Crystallization of Macromolecules

PubMed Central

Friedmann, David; Messick, Troy; Marmorstein, Ronen

2014-01-01

X-ray crystallography has evolved into a very powerful tool to determine the three-dimensional structure of macromolecules and macromolecular complexes. The major bottleneck in structure determination by X-ray crystallography is the preparation of suitable crystalline samples. This unit outlines steps for the crystallization of a macromolecule, starting with a purified, homogeneous sample. The first protocols describe preparation of the macromolecular sample (i.e., proteins, nucleic acids, and macromolecular complexes). The preparation and assessment of crystallization trials is then described, along with a protocol for confirming whether the crystals obtained are composed of macromolecule as opposed to a crystallization reagent . Next, the optimization of crystallization conditions is presented. Finally, protocols that facilitate the growth of larger crystals through seeding are described. PMID:22045560

Performance of fly ash based geopolymer incorporating palm kernel shell for lightweight concrete

NASA Astrophysics Data System (ADS)

Razak, Rafiza Abd; Abdullah, Mohd Mustafa Al Bakri; Yahya, Zarina; Jian, Ang Zhi; Nasri, Armia

2017-09-01

A concrete which cement is totally replaced by source material such as fly ash and activated by highly alkaline solutions is known as geopolymer concrete. Fly ash is the most common source material for geopolymer because it is a by-product material, so it can get easily from all around the world. An investigation has been carried out to select the most suitable ingredients of geopolymer concrete so that the geopolymer concrete can achieve the desire compressive strength. The samples were prepared to determine the suitable percentage of palm kernel shell used in geopolymer concrete and cured for 7 days in oven. After that, other samples were prepared by using the suitable percentage of palm kernel shell and cured for 3, 14, 21 and 28 days in oven. The control sample consisting of ordinary Portland cement and palm kernel shell and cured for 28 days were prepared too. The NaOH concentration of 12M, ratio Na2SiO3 to NaOH of 2.5, ratio fly ash to alkaline activator solution of 2.0 and ratio water to geopolymer of 0.35 were fixed throughout the research. The density obtained for the samples were 1.78 kg/m3, water absorption of 20.41% and the compressive strength of 14.20 MPa. The compressive strength of geopolymer concrete is still acceptable as lightweight concrete although the compressive strength is lower than OPC concrete. Therefore, the proposed method by using fly ash mixed with 10% of palm kernel shell can be used to design geopolymer concrete.

Comparison of green sample preparation techniques in the analysis of pyrethrins and pyrethroids in baby food by liquid chromatography-tandem mass spectrometry.

PubMed

Petrarca, Mateus Henrique; Ccanccapa-Cartagena, Alexander; Masiá, Ana; Godoy, Helena Teixeira; Picó, Yolanda

2017-05-12

A new selective and sensitive liquid chromatography triple quadrupole mass spectrometry method was developed for simultaneous analysis of natural pyrethrins and synthetic pyrethroids residues in baby food. In this study, two sample preparation methods based on ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and salting-out assisted liquid-liquid extraction (SALLE) were optimized, and then, compared regarding the performance criteria. Appropriate linearity in solvent and matrix-based calibrations, and suitable recoveries (75-120%) and precision (RSD values≤16%) were achieved for selected analytes by any of the sample preparation procedures. Both methods provided the analytical selectivity required for the monitoring of the insecticides in fruit-, cereal- and milk-based baby foods. SALLE, recognized by cost-effectiveness, and simple and fast execution, provided a lower enrichment factor, consequently, higher limits of quantification (LOQs) were obtained. Some of them too high to meet the strict legislation regarding baby food. Nonetheless, the combination of ultrasound and DLLME also resulted in a high sample throughput and environmental-friendly method, whose LOQs were lower than the default maximum residue limit (MRL) of 10μgkg -1 set by European Community for baby foods. In the commercial baby foods analyzed, cyhalothrin and etofenprox were detected in different samples, demonstrating the suitability of proposed method for baby food control. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

Specimen preparation for high-resolution cryo-EM

PubMed Central

Passmore, Lori A.; Russo, Christopher J.

2016-01-01

Imaging a material with electrons at near-atomic resolution requires a thin specimen that is stable in the vacuum of the transmission electron microscope. For biological samples, this comprises a thin layer of frozen aqueous solution containing the biomolecular complex of interest. The process of preparing a high-quality specimen is often the limiting step in the determination of structures by single-particle electron cryomicroscopy (cryo-EM). Here we describe a systematic approach for going from a purified biomolecular complex in aqueous solution to high-resolution electron micrographs that are suitable for 3D structure determination. This includes a series of protocols for the preparation of vitrified specimens on various specimen supports, including all-gold and graphene. We also describe techniques for troubleshooting when a preparation fails to yield suitable specimens, and common mistakes to avoid during each part of the process. Finally, we include recommendations for obtaining the highest quality micrographs from prepared specimens with current microscope, detector and support technology. PMID:27572723

Sampling of Atmospheric Precipitation and Deposits for Analysis of Atmospheric Pollution

PubMed Central

Skarżyńska, K.; Polkowska, Ż; Namieśnik, J.

2006-01-01

This paper reviews techniques and equipment for collecting precipitation samples from the atmosphere (fog and cloud water) and from atmospheric deposits (dew, hoarfrost, and rime) that are suitable for the evaluation of atmospheric pollution. It discusses the storage and preparation of samples for analysis and also presents bibliographic information on the concentration ranges of inorganic and organic compounds in the precipitation and atmospheric deposit samples. PMID:17671615

Visualizing preparation using asymmetrical choline-like ionic liquids for scanning electron microscope observation of non-conductive biological samples.

PubMed

Abe, Shigeaki; Hyono, Atsushi; Kawai, Koji; Yonezawa, Tetsu

2014-03-01

In this study, we investigated conductivity preparation for scanning electron microscope (SEM) observation that used novel asymmetrical choline-type room temperature ionic liquids (RTIL). By immersion in only an RTIL solution, clear SEM images of several types of biological samples were successfully observed. In addition, we could visualize protozoans using RTILs without any dilution. These results suggested that the asymmetrical choline-type RTILs used in this study are suitable for visualizing of biological samples by SEM. Treatment without the need for dilution can obviate the need for adjusting the RTIL concentration and provide for a rapid and easy conductivity treatment for insulating samples.

Preparation and validation of gross alpha/beta samples used in EML`s quality assessment program

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

Scarpitta, S.C.

1997-10-01

A set of water and filter samples have been incorporated into the existing Environmental Measurements Laboratory`s (EML) Quality Assessment Program (QAP) for gross alpha/beta determinations by participating DOE laboratories. The participating laboratories are evaluated by comparing their results with the EML value. The preferred EML method for measuring water and filter samples, described in this report, uses gas flow proportional counters with 2 in. detectors. Procedures for sample preparation, quality control and instrument calibration are presented. Liquid scintillation (LS) counting is an alternative technique that is suitable for quantifying both the alpha ({sup 241}Am, {sup 230}Th and {sup 238}Pu) andmore » beta ({sup 90}Sr/{sup 90}Y) activity concentrations in the solutions used to prepare the QAP water and air filter samples. Three LS counting techniques (Cerenkov, dual dpm and full spectrum analysis) are compared. These techniques may be used to validate the activity concentrations of each component in the alpha/beta solution before the QAP samples are actually prepared.« less

Synthesis, Optical and Electrochemical Properties of Y2O3 Nanoparticles Prepared by Co-Precipitation Method.

PubMed

Saravanan, Thulasingam; Raj, Srinivasan Gokul; Chandar, Nagamuthu Raja Krishna; Jayavel, Ramasamy

2015-06-01

Y2O3 nanoparticles were synthesized by co-precipitation route using yttrium nitrate hexahydrate and ammonium hydroxide as precursors. The prepared sample was calcined at 500 degrees C and subjected to various characterization studies like thermal analysis (TG/DTA), X-ray diffraction (XRD), transmission electron microscope (TEM), UV-visible (UV-Vis) and photoluminescence (PL) spectroscopy. The XRD pattern showed the cubic fluorite structure of Y2O3 without any impurity peaks, revealing high purity of the prepared sample. TEM images revealed that the calcined Y2O3 nanoparticles consist of spherical-like morphology with an average particle size of 12 nm. The absorption spectrum of calcined samples shows blue-shift compared to the as-prepared sample, which was further confirmed by PL studies. The possible formation mechanism of Y2O3 nanoparticles has been discussed based on the experimental results. Electrochemical behavior of Y2O3 nanoparticles was studied by cyclic voltammetry to assess their suitability for supercapacitor applications.

High-Throughput Analytical Techniques for the Determination of the Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea, Part VII: A GC-MS, GC-MS/MS, and LC-MS/MS Study of the Degradation Profiles of Pesticide Residues in Green Tea.

