with ultra-short laser pulses (Conference Presentation)

NASA Astrophysics Data System (ADS)

Remund, Stefan M.; Jaeggi, Beat; Kramer, Thorsten; Neuenschwander, Beat

2017-03-01

The resulting surface roughness and waviness after processing with ultra-short pulsed laser radiation depend on the laser parameters as well as on the machining strategy and the scanning system. However the results depend on the material and its initial surface quality and finishing as well. The improvement of surface finishing represents effort and produces additional costs. For industrial applications it is important to reduce the preparation of a workpiece for laser micro-machining to optimize quality and reduce costs. The effects of the ablation process and the influence of the machining strategy and scanning system onto the surface roughness and waviness can be differenced due to their separate manner. By using the optimal laser parameters on an initially perfect surface, the ablation process mainly increases the roughness to a certain value for most metallic materials. However, imperfections in the scanning system causing a slight variation in the scanning speed lead to a raise of the waviness on the sample surface. For a basic understanding of the influence of grinding marks, the sample surfaces were initially furnished with regular grooves of different depths and spatial frequencies to gain a homogenous and well-defined original surface. On these surfaces the effect of different beam waists and machining strategy are investigated and the results are compared with a simulation of the process. Furthermore the behaviors of common surface finishes used in industrial applications for laser micro-machining are studied and the relation onto the resulting surface roughness and waviness is presented.

Target-induced formation of gold amalgamation on DNA-based sensing platform for electrochemical monitoring of mercury ion coupling with cycling signal amplification strategy.

PubMed

Chen, Jinfeng; Tang, Juan; Zhou, Jun; Zhang, Lan; Chen, Guonan; Tang, Dianping

2014-01-31

Heavy metal ion pollution poses severe risks in human health and environmental pollutant, because of the likelihood of bioaccumulation and toxicity. Driven by the requirement to monitor trace-level mercury ion (Hg(2+)), herein we construct a new DNA-based sensor for sensitive electrochemical monitoring of Hg(2+) by coupling target-induced formation of gold amalgamation on DNA-based sensing platform with gold amalgamation-catalyzed cycling signal amplification strategy. The sensor was simply prepared by covalent conjugation of aminated poly-T(25) oligonucleotide onto the glassy carbon electrode by typical carbodiimide coupling. Upon introduction of target analyte, Hg(2+) ion was intercalated into the DNA polyion complex membrane based on T-Hg(2+)-T coordination chemistry. The chelated Hg(2+) ion could induce the formation of gold amalgamation, which could catalyze the p-nitrophenol with the aid of NaBH4 and Ru(NH3)6(3+) for cycling signal amplification. Experimental results indicated that the electronic signal of our system increased with the increasing Hg(2+) level in the sample, and has a detection limit of 0.02nM with a dynamic range of up to 1000nM Hg(2+). The strategy afforded exquisite selectivity for Hg(2+) against other environmentally related metal ions. In addition, the methodology was evaluated for the analysis of Hg(2+) in spiked tap-water samples, and the recovery was 87.9-113.8%. Copyright © 2013 Elsevier B.V. All rights reserved.

Impact of Anesthesia and Euthanasia on Metabolomics of Mammalian Tissues: Studies in a C57BL/6J Mouse Model

PubMed Central

Overmyer, Katherine A.; Thonusin, Chanisa; Qi, Nathan R.; Burant, Charles F.; Evans, Charles R.

2015-01-01

A critical application of metabolomics is the evaluation of tissues, which are often the primary sites of metabolic dysregulation in disease. Laboratory rodents have been widely used for metabolomics studies involving tissues due to their facile handing, genetic manipulability and similarity to most aspects of human metabolism. However, the necessary step of administration of anesthesia in preparation for tissue sampling is not often given careful consideration, in spite of its potential for causing alterations in the metabolome. We examined, for the first time using untargeted and targeted metabolomics, the effect of several commonly used methods of anesthesia and euthanasia for collection of skeletal muscle, liver, heart, adipose and serum of C57BL/6J mice. The data revealed dramatic, tissue-specific impacts of tissue collection strategy. Among many differences observed, post-euthanasia samples showed elevated levels of glucose 6-phosphate and other glycolytic intermediates in skeletal muscle. In heart and liver, multiple nucleotide and purine degradation metabolites accumulated in tissues of euthanized compared to anesthetized animals. Adipose tissue was comparatively less affected by collection strategy, although accumulation of lactate and succinate in euthanized animals was observed in all tissues. Among methods of tissue collection performed pre-euthanasia, ketamine showed more variability compared to isoflurane and pentobarbital. Isoflurane induced elevated liver aspartate but allowed more rapid initiation of tissue collection. Based on these findings, we present a more optimal collection strategy mammalian tissues and recommend that rodent tissues intended for metabolomics studies be collected under anesthesia rather than post-euthanasia. PMID:25658945

Impact of anesthesia and euthanasia on metabolomics of mammalian tissues: studies in a C57BL/6J mouse model.