PubMed

Chang, Qiao-Ying; Pang, Guo-Fang; Fan, Chun-Lin; Chen, Hui; Yang, Fang; Li, Jie; Wen, Bi-Fang

2016-11-01

GC-MS, GC-tandem MS (MS/MS), and LC-MS/MS were used to mathematically define the degradation profiles of pesticide residues in two field trials. Nineteen pesticides were studied in the first field trial and 11 in the second. The results of the field trials demonstrated that the degradation profiles of pesticide residues in green tea can be described with power functions to successfully estimate the amount of time, following pesticide application, pesticide residues appearing in tea in concentrations at and/or above the maximum residue limit (MRL) decrease to concentrations below the MRL. Stability tests on green tea samples stored at room temperature were conducted to determine whether pesticide-incurred green tea samples prepared according to the method used in the field trials would be suitable for the preparation of reference standards for laboratory-proficiency testing trials. This paper reports the results of a GC-MS, GC-MS/MS, and LC-MS/MS study, as well as the suitability of the samples prepared under these conditions for use as pesticide reference standards in tea analysis.

Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.

2004-01-01

A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

Portable sample preparation and analysis system for micron and sub-micron particle characterization using light scattering and absorption spectroscopy

DOEpatents

Stark, Peter C [Los Alamos, NM; Zurek, Eduardo [Barranquilla, CO; Wheat, Jeffrey V [Fort Walton Beach, FL; Dunbar, John M [Santa Fe, NM; Olivares, Jose A [Los Alamos, NM; Garcia-Rubio, Luis H [Temple Terrace, FL; Ward, Michael D [Los Alamos, NM

2011-07-26

There is provided a method and device for remote sampling, preparation and optical interrogation of a sample using light scattering and light absorption methods. The portable device is a filtration-based device that removes interfering background particle material from the sample matrix by segregating or filtering the chosen analyte from the sample solution or matrix while allowing the interfering background particles to be pumped out of the device. The segregated analyte is then suspended in a diluent for analysis. The device is capable of calculating an initial concentration of the analyte, as well as diluting the analyte such that reliable optical measurements can be made. Suitable analytes include cells, microorganisms, bioparticles, pathogens and diseases. Sample matrixes include biological fluids such as blood and urine, as well as environmental samples including waste water.

Self-contained high-pressure cell, apparatus, and procedure for the preparation of encapsulated proteins dissolved in low viscosity fluids for nuclear magnetic resonance spectroscopy

NASA Astrophysics Data System (ADS)

Peterson, Ronald W.; Wand, A. Joshua

2005-09-01

The design of a sample cell for high-performance nuclear magnetic resonance (NMR) at elevated pressure is described. The cell has been optimized for the study of encapsulated proteins dissolved in low viscosity fluids but is suitable for more general nuclear magnetic resonance (NMR) spectroscopy of biomolecules at elevated pressure. The NMR cell is comprised of an alumina-toughened zirconia tube mounted on a self-sealing nonmagnetic metallic valve. The cell has several advantages, including relatively low cost, excellent NMR performance, high-pressure tolerance, chemical inertness, and a relatively large active volume. Also described is a low volume sample preparation device that allows for the preparation of samples under high hydrostatic pressure and their subsequent transfer to the NMR cell.

Two New Nuclear Isolation Buffers for Plant DNA Flow Cytometry: A Test with 37 Species

PubMed Central

Loureiro, João; Rodriguez, Eleazar; Doležel, Jaroslav; Santos, Conceição

2007-01-01

Background and Aims After the initial boom in the application of flow cytometry in plant sciences in the late 1980s and early 1990s, which was accompanied by development of many nuclear isolation buffers, only a few efforts were made to develop new buffer formulas. In this work, recent data on the performance of nuclear isolation buffers are utilized in order to develop new buffers, general purpose buffer (GPB) and woody plant buffer (WPB), for plant DNA flow cytometry. Methods GPB and WPB were used to prepare samples for flow cytometric analysis of nuclear DNA content in a set of 37 plant species that included herbaceous and woody taxa with leaf tissues differing in structure and chemical composition. The following parameters of isolated nuclei were assessed: forward and side light scatter, propidium iodide fluorescence, coefficient of variation of DNA peaks, quantity of debris background, and the number of particles released from sample tissue. The nuclear genome size of 30 selected species was also estimated using the buffer that performed better for a given species. Key Results In unproblematic species, the use of both buffers resulted in high quality samples. The analysis of samples obtained with GPB usually resulted in histograms of DNA content with higher or similar resolution than those prepared with the WPB. In more recalcitrant tissues, such as those from woody plants, WPB performed better and GPB failed to provide acceptable results in some cases. Improved resolution of DNA content histograms in comparison with previously published buffers was achieved in most of the species analysed. Conclusions WPB is a reliable buffer which is also suitable for the analysis of problematic tissues/species. Although GPB failed with some plant species, it provided high-quality DNA histograms in species from which nuclear suspensions are easy to prepare. The results indicate that even with a broad range of species, either GPB or WPB is suitable for preparation of high-quality suspensions of intact nuclei suitable for DNA flow cytometry. PMID:17684025

Preparation of a standardised faecal slurry for ex-vivo microbiota studies which reduces inter-individual donor bias.

PubMed

O'Donnell, Michelle M; Rea, Mary C; O'Sullivan, Órla; Flynn, Cal; Jones, Beth; McQuaid, Albert; Shanahan, Fergus; Ross, R Paul

2016-10-01

In-vitro gut fermentation systems provide suitable models for studying gut microbiota composition and functionality. However, such methods depend on the availability of donors and the assumption of reproducibility between microbial communities before experimental treatments commence. The aim of this study was to develop a frozen standardised inoculum (FSI) which minimizes inter-individual variation and to determine its stability over time using culture-dependent and culture-independent techniques. A method for the preparation difference of a FSI is described which involves pooling the faecal samples, centrifugation and pelleting of the cell biomass and finally homogenising the cell pellets with phosphate buffer and glycerol. Using this approach, no significant difference in total anaerobe cell viability was observed between the fresh standardised inoculum (before freezing) and the 12days post freezing FSI. Moreover, Quantitative PCR revealed no significant alterations in the estimated bacterial numbers in the FSI preparations for any of the phyla. MiSeq sequencing revealed minute differences in the relative abundance at phylum, family and genus levels between the FSI preparations. Differences in the microbiota denoted as significant were limited between preparations in the majority of cases to changes in percentage relative abundance of ±0.5%. The independently prepared FSIs revealed a high degree of reproducibility in terms of microbial composition between the three preparations. This study provides a method to produce a standardised human faecal inoculum suitable for freezing. Based on culture-dependent and independent analysis, the method ensures a degree of reproducibility between preparations by lessening the effect of inter-individual variation among the donors, thereby making the system more suitable for the accurate interpretation of the effects of experimental treatments. Copyright © 2016 Elsevier B.V. All rights reserved.

Security writing application of thermal decomposition assisted NaYF4:Er3+/Yb3+ upconversion phosphor

NASA Astrophysics Data System (ADS)

Kumar, A.; Tiwari, S. P.; Esteves da Silva, Joaquim C. G.; Kumar, K.

2018-07-01

The authors have synthesized water-dispersible NaYF4:Er3+/Yb3+ upconversion particles via a thermal decomposition route and optimized the green upconversion emission through a concentration variation of the Yb3+ sensitizer. The prepared particles were found to be ellipsoid in shape having an average particle dimension of 600  ×  150 nm. It is observed that the sample with 18 mmol% Yb3+ ion concentration and 2 mmol% Er3+ ion gives optimum upconversion intensity in the green region under 980 nm excitation. Colloidal dispersibility of the sample in different solvents was checked and hexane was found to be the best medium for the prepared particles. The particle size of the sample was found to be suitable for the preparation of colloidal ink and security writing on a plain sheet of paper. This was demonstrated successfully using ink prepared in polyvinyl chloride gold medium.

Improved thermoelectric properties of Bi2Te3-xSex alloys by melt spinning and resistance pressing sintering

NASA Astrophysics Data System (ADS)

Cai, Xinzhi; Fan, Xi'an; Rong, Zhenzhou; Yang, Fan; Gan, Zhanghua; Li, Guangqiang

2014-03-01

Starting from bismuth, tellurium and selenium chunks, n-type Bi2Te3-xSex (x ⩽ 0.3) alloys were obtained by melt spinning (MS) combined with a resistance pressing sintering (RPS) process. The phases, microstructures and compositions of the samples were evaluated by x-ray diffraction, field emission scanning electron microscopy, and energy dispersive x-ray spectroscopy during each step in the preparation process, respectively. The influences of Se doping, MS and RPS processes on the thermoelectric (TE) properties of Bi2Te3-xSex alloys were investigated in detail. The Bi2Te3-xSex powders could be well compacted by the RPS process and the relative densities of the bulks prepared by RPS were all higher than 96%. The partially oriented lamellar structure could be observed at some regions of the samples prepared by RPS, and the monolayer thickness of the lamellar structure in the MS-RPS samples was smaller than that in the smelting-RPS sample. The MS process was confirmed as an excellent method to obtain fine microstructures and low lattice thermal conductivity for the TE materials. All evidence about electrical and thermal transport properties suggested that suitably increasing the Se content could effectively improve the ZT value. The maximum ZT value of 0.84 was obtained for the Bi2Te2.7Se0.3 prepared by MS-RPS at 423 K. As opposed to the conventional hot pressing and spark plasma sintering, the RPS method introduced here is more suitable for practical industrial application due to its cost saving and high efficiency.

Determination of ruthenium in pharmaceutical compounds by graphite furnace atomic absorption spectroscopy.

PubMed

Jia, Xiujuan; Wang, Tiebang; Bu, Xiaodong; Tu, Qiang; Spencer, Sandra

2006-04-11

A graphite furnace atomic absorption (GFAA) spectrometric method for the determination of ruthenium (Rh) in solid and liquid pharmaceutical compounds has been developed. Samples are dissolved or diluted in dimethyl sulfoxide (DMSO) without any other treatment before they were analyzed by GFAA with a carefully designed heating program to avoid pre-atomization signal loss and to achieve suitable sensitivity. Various inorganic and organic solvents were tested and compared and DMSO was found to be the most suitable. In addition, ruthenium was found to be stable in DMSO for at least 5 days. Spike recoveries ranged from 81 to 100% and the limit of quantitation (LOQ) was determined to be 0.5 microg g(-1) for solid samples or 0.005 microg ml(-1) for liquid samples based a 100-fold dilution. The same set of samples was also analyzed by ICP-MS with a different sample preparation method, and excellent agreement was achieved.

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.

New Methods of Sample Preparation for Atom Probe Specimens

NASA Technical Reports Server (NTRS)

Kuhlman, Kimberly, R.; Kowalczyk, Robert S.; Ward, Jennifer R.; Wishard, James L.; Martens, Richard L.; Kelly, Thomas F.

2003-01-01

Magnetite is a common conductive mineral found on Earth and Mars. Disk-shaped precipitates approximately 40 nm in diameter have been shown to have manganese and aluminum concentrations. Atom-probe field-ion microscopy (APFIM) is the only technique that can potentially quantify the composition of these precipitates. APFIM will be used to characterize geological and planetary materials, analyze samples of interest for geomicrobiology; and, for the metrology of nanoscale instrumentation. Prior to APFIM sample preparation was conducted by electropolishing, the method of sharp shards (MSS), or Bosch process (deep reactive ion etching) with focused ion beam (FIB) milling as a final step. However, new methods are required for difficult samples. Many materials are not easily fabricated using electropolishing, MSS, or the Bosch process, FIB milling is slow and expensive, and wet chemistry and the reactive ion etching are typically limited to Si and other semiconductors. APFIM sample preparation using the dicing saw is commonly used to section semiconductor wafers into individual devices following manufacture. The dicing saw is a time-effective method for preparing high aspect ratio posts of poorly conducting materials. Femtosecond laser micromachining is also suitable for preparation of posts. FIB time required is reduced by about a factor of 10 and multi-tip specimens can easily be fabricated using the dicing saw.

Optimization and validation of a fully automated silica-coated magnetic beads purification technology in forensics.

PubMed

Nagy, M; Otremba, P; Krüger, C; Bergner-Greiner, S; Anders, P; Henske, B; Prinz, M; Roewer, L

2005-08-11

Automated procedures for forensic DNA analyses are essential not only for large-throughput sample preparation, but are also needed to avoid errors during routine sample preparation. The most critical stage in PCR-based forensic analysis is DNA isolation, which should yield as much highly purified DNA as possible. The extraction method used consists of pre-treatment of stains and samples, cell lysis using chaotropic reagents, binding of the DNA to silica-coated magnetic particles, followed by elution of the DNA. Our work focuses mainly on sample preparation, obtaining the maximum possible amount of biological material from forensic samples, and the following cell lysis, to create a simple standardized lysis protocol suitable for nearly all forensic material. After optimization and validation, the M-48 BioRobot((R)) workstation has been used for more than 20,000 routine lab samples. There has been no evidence of cross contamination. Resulting DNA from as small as three nuclear cells yield reliable complete STR amplification profiles. The DNA remains stable after 2 years of storage.

Ultra fine grained Ti prepared by severe plastic deformation

NASA Astrophysics Data System (ADS)

Lukáč, F.; Čížek, J.; Knapp, J.; Procházka, I.; Zháňal, P.; Islamgaliev, R. K.

2016-01-01

The positron annihilation spectroscopy was employed for characterisation of defects in pure Ti with ultra fine grained (UFG) structure. UFG Ti samples were prepared by two techniques based on severe plastic deformation (SPD): (i) high pressure torsion (HPT) and (ii) equal channel angular pressing (ECAP). Although HPT is the most efficient technique for grain refinement, the size of HPT-deformed specimens is limited. On the other hand, ECAP is less efficient in grain refinement but enables to produce larger samples more suitable for industrial applications. Characterisation of defects by positron annihilation spectroscopy was accompanied by hardness testing in order to monitor the development of mechanical properties of UFG Ti.

Graphene quantum dots, graphene oxide, carbon quantum dots and graphite nanocrystals in coals

NASA Astrophysics Data System (ADS)

Dong, Yongqiang; Lin, Jianpeng; Chen, Yingmei; Fu, Fengfu; Chi, Yuwu; Chen, Guonan

2014-06-01

Six coal samples of different ranks have been used to prepare single-layer graphene quantum dots (S-GQDs). After chemical oxidation and a series of centrifugation separation, every coal could be treated into two fractions, namely, CoalA and CoalB. According to the characterization results of TEM, AFM, XRD, Raman and FTIR, CoalA was revealed to be mainly composed of S-GQDs, which have an average height of about 0.5 nm and an average plane dimension of about 10 nm. The obtained S-GQDs showed excitation-dependent fluorescence and excellent electrochemiluminescence. CoalB was found to be some other carbon-based nanomaterials (CNMs), including agglomerated GQDs, graphene oxide, carbon quantum dots and agglomerated carbon nanocrystals. Generally, low-ranked coals might be more suitable for the preparation of S-GQDs. The production yield of S-GQDs from the six investigated coals decreased from 56.30% to 14.66% when the coal rank increased gradually. In contrast, high-ranked coals had high production yield of CoalB and might be more suitable for preparing other CNMs that were contained in CoalB, although those CNMs were difficult to separate from each other in our experiment.Six coal samples of different ranks have been used to prepare single-layer graphene quantum dots (S-GQDs). After chemical oxidation and a series of centrifugation separation, every coal could be treated into two fractions, namely, CoalA and CoalB. According to the characterization results of TEM, AFM, XRD, Raman and FTIR, CoalA was revealed to be mainly composed of S-GQDs, which have an average height of about 0.5 nm and an average plane dimension of about 10 nm. The obtained S-GQDs showed excitation-dependent fluorescence and excellent electrochemiluminescence. CoalB was found to be some other carbon-based nanomaterials (CNMs), including agglomerated GQDs, graphene oxide, carbon quantum dots and agglomerated carbon nanocrystals. Generally, low-ranked coals might be more suitable for the preparation of S-GQDs. The production yield of S-GQDs from the six investigated coals decreased from 56.30% to 14.66% when the coal rank increased gradually. In contrast, high-ranked coals had high production yield of CoalB and might be more suitable for preparing other CNMs that were contained in CoalB, although those CNMs were difficult to separate from each other in our experiment. Electronic supplementary information (ESI) available: Elemental analysis results of coal samples, FTIR spectra of CoalA and CoalB, ECL responses of CoalA/S2O82-. See DOI: 10.1039/c4nr01482k

The planning and establishment of a sample preparation laboratory for drug discovery

PubMed Central

Dufresne, Claude

2000-01-01

Nature has always been a productive source of new drugs. With the advent of high-throughput screening, it has now become possible to rapidly screen large sample collections. In addition to seeking greater diversity from natural product sources (micro-organisms, plants, etc.), fractionation of the crude extracts prior to screening is becoming a more important part of our efforts. As sample preparation protocols become more involved, automation can help to achieve and maintain a desired sample throughput. To address the needs of our screening program, two robotic systems were designed. The first system processes crude extracts all the way to 96-well plates, containing solutions suitable for screening in biological and biochemical assays. The system can dissolve crude extracts, fractionate them on solid-phase extraction cartridges, dry and weigh each fraction, re-dissolve them to a known concentration, and prepare mother plates. The second system replicates mother plates into a number of daughter plates. PMID:18924691

21 CFR 606.122 - Instruction circular.

Code of Federal Regulations, 2012 CFR

2012-04-01

...: (1) Instructions to administer a suitable plasma volume expander if Red Blood Cells are substituted... approximate volume of plasma from which a sample unit of Platelets is prepared. (2) Instructions to begin administration as soon as possible, but not more than 4 hours after entering the container. (m) For Plasma, the...

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.

The Laser Ablation Ion Funnel: Sampling for in situ Mass Spectrometry on Mars

NASA Technical Reports Server (NTRS)

Johnson, Paul V.; Hodyss, Robert; Tang, Keqi; Brinckerhoff, William B.; Smith, Richard D.