PubMed

Overmyer, Katherine A; Thonusin, Chanisa; Qi, Nathan R; Burant, Charles F; Evans, Charles R

2015-01-01

A critical application of metabolomics is the evaluation of tissues, which are often the primary sites of metabolic dysregulation in disease. Laboratory rodents have been widely used for metabolomics studies involving tissues due to their facile handing, genetic manipulability and similarity to most aspects of human metabolism. However, the necessary step of administration of anesthesia in preparation for tissue sampling is not often given careful consideration, in spite of its potential for causing alterations in the metabolome. We examined, for the first time using untargeted and targeted metabolomics, the effect of several commonly used methods of anesthesia and euthanasia for collection of skeletal muscle, liver, heart, adipose and serum of C57BL/6J mice. The data revealed dramatic, tissue-specific impacts of tissue collection strategy. Among many differences observed, post-euthanasia samples showed elevated levels of glucose 6-phosphate and other glycolytic intermediates in skeletal muscle. In heart and liver, multiple nucleotide and purine degradation metabolites accumulated in tissues of euthanized compared to anesthetized animals. Adipose tissue was comparatively less affected by collection strategy, although accumulation of lactate and succinate in euthanized animals was observed in all tissues. Among methods of tissue collection performed pre-euthanasia, ketamine showed more variability compared to isoflurane and pentobarbital. Isoflurane induced elevated liver aspartate but allowed more rapid initiation of tissue collection. Based on these findings, we present a more optimal collection strategy mammalian tissues and recommend that rodent tissues intended for metabolomics studies be collected under anesthesia rather than post-euthanasia.

ACT Test

MedlinePlus

... Sample Required? A blood sample drawn from a vein in your arm Test Preparation Needed? None Looking ... is obtained by inserting a needle into a vein in the arm. Is any test preparation needed ...

Separation of Be and Al for AMS using single-step column chromatography

NASA Astrophysics Data System (ADS)

Binnie, Steven A.; Dunai, Tibor J.; Voronina, Elena; Goral, Tomasz; Heinze, Stefan; Dewald, Alfred

2015-10-01

With the aim of simplifying AMS target preparation procedures for TCN measurements we tested a new extraction chromatography approach which couples an anion exchange resin (WBEC) to a chelating resin (Beryllium resin) to separate Be and Al from dissolved quartz samples. Results show that WBEC-Beryllium resin stacks can be used to provide high purity Be and Al separations using a combination of hydrochloric/oxalic and nitric acid elutions. 10Be and 26Al concentrations from quartz samples prepared using more standard procedures are compared with results from replicate samples prepared using the coupled WBEC-Beryllium resin approach and show good agreement. The new column procedure is performed in a single step, reducing sample preparation times relative to more traditional methods of TCN target production.

Recombinant Intrinsically Disordered Proteins for NMR: Tips and Tricks.

PubMed

Calçada, Eduardo O; Korsak, Magdalena; Kozyreva, Tatiana

2015-01-01

The growing recognition of the several roles that intrinsically disordered proteins play in biology places an increasing importance on protein sample availability to allow the characterization of their structural and dynamic properties. The sample preparation is therefore the limiting step to allow any biophysical method being able to characterize the properties of an intrinsically disordered protein and to clarify the links between these properties and the associated biological functions. An increasing array of tools has been recruited to help prepare and characterize the structural and dynamic properties of disordered proteins. This chapter describes their sample preparation, covering the most common drawbacks/barriers usually found working in the laboratory bench. We want this chapter to be the bedside book of any scientist interested in preparing intrinsically disordered protein samples for further biophysical analysis.

Current trends in sample preparation for cosmetic analysis.

PubMed

Zhong, Zhixiong; Li, Gongke

2017-01-01

The widespread applications of cosmetics in modern life make their analysis particularly important from a safety point of view. There is a wide variety of restricted ingredients and prohibited substances that primarily influence the safety of cosmetics. Sample preparation for cosmetic analysis is a crucial step as the complex matrices may seriously interfere with the determination of target analytes. In this review, some new developments (2010-2016) in sample preparation techniques for cosmetic analysis, including liquid-phase microextraction, solid-phase microextraction, matrix solid-phase dispersion, pressurized liquid extraction, cloud point extraction, ultrasound-assisted extraction, and microwave digestion, are presented. Furthermore, the research and progress in sample preparation techniques and their applications in the separation and purification of allowed ingredients and prohibited substances are reviewed. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.