2011-01-01

A considerable investment has been made by NASA and other space agencies to develop instrumentation suitable for in situ analytical investigation of extra terrestrial bodies including various mass spectrometers (time-of-flight, quadrupole ion trap, quadrupole mass filters, etc.). However, the front-end sample handling that is needed to collect and prepare samples for interrogation by such instrumentation remains underdeveloped. Here we describe a novel approach tailored to the exploration of Mars where ions are created in the ambient atmosphere via laser ablation and then efficiently transported into a mass spectrometer for in situ analysis using an electrodynamic ion funnel. This concept would enable elemental and isotopic analysis of geological samples with the analysis of desorbed organic material a possibility as well. Such an instrument would be suitable for inclusion on all potential missions currently being considered such as the Mid-Range Rover, the Astrobiology Field Laboratory, and Mars Sample Return (i.e., as a sample pre-selection triage instrument), among others.

Nucleation of biomimetic apatite in synthetic body fluids: dense and porous scaffold development.

PubMed

Landi, Elena; Tampieri, Anna; Celotti, Giancarlo; Langenati, Ratih; Sandri, Monica; Sprio, Simone

2005-06-01

The effectiveness of synthetic body fluids (SBF) as biomimetic sources to synthesize carbonated hydroxyapatite (CHA) powder similar to the biological inorganic phase, in terms of composition and microstructure, was investigated. CHA apatite powders were prepared following two widely experimented routes: (1) calcium nitrate tetrahydrate and diammonium hydrogen phosphate and (2) calcium hydroxide and ortophosphoric acid, but using SBF as synthesis medium instead of pure water. The characteristics of the as-prepared powders were compared, also with the features of apatite powders synthesized via pure water-based classical methods. The powder thermal resistance and behaviour during densification were studied together with the mechanical properties of the dense samples. The sponge impregnation process was used to prepare porous samples having morphological and mechanical characteristics suitable for bone substitution. Using this novel synthesis was it possible to prepare nanosized (approximately equal to 20 nm), pure, carbonate apatite powder containing Mg, Na, K ions, with morphological and compositional features mimicking natural apatite and with improved thermal properties. After sintering at 1250 degrees C the carbonate-free apatite porous samples showed a surprising, high compressive strength together with a biomimetic morphology.

Establishment of the first international standard for PEGylated granulocyte colony stimulating factor (PEG-G-CSF): Report of an international collaborative study

PubMed Central

Wadhwa, Meenu; Bird, Chris; Dougall, Thomas; Rigsby, Peter; Bristow, Adrian; Thorpe, Robin

2015-01-01

We assessed the feasibility of developing a suitable international reference standard for determination of in vitro biological activity of human sequence recombinant PEG-G-CSF products with a 20 kD linear PEG linked to the N-terminal methionyl residue of G-CSF (INN Filgrastim), produced using a conjugation process and coupling chemistry similar to that employed for the lead PEGfilgrastim product. Based on initial data which showed that the current WHO 2nd international standard, IS for G-CSF (09/136) or alternatively, a PEG-G-CSF standard with a unitage traceable to the G-CSF IS may potentially serve as the IS for PEG-G-CSF products, two candidate preparations of PEG-G-CSF were formulated and lyophilized at NIBSC. These preparations were tested by 23 laboratories using in vitro bioassays in a multi-centre collaborative study. Results indicated that on the basis of parallelism, the current WHO 2nd IS for G-CSF or any of the PEG-G-CSF samples could be used as the international standard for PEG-G-CSF preparations. However, because of the variability in potency estimates seen when PEG-G-CSF preparations were compared with the current WHO 2nd IS for G-CSF, a candidate PEG-G-CSF was suitable as the WHO IS. The preparation 12/188 was judged suitable to serve as the WHO IS based on in vitro biological activity data. Therefore, the preparation coded 12/188 was established by the WHO Expert Committee on Biological Standardization (ECBS) in 2013 as the WHO 1st IS for human PEGylated G-CSF with an assigned in vitro bioactivity of 10,000 IU per ampoule. PMID:25450254

Analysis of the silicone polymer surface aging profile with laser-induced breakdown spectroscopy

NASA Astrophysics Data System (ADS)

Wang, Xilin; Hong, Xiao; Wang, Han; Chen, Can; Zhao, Chenlong; Jia, Zhidong; Wang, Liming; Zou, Lin

2017-10-01

Silicone rubber composite materials have been widely used in high voltage transmission lines for anti-pollution flashover. The aging surface of silicone rubber materials decreases service properties, causing loss of the anti-pollution ability. In this paper, as an analysis method requiring no sample preparation that is able to be conducted on site and suitable for nearly all types of materials, laser-induced breakdown spectroscopy (LIBS) was used for the analysis of newly prepared and aging (out of service) silicone rubber composites. With scanning electron microscopy (SEM) and hydrophobicity test, LIBS was proven to be nearly non-destructive for silicone rubber. Under the same LIBS testing parameters, a linear relationship was observed between ablation depth and laser pulses number. With the emission spectra, all types of elements and their distribution in samples along the depth direction from the surface to the inner part were acquired and verified with EDS results. This research showed that LIBS was suitable to detect the aging layer depth and element distribution of the silicone rubber surface.

M3FT-17OR0301070211 - Preparation of Hot Isostatically Pressed AgZ Waste Form Samples

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

Jubin, Robert Thomas; Bruffey, Stephanie H.; Jordan, Jacob A.

The production of radioactive iodine-bearing waste forms that exhibit long-term stability and are suitable for permanent geologic disposal has been the subject of substantial research interest. One potential method of iodine waste form production is hot isostatic pressing (HIP). Recent studies at Oak Ridge National Laboratory (ORNL) have investigated the conversion of iodine-loaded silver mordenite (I-AgZ) directly to a waste form by HIP. ORNL has performed HIP with a variety of sample compositions and pressing conditions. The base mineral has varied among AgZ (in pure and engineered forms), silver-exchanged faujasite, and silverexchanged zeolite A. Two iodine loading methods, occlusion andmore » chemisorption, have been explored. Additionally, the effects of variations in temperature and pressure of the process have been examined, with temperature ranges of 525°C–1,100°C and pressure ranges of 100–300 MPa. All of these samples remain available to collaborators upon request. The sample preparation detailed in this document is an extension of that work. In addition to previously prepared samples, this report documents the preparation of additional samples to support stability testing. These samples include chemisorbed I-AgZ and pure AgI. Following sample preparation, each sample was processed by HIP by American Isostatic Presses Inc. and returned to ORNL for storage. ORNL will store the samples until they are requested by collaborators for durability testing. The sample set reported here will support waste form durability testing across the national laboratories and will provide insight into the effects of varied iodine content on iodine retention by the produced waste form and on potential improvements in waste form durability provided by the zeolite matrix.« less

How Confocal Is Confocal Raman Microspectroscopy on the Skin? Impact of Microscope Configuration and Sample Preparation on Penetration Depth Profiles.

PubMed

Lunter, Dominique Jasmin

2016-01-01

The aim of the study was to elucidate the effect of sample preparation and microscope configuration on the results of confocal Raman microspectroscopic evaluation of the penetration of a pharmaceutical active into the skin (depth profiling). Pig ear skin and a hydrophilic formulation containing procaine HCl were used as a model system. The formulation was either left on the skin during the measurement, or was wiped off or washed off prior to the analysis. The microscope configuration was varied with respect to objectives and pinholes used. Sample preparation and microscope configuration had a tremendous effect on the results of depth profiling. Regarding sample preparation, the best results could be observed when the formulation was washed off the skin prior to the analysis. Concerning microscope configuration, the use of a 40 × 0.6 numerical aperture (NA) objective in combination with a 25-µm pinhole or a 100 × 1.25 NA objective in combination with a 50-µm pinhole was found to be advantageous. Complete removal of the sample from the skin before the analysis was found to be crucial. A thorough analysis of the suitability of the chosen microscope configuration should be performed before acquiring concentration depth profiles. © 2016 S. Karger AG, Basel.

Physical pretreatment of biogenic-rich trommel fines for fast pyrolysis.

PubMed

Eke, Joseph; Onwudili, Jude A; Bridgwater, Anthony V

2017-12-01

Energy from Waste (EfW) technologies such as fluidized bed fast pyrolysis, are beneficial for both energy generation and waste management. Such technologies, however face significant challenges due to the heterogeneous nature, particularly the high ash contents of some municipal solid waste types e.g. trommel fines. A study of the physical/mechanical and thermal characteristics of these complex wastes is important for two main reasons; (a) to inform the design and operation of pyrolysis systems to handle the characteristics of such waste; (b) to control/modify the characteristics of the waste to fit with existing EFW technologies via appropriate feedstock preparation methods. In this study, the preparation and detailed characterisation of a sample of biogenic-rich trommel fines has been carried out with a view to making the feedstock suitable for fast pyrolysis based on an existing fluidized bed reactor. Results indicate that control of feed particle size was very important to prevent problems of dust entrainment in the fluidizing gas as well as to prevent feeder hardware problems caused by large stones and aggregates. After physical separation and size reduction, nearly 70wt% of the trommel fines was obtained within the size range suitable for energy recovery using the existing fast pyrolysis system. This pyrolyzable fraction could account for about 83% of the energy content of the 'as received' trommel fines sample. Therefore there was no significant differences in the thermochemical properties of the raw and pre-treated feedstocks, indicating that suitably prepared trommel fines samples can be used for energy recovery, with significant reduction in mass and volume of the original waste. Consequently, this can lead to more than 90% reduction in the present costs of disposal of trommel fines in landfills. In addition, the recovered plastics and textile materials could be used as refuse derived fuel. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effect of Sintering Temperature on Structural, Dielectric, and Magnetic Properties of Multiferroic YFeO₃ Ceramics Fabricated by Spark Plasma Sintering.

PubMed

Wang, Meng; Wang, Ting; Song, Shenhua; Ma, Qing; Liu, Renchen

2017-03-07

Based on precursor powders with a size of 200-300 nm prepared by the low-temperature solid reaction method, phase-pure YFeO₃ ceramics are fabricated using spark plasma sintering (SPS) at different temperatures. X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YFeO₃ ceramics can be prepared using SPS, while the results from X-ray photoelectron spectroscopy (XPS) show that the concentration of oxygen vacancies resulting from transformation from Fe 3+ to Fe 2+ is low. The relative density of the 1000 °C-sintered sample is as high as 97.7%, which is much higher than those of the samples sintered at other temperatures. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods. These findings indicate that the YFeO₃ ceramics prepared by the low temperature solid reaction and SPS methods possess excellent dielectric and magnetic properties, making them suitable for potential applications involving magnetic storage.

Evaluation of specimen preparation techniques for micro-PIXE localisation of elements in hyperaccumulating plants

NASA Astrophysics Data System (ADS)

Kachenko, Anthony G.; Siegele, Rainer; Bhatia, Naveen P.; Singh, Balwant; Ionescu, Mihail

2008-04-01

Hybanthus floribundus subsp. floribundus, a rare Australian Ni-hyperaccumulating shrub and Pityrogramma calomelanos var. austroamericana, an Australian naturalized As-hyperaccumulating fern are promising species for use in phytoremediation of contaminated sites. Micro-proton-induced X-ray emission (μ-PIXE) spectroscopy was used to map the elemental distribution of the accumulated metal(loid)s, Ca and K in leaf or pinnule tissues of the two plant species. Samples were prepared by two contrasting specimen preparation techniques: freeze-substitution in tetrahydrofuran (THF) and freeze-drying. The specimens were analysed to compare the suitability of each technique in preserving (i) the spatial elemental distribution and (ii) the tissue structure of the specimens. Further, the μ-PIXE results were compared with concentration of elements in the bulk tissue obtained by ICP-AES analysis. In H. floribundus subsp. floribundus, μ-PIXE analysis revealed Ni, Ca and K concentrations in freeze-dried leaf tissues were at par with bulk tissue concentrations. Elemental distribution maps illustrated that Ni was preferentially localised in the adaxial epidermal tissues (1% DW) and least concentration was found in spongy mesophyll tissues (0.53% DW). Conversely, elemental distribution maps of THF freeze-substituted tissues indicated significantly lower Ni, Ca and K concentrations than freeze-dried specimens and bulk tissue concentrations. Moreover, Ni concentrations were uniform across the whole specimen and no localisation was observed. In P. calomelanos var. austroamericana freeze-dried pinnule tissues, μ-PIXE revealed statistically similar As, Ca and K concentrations as compared to bulk tissue concentrations. Elemental distribution maps showed that As localisation was relatively uniform across the whole specimen. Once again, THF freeze-substituted tissues revealed a significant loss of As compared to freeze-dried specimens and the concentrations obtained by bulk tissue analysis. The results demonstrate that freeze-drying is a suitable sample preparation technique to study elemental distribution of ions in H. floribundus and P. calomelanos plant tissues using μ-PIXE spectroscopy. Furthermore, cellular structure was preserved in samples prepared using this technique.

A novel sample preparation method to avoid influence of embedding medium during nano-indentation

NASA Astrophysics Data System (ADS)

Meng, Yujie; Wang, Siqun; Cai, Zhiyong; Young, Timothy M.; Du, Guanben; Li, Yanjun

2013-02-01

The effect of the embedding medium on the nano-indentation measurements of lignocellulosic materials was investigated experimentally using nano-indentation. Both the reduced elastic modulus and the hardness of non-embedded cell walls were found to be lower than those of the embedded samples, proving that the embedding medium used for specimen preparation on cellulosic material during nano-indentation can modify cell-wall properties. This leads to structural and chemical changes in the cell-wall constituents, changes that may significantly alter the material properties. Further investigation was carried out to detect the influence of different vacuum times on the cell-wall mechanical properties during the embedding procedure. Interpretation of the statistical analysis revealed no linear relationships between vacuum time and the mechanical properties of cell walls. The quantitative measurements confirm that low-viscosity resin has a rapid penetration rate early in the curing process. Finally, a novel sample preparation method aimed at preventing resin diffusion into lignocellulosic cell walls was developed using a plastic film to wrap the sample before embedding. This method proved to be accessible and straightforward for many kinds of lignocellulosic material, but is especially suitable for small, soft samples.

[Determination of LF-VD refining furnace slag by X ray fluorescence spectrometry].

PubMed

Kan, Bin; Cheng, Jian-ping; Song, Zu-feng

2004-10-01

Eight components, i.e. TFe, CaO, MgO, Al2O3, SiO2, TiO2, MnO and P2O5 in refining furnace slag were determined by X ray fluorescence spectrometer. Because the content of CaO was high, the authors selected 12 national and departmental grade slag standard samples and prepared a series of synthetic standard samples by adding spectrally pure reagents to them. The calibration curve is suitable to the sample analysis of CaO, MgO and SiO2 with widely varying range. Meanwhile, the points on the curve are even. The samples were prepared at high temperature by adding Li2B4O7 as flux. The experiments for the selection of the sample preparation conditions about strip reagents, melting temperature and dulition ratio were carried out. The matrix effects on absorption and enhancement were corrected by means of PH model and theoretical alpha coefficient. Moreover, the precision and accuracy experiments were performed. In comparison with chemical analysis method, the quantitative analytical results for each component are satisfactory. The method has proven rapid, precise and simple.

Total Arsenic, Cadmium, and Lead Determination in Brazilian Rice Samples Using ICP-MS

PubMed Central

Buzzo, Márcia Liane; de Arauz, Luciana Juncioni; Carvalho, Maria de Fátima Henriques; Arakaki, Edna Emy Kumagai; Matsuzaki, Richard; Tiglea, Paulo

2016-01-01

This study is aimed at investigating a suitable method for rice sample preparation as well as validating and applying the method for monitoring the concentration of total arsenic, cadmium, and lead in rice by using Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Various rice sample preparation procedures were evaluated. The analytical method was validated by measuring several parameters including limit of detection (LOD), limit of quantification (LOQ), linearity, relative bias, and repeatability. Regarding the sample preparation, recoveries of spiked samples were within the acceptable range from 89.3 to 98.2% for muffle furnace, 94.2 to 103.3% for heating block, 81.0 to 115.0% for hot plate, and 92.8 to 108.2% for microwave. Validation parameters showed that the method fits for its purpose, being the total arsenic, cadmium, and lead within the Brazilian Legislation limits. The method was applied for analyzing 37 rice samples (including polished, brown, and parboiled), consumed by the Brazilian population. The total arsenic, cadmium, and lead contents were lower than the established legislative values, except for total arsenic in one brown rice sample. This study indicated the need to establish monitoring programs for emphasizing the study on this type of cereal, aiming at promoting the Public Health. PMID:27766178

Nanostructured giant magneto-impedance multilayers deposited onto flexible substrates for low pressure sensing

PubMed Central

2012-01-01

Nanostructured FeNi-based multilayers are very suitable for use as magnetic sensors using the giant magneto-impedance effect. New fields of application can be opened with these materials deposited onto flexible substrates. In this work, we compare the performance of samples prepared onto a rigid glass substrate and onto a cyclo olefin copolymer flexible one. Although a significant reduction of the field sensitivity is found due to the increased effect of the stresses generated during preparation, the results are still satisfactory for use as magnetic field sensors in special applications. Moreover, we take advantage of the flexible nature of the substrate to evaluate the pressure dependence of the giant magneto-impedance effect. Sensitivities up to 1 Ω/Pa are found for pressures in the range of 0 to 1 Pa, demostrating the suitability of these nanostructured materials deposited onto flexible substrates to build sensitive pressure sensors. PMID:22525096

Determination of Phenols and Trimethylamine in Industrial Effluents

NASA Technical Reports Server (NTRS)

Levaggi, D. A.; Feldstein, M.

1971-01-01

For regulatory purposes to control certain odorous compounds the analysis of phenols and trimethylamines in industrial effluents is necessary. The Bay Area Air Pollution Control District laboratory has been determining these gases by gas chromatographic techniques. The procedures for sample collection, preparation for analysis and determination are described in detail. Typical data from various sources showing the effect of proposed regulations is shown. Extensive sampling and usage of these procedures has shown them to be accurate, reliable and suitable to all types of source effluents.

Analysis of defect structure in silicon. Characterization of samples from UCP ingot 5848-13C

NASA Technical Reports Server (NTRS)

Natesh, R.; Guyer, T.; Stringfellow, G. B.

1982-01-01

Statistically significant quantitative structural imperfection measurements were made on samples from ubiquitous crystalline process (UCP) Ingot 5848 - 13 C. Important trends were noticed between the measured data, cell efficiency, and diffusion length. Grain boundary substructure appears to have an important effect on the conversion efficiency of solar cells from Semix material. Quantitative microscopy measurements give statistically significant information compared to other microanalytical techniques. A surface preparation technique to obtain proper contrast of structural defects suitable for QTM analysis was perfected.

Optimizing Illumina next-generation sequencing library preparation for extremely AT-biased genomes.

PubMed

Oyola, Samuel O; Otto, Thomas D; Gu, Yong; Maslen, Gareth; Manske, Magnus; Campino, Susana; Turner, Daniel J; Macinnis, Bronwyn; Kwiatkowski, Dominic P; Swerdlow, Harold P; Quail, Michael A

2012-01-03

Massively parallel sequencing technology is revolutionizing approaches to genomic and genetic research. Since its advent, the scale and efficiency of Next-Generation Sequencing (NGS) has rapidly improved. In spite of this success, sequencing genomes or genomic regions with extremely biased base composition is still a great challenge to the currently available NGS platforms. The genomes of some important pathogenic organisms like Plasmodium falciparum (high AT content) and Mycobacterium tuberculosis (high GC content) display extremes of base composition. The standard library preparation procedures that employ PCR amplification have been shown to cause uneven read coverage particularly across AT and GC rich regions, leading to problems in genome assembly and variation analyses. Alternative library-preparation approaches that omit PCR amplification require large quantities of starting material and hence are not suitable for small amounts of DNA/RNA such as those from clinical isolates. We have developed and optimized library-preparation procedures suitable for low quantity starting material and tolerant to extremely high AT content sequences. We have used our optimized conditions in parallel with standard methods to prepare Illumina sequencing libraries from a non-clinical and a clinical isolate (containing ~53% host contamination). By analyzing and comparing the quality of sequence data generated, we show that our optimized conditions that involve a PCR additive (TMAC), produces amplified libraries with improved coverage of extremely AT-rich regions and reduced bias toward GC neutral templates. We have developed a robust and optimized Next-Generation Sequencing library amplification method suitable for extremely AT-rich genomes. The new amplification conditions significantly reduce bias and retain the complexity of either extremes of base composition. This development will greatly benefit sequencing clinical samples that often require amplification due to low mass of DNA starting material.

Frozen tissue preparation for high-resolution multiplex histological analyses of human brain specimens.

PubMed

Shao, Fangjie; Jiang, Wenhong; Gao, Qingqing; Li, Baizhou; Sun, Chongran; Wang, Qiyuan; Chen, Qin; Sun, Bing; Shen, Hong; Zhu, Keqing; Zhang, Jianmin; Liu, Chong

2017-10-01

The availability of a comprehensive tissue library is essential for elucidating the function and pathology of human brains. Considering the irreplaceable status of the formalin-fixation-paraffin-embedding (FFPE) preparation in routine pathology and the advantage of ultra-low temperature to preserve nucleic acids and proteins for multi-omics studies, these methods have become major modalities for the construction of brain tissue libraries. Nevertheless, the use of FFPE and snap-frozen samples is limited in high-resolution histological analyses because the preparation destroys tissue integrity and/or many important cellular markers. To overcome these limitations, we detailed a protocol to prepare and analyze frozen human brain samples that is particularly suitable for high-resolution multiplex immunohistological studies. As an alternative, we offered an optimized procedure to rescue snap-frozen tissues for the same purpose. Importantly, we provided a guideline to construct libraries of frozen tissue with minimal effort, cost and space. Taking advantage of this new tissue preparation modality to nicely preserve the cellular information that was otherwise damaged using conventional methods and to effectively remove tissue autofluorescence, we described the high-resolution landscape of the cellular composition in both lower-grade gliomas and glioblastoma multiforme samples. Our work showcases the great value of fixed frozen tissue in understanding the cellular mechanisms of CNS functions and abnormalities.

One-pot template-free synthesis of porous CdMoO4 microspheres and their enhanced photocatalytic activity

NASA Astrophysics Data System (ADS)

Madhusudan, Puttaswamy; Zhang, Jinfeng; Yu, Jiaguo; Cheng, Bei; Xu, Difa; Zhang, Jun

2016-11-01

The optical and catalytic performances of materials strongly depend on their size, morphology, dimensionality and structure. Herein, we demonstrate a facile one-pot template free synthesis of hierarchical CdMoO4 porous microspheres via a simple low temperature oil bath method. The photoactivity of the as-prepared samples was evaluated by photocatalytic decolorization of Methyl Orange (MO) and Methylene Blue (MB) mixed dye aqueous solutions at ambient temperature under full solar spectrum. The results indicated that the concentration of ammonium molybdate and reaction time greatly influence the diameter, average crystallite size, specific surface area, pore structure and photocatalytic activity of the prepared samples. Especially, under the suitable conditions the prepared hierarchical CdMoO porous microspheres exhibited enhanced photocatalytic activity and high stability. Furthermore, it is found that the photocatalytic activity and formation rate of hydroxyl radicals greatly depend on the particle sizes and morphology of as-prepared samples. This work not only demonstrates a simple way to fabricate the hierarchical CdMoO4 porous microspheres but also shows a possibility for utilization of CdMoO4 porous microspheres for the photocatalytic treatment of waste water pollutants.

Next-generation sequencing library preparation method for identification of RNA viruses on the Ion Torrent Sequencing Platform.

PubMed

Chen, Guiqian; Qiu, Yuan; Zhuang, Qingye; Wang, Suchun; Wang, Tong; Chen, Jiming; Wang, Kaicheng

2018-05-09

Next generation sequencing (NGS) is a powerful tool for the characterization, discovery, and molecular identification of RNA viruses. There were multiple NGS library preparation methods published for strand-specific RNA-seq, but some methods are not suitable for identifying and characterizing RNA viruses. In this study, we report a NGS library preparation method to identify RNA viruses using the Ion Torrent PGM platform. The NGS sequencing adapters were directly inserted into the sequencing library through reverse transcription and polymerase chain reaction, without fragmentation and ligation of nucleic acids. The results show that this method is simple to perform, able to identify multiple species of RNA viruses in clinical samples.

Non-Transfusional Hemocomponents: From Biology to the Clinic-A Literature Review.

PubMed

Gasparro, Roberta; Qorri, Erda; Valletta, Alessandra; Masucci, Michele; Sammartino, Pasquale; Amato, Alessandra; Marenzi, Gaetano

2018-03-31

Non-transfusional hemocomponents for surgical use are autogenous products prepared through the centrifugation of a blood sample from a patient. Their potential beneficial outcomes include hard and soft tissue regeneration, local hemostasis, and the acceleration of wound healing. Therefore, they are suitable for application in different medical fields as therapeutic options and in surgical practices that require tissue regeneration.

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.

Sources and preparation of data for assessing trends in concentrations of pesticides in streams of the United States, 1992-2006

USGS Publications Warehouse

Martin, Jeffrey D.

2009-01-01

This report provides a water-quality data set of 44 commonly used pesticides and 8 pesticide degradates suitable for a national assessment of trends in pesticide concentrations in streams of the United States. Water-quality samples collected from January 1992 through August 2006 at stream-water sites of the U.S. Geological Survey National Water-Quality Assessment Program and the National Stream Quality Accounting Network Program were compiled, reviewed, selected, and prepared for trend analysis as described in this report. Samples analyzed at the U.S. Geological Survey National Water Quality Laboratory by a gas chromatography/mass spectrometry analytical method were the most extensive in time and space and were selected for national trend analysis. The selection criteria described in the report produced a trend data set of 16,869 pesticide samples at 201 stream and river sites.

An investigation on mechanical properties of steel fibre reinforced for underwater welded joint

NASA Astrophysics Data System (ADS)

Navin, K.; Zakaria, M. S.; Zairi, S.

2017-09-01

Underwater pipelines are always exposed to water and have a high tendency to have corrosion especially on the welded joint. This research is about using fiber glass as steel fiber to coat the welded joint to determine the effectiveness in corrosion prevention of the welded joint. Number of coating is varied to determine the better number coating to coat the pipeline. Few samples were left without immersion in salt water and few samples are immersed into salt water with same salinity as sea water. The material sample is prepared in dog bone shape to enable to be used in Universal Tensile Machine (UTM). The material prepared is left immersed for recommended time and tested in Universal Tensile Machine. Upon analyzing the result, the result is used to determine the breakage point whether broken on the welded joint or different place and also the suitable number of coating to be used.

Enhanced Multiferroic Properties of YMnO3 Ceramics Fabricated by Spark Plasma Sintering Along with Low-Temperature Solid-State Reaction

PubMed Central

Wang, Meng; Wang, Ting; Song, Shenhua; Ravi, Muchakayala; Liu, Renchen; Ji, Shishan

2017-01-01

Based on precursor powders with a size of 200–300 nm prepared by the low-temperature solid-state reaction method, phase-pure YMnO3 ceramics are fabricated using spark plasma sintering (SPS). X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YMnO3 ceramics can be prepared by SPS at 1000 °C for 5 minutes with annealing at 800 °C for 2 h. The relative density of the sample is as high as 97%, which is much higher than those of the samples sintered by other methods. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods and SPS with ball-milling precursors, and the ferroelectric loops at room temperature can be detected. These findings indicate that the YMnO3 ceramics prepared by the low temperature solid reaction method and SPS possess excellent dielectric lossy ferroelectric properties at room temperature, and magnetic properties at low temperature (10 K), making them suitable for potential multiferroic applications. PMID:28772832

Effect of Sintering Temperature on Structural, Dielectric, and Magnetic Properties of Multiferroic YFeO3 Ceramics Fabricated by Spark Plasma Sintering

PubMed Central

Wang, Meng; Wang, Ting; Song, Shenhua; Ma, Qing; Liu, Renchen

2017-01-01

Based on precursor powders with a size of 200–300 nm prepared by the low-temperature solid reaction method, phase-pure YFeO3 ceramics are fabricated using spark plasma sintering (SPS) at different temperatures. X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YFeO3 ceramics can be prepared using SPS, while the results from X-ray photoelectron spectroscopy (XPS) show that the concentration of oxygen vacancies resulting from transformation from Fe3+ to Fe2+ is low. The relative density of the 1000 °C-sintered sample is as high as 97.7%, which is much higher than those of the samples sintered at other temperatures. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods. These findings indicate that the YFeO3 ceramics prepared by the low temperature solid reaction and SPS methods possess excellent dielectric and magnetic properties, making them suitable for potential applications involving magnetic storage. PMID:28772626

A guide to large-scale RNA sample preparation.

PubMed

Baronti, Lorenzo; Karlsson, Hampus; Marušič, Maja; Petzold, Katja

2018-05-01

RNA is becoming more important as an increasing number of functions, both regulatory and enzymatic, are being discovered on a daily basis. As the RNA boom has just begun, most techniques are still in development and changes occur frequently. To understand RNA functions, revealing the structure of RNA is of utmost importance, which requires sample preparation. We review the latest methods to produce and purify a variation of RNA molecules for different purposes with the main focus on structural biology and biophysics. We present a guide aimed at identifying the most suitable method for your RNA and your biological question and highlighting the advantages of different methods. Graphical abstract In this review we present different methods for large-scale production and purification of RNAs for structural and biophysical studies.

The effects of crosslinkers on physical, mechanical, and cytotoxic properties of gelatin sponge prepared via in-situ gas foaming method as a tissue engineering scaffold.

PubMed

Poursamar, S Ali; Lehner, Alexander N; Azami, Mahmoud; Ebrahimi-Barough, Somayeh; Samadikuchaksaraei, Ali; Antunes, A P M

2016-06-01

In this study porous gelatin scaffolds were prepared using in-situ gas foaming, and four crosslinking agents were used to determine a biocompatible and effective crosslinker that is suitable for such a method. Crosslinkers used in this study included: hexamethylene diisocyanate (HMDI), poly(ethylene glycol) diglycidyl ether (epoxy), glutaraldehyde (GTA), and genipin. The prepared porous structures were analyzed using Fourier Transform Infrared Spectroscopy (FT-IR), thermal and mechanical analysis as well as water absorption analysis. The microstructures of the prepared samples were analyzed using Scanning Electron Microscopy (SEM). The effects of the crosslinking agents were studied on the cytotoxicity of the porous structure indirectly using MTT analysis. The affinity of L929 mouse fibroblast cells for attachment on the scaffold surfaces was investigated by direct cell seeding and DAPI-staining technique. It was shown that while all of the studied crosslinking agents were capable of stabilizing prepared gelatin scaffolds, there are noticeable differences among physical and mechanical properties of samples based on the crosslinker type. Epoxy-crosslinked scaffolds showed a higher capacity for water absorption and more uniform microstructures than the rest of crosslinked samples, whereas genipin and GTA-crosslinked scaffolds demonstrated higher mechanical strength. Cytotoxicity analysis showed the superior biocompatibility of the naturally occurring genipin in comparison with other synthetic crosslinking agents, in particular relative to GTA-crosslinked samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Influence of the sintering temperature on the electrical properties of Ce-doped WO3 ceramics prepared from nano-powders

NASA Astrophysics Data System (ADS)

Dong, Liang; Chen, Han-Jun; Wang, Yu; Li, De-Zhu; Li, Tong-Ye; Zhao, Yong

2007-04-01

Using a nm-level powder fabricated by a wet chemical method as precursor, the CeO2-doped WO3 ceramics were prepared by the conventional solid state reaction at sintering temperatures from 600 to 1100 °C. The x-ray diffraction analysis reveals the coexistence of different WO3 phases in the samples sintered at temperatures below 900 °C, whereas a single phase appears in the samples sintered above 1000 °C. No new Ce-W compound appears. As the sintering temperature increases, the electrical properties of the samples display an interesting transformation from linear to nonlinear behaviour. The measurements of scanning electron microscope, complex impedance and electrical stability indicate that a lot of grain boundary regions in the samples sintered at low temperatures strongly influences the electrical transportation. Therefore, the electrical nonlinearity is due to a basic process controlled by the back-to-back Schottky barriers at grain boundaries with suitable thickness as well as the coexistence of phases.

Effect of variable cerium concentration on photoluminescence behaviour in ZrO2 phosphor synthesized by combustion synthesis method

NASA Astrophysics Data System (ADS)

Dubey, Vikas; Kaur, Jagjeet

2016-05-01

Present paper reports synthesis and characterization of trivalent cerium (Ce3+) doped zirconium dioxide (ZrO2) phosphors. Effect of variable concentration of cerium on photoluminescence (PL) is studied. Samples were prepared by combustion synthesis technique which is suitable for less time taking techniques also for large scale production for phosphors. Starting material used for sample preparation are Zr(NO3)3 and Ce(NO3)3 and urea used as a fuel. All prepared phosphor with variable concentration of Ce3+ (0.1 to 2mol%) was studied by photoluminescence analysis it is found that the excitation spectra of prepared phosphor shows broad excitation centred at 390nm. The excitation spectra with variable concentration of Ce3+ show strong peaks at 447nm. Spectrophotometric determinations of peaks are evaluated by Commission Internationale de I'Eclairage technique. Using this phosphor, the desired CIE values including emissions throughout the violet (390 nm) and blue (427 nm) of the spectra were achieved. Efficient blue light emitting diodes were fabricated using Ce3+ doped phosphor based on near ultraviolet (NUV) excited LED lights.

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

Dubey, Vikas, E-mail: jsvikasdubey@gmail.com; Kaur, Jagjeet

Present paper reports synthesis and characterization of trivalent cerium (Ce{sup 3+}) doped zirconium dioxide (ZrO{sub 2}) phosphors. Effect of variable concentration of cerium on photoluminescence (PL) is studied. Samples were prepared by combustion synthesis technique which is suitable for less time taking techniques also for large scale production for phosphors. Starting material used for sample preparation are Zr(NO{sub 3}){sub 3} and Ce(NO{sub 3}){sub 3} and urea used as a fuel. All prepared phosphor with variable concentration of Ce{sup 3+} (0.1 to 2mol%) was studied by photoluminescence analysis it is found that the excitation spectra of prepared phosphor shows broad excitationmore » centred at 390nm. The excitation spectra with variable concentration of Ce{sup 3+} show strong peaks at 447nm. Spectrophotometric determinations of peaks are evaluated by Commission Internationale de I’Eclairage technique. Using this phosphor, the desired CIE values including emissions throughout the violet (390 nm) and blue (427 nm) of the spectra were achieved. Efficient blue light emitting diodes were fabricated using Ce{sup 3+} doped phosphor based on near ultraviolet (NUV) excited LED lights.« less

Standardized cell samples for midIR technology development

NASA Astrophysics Data System (ADS)

Kastl, Lena; Rommel, Christina E.; Kemper, Björn; Schnekenburger, Jürgen

2015-03-01

The application of midIR spectroscopy towards human cell and tissue samples is impaired by the need for technical solutions and lacking sample standards for technology development. We here present the standardization of stable test samples for the continuous development and testing of novel optical system components. We have selected cell lines representing the major cellular skin constituents keratinocytes and fibroblasts (NIH-3T3, HaCaT). In addition, two skin cancer cell types (A-375 and SK-MEL-28 cells) were analyzed. Cells were seeded on CaF2 substrates and measured dried and under aqueous medium as well as fixated and unfixated. Several independent cell preparations were analyzed with an FTIR spectrometer in the wave number range from 1000 - 4000 cm-1. The obtained data demonstrate that fixed and dehydrated cells on CaF2 can be stored in pure ethanol for several weeks without significant losses in quality of the spectral properties. The established protocol of cell seeding on CaF2 substrates, chemical fixation, dehydration, storage under ethanol and air-drying is suitable for the production of reliable midIR standards. The retrieved spectra demonstrate that fixed cells on CaF2 can be prepared reproducibly; with stable midIR spectral properties over several weeks and properties mimicking reliable unfixed cells. Moreover, the fixated samples on CaF2 show clear differences in the cell type specific spectra that can be identified by principle component analysis. In summary, the standardized cell culture samples on CaF2 substrates are suitable for the development of a midIR device and the optimization of the specific midIR spectra.

Microarray-based comparison of three amplification methods for nanogram amounts of total RNA

PubMed Central

Singh, Ruchira; Maganti, Rajanikanth J.; Jabba, Sairam V.; Wang, Martin; Deng, Glenn; Heath, Joe Don; Kurn, Nurith; Wangemann, Philine

2007-01-01

Gene expression profiling using microarrays requires microgram amounts of RNA, which limits its direct application for the study of nanogram RNA samples obtained using microdissection, laser capture microscopy, or needle biopsy. A novel system based on Ribo-SPIA technology (RS, Ovation-Biotin amplification and labeling system) was recently introduced. The utility of the RS system, an optimized prototype system for picogram RNA samples (pRS), and two T7-based systems involving one or two rounds of amplification (OneRA, Standard Protocol, or TwoRA, Small Sample Prototcol, version II) were evaluated in the present study. Mouse kidney (MK) and mouse universal reference (MUR) RNA samples, 0.3 ng to 10 μg, were analyzed using high-density Affymetrix Mouse Genome 430 2.0 GeneChip arrays. Call concordance between replicates, correlations of signal intensity, signal intensity ratios, and minimal fold increase necessary for significance were determined. All systems amplified partially overlapping sets of genes with similar signal intensity correlations. pRS amplified the highest number of genes from 10-ng RNA samples. We detected 24 of 26 genes verified by RT-PCR in samples prepared using pRS. TwoRA yielded somewhat higher call concordances than did RS and pRS (91.8% vs. 89.3% and 88.1%, respectively). Although all target preparation methods were suitable, pRS amplified the highest number of targets and was found to be suitable for amplification of as little as 0.3 ng of total RNA. In addition, RS and pRS were faster and simpler to use than the T7-based methods and resulted in the generation of cDNA, which is more stable than cRNA. PMID:15613496

A simple non-enzymatic method for the preparation of white spot syndrome virus (WSSV) DNA from the haemolymph of Marsupenaeus japonicus using FTA matrix cards.

PubMed

Sudhakaran, R; Mekata, T; Kono, T; Supamattaya, K; Linh, N T H; Suzuki, Y; Sakai, M; Itami, T

2009-07-01

White spot syndrome virus (WSSV) is an important shrimp pathogen responsible for large economic losses for the shrimp culture industry worldwide. The nucleic acids of the virus must be adequately preserved and transported from the field to the laboratory before molecular diagnostic analysis is performed. Here, we developed a new method to isolate WSSV-DNA using Flinders Technology Associates filter paper (FTA matrix card; Whatman) without centrifugation or hazardous steps involved. FTA technology is a new method allowing the simple collection, shipment and archiving of nucleic acids from haemolymph samples providing DNA protection against nucleases, oxidation, UV damage, microbial and fungal attack. DNA samples prepared from 10-fold dilutions of moribund shrimp haemolymph using FTA matrix cards were analysed using semi-quantitative and quantitative polymerase chain reaction (PCR) and were compared with two commercially available DNA isolation methods, the blood GenomicPrep Mini Spin Kit (GE Healthcare) and the DNAzol (Invitrogen). Sequence analysis was performed for the DNA samples prepared using the various isolation procedures and no differences in the sequence among these methods were identified. Results based on the initial copy number of DNA prepared from the GenomicPrep Mini Spin Kit are a little more sensitive than the DNA prepared from FTA matrix cards, whereas the DNAzol method is not suitable for blood samples. Our data shows the efficiency of retention capacity of WSSV-DNA samples from impregnated FTA matrix cards. Matrix cards were easy to store and ship for long periods of time. They provide ease of handling and are a reliable alternative for sample collection and for molecular detection and characterization of WSSV isolates.

Sequencing historical specimens: successful preparation of small specimens with low amounts of degraded DNA.

PubMed

Sproul, John S; Maddison, David R

2017-11-01

Despite advances that allow DNA sequencing of old museum specimens, sequencing small-bodied, historical specimens can be challenging and unreliable as many contain only small amounts of fragmented DNA. Dependable methods to sequence such specimens are especially critical if the specimens are unique. We attempt to sequence small-bodied (3-6 mm) historical specimens (including nomenclatural types) of beetles that have been housed, dried, in museums for 58-159 years, and for which few or no suitable replacement specimens exist. To better understand ideal approaches of sample preparation and produce preparation guidelines, we compared different library preparation protocols using low amounts of input DNA (1-10 ng). We also explored low-cost optimizations designed to improve library preparation efficiency and sequencing success of historical specimens with minimal DNA, such as enzymatic repair of DNA. We report successful sample preparation and sequencing for all historical specimens despite our low-input DNA approach. We provide a list of guidelines related to DNA repair, bead handling, reducing adapter dimers and library amplification. We present these guidelines to facilitate more economical use of valuable DNA and enable more consistent results in projects that aim to sequence challenging, irreplaceable historical specimens. © 2017 John Wiley & Sons Ltd.

Design and evaluation of bilayered buccal film preparations for local administration of lidocaine hydrochloride.

PubMed

Preis, Maren; Woertz, Christina; Schneider, Katharina; Kukawka, Jennifer; Broscheit, Jens; Roewer, Norbert; Breitkreutz, Jörg

2014-04-01

Bilayered oromucosal film preparations (buccal films) offer a promising way to enable drug administration via the oral cavity. Adding a non-soluble or slowly eroding/dissolving backing layer to a mucoadhesive drug-loaded layer enables unidirectional drug delivery. The aim of this study was to investigate different approaches to the manufacture of bilayered films and to examine their properties by applying different characterization methods including an optimized experimental setup for the study of drug release from bilayered films. A solvent suitability study was performed screening over 15 polymers with respect to their feasibility for viscous film formation for film preparation by solvent casting method. Two methods (double-casting and pasting) were found as suitable methods for bilayered film manufacturing. Results from drug release experiments indicated that slowly eroding hypromellose backing layer films revealed the best shielding of the drug-loaded layer to enable unidirectional drug release. In summary, manufacturing of bilayered films using the described methods was feasible. Furthermore, the use of an optimized experimental setup for drug dissolution studies enabled monitoring of drug release without delays in sampling. Copyright © 2014 Elsevier B.V. All rights reserved.

Hydrogen concentration analysis in clinopyroxene using proton-proton scattering analysis

NASA Astrophysics Data System (ADS)

Weis, Franz A.; Ros, Linus; Reichart, Patrick; Skogby, Henrik; Kristiansson, Per; Dollinger, Günther

2018-02-01

Traditional methods to measure water in nominally anhydrous minerals (NAMs) are, for example, Fourier transformed infrared (FTIR) spectroscopy or secondary ion mass spectrometry (SIMS). Both well-established methods provide a low detection limit as well as high spatial resolution yet may require elaborate sample orientation or destructive sample preparation. Here we analyze the water content in erupted volcanic clinopyroxene phenocrysts by proton-proton scattering and reproduce water contents measured by FTIR spectroscopy. We show that this technique provides significant advantages over other methods as it can provide a three-dimensional distribution of hydrogen within a crystal, making the identification of potential inclusions possible as well as elimination of surface contamination. The sample analysis is also independent of crystal structure and orientation and independent of matrix effects other than sample density. The results are used to validate the accuracy of wavenumber-dependent vs. mineral-specific molar absorption coefficients in FTIR spectroscopy. In addition, we present a new method for the sample preparation of very thin crystals suitable for proton-proton scattering analysis using relatively low accelerator potentials.

Ionization behavior of polyphosphoinositides determined via the preparation of pH titration curves using solid-state 31P NMR.

PubMed

Graber, Zachary T; Kooijman, Edgar E

2013-01-01

Detailed knowledge of the degree of ionization of lipid titratable groups is important for the evaluation of protein-lipid and lipid-lipid interactions. The degree of ionization is commonly evaluated by acid-base titration, but for lipids localized in a multicomponent membrane interface this is not a suitable technique. For phosphomonoester-containing lipids such as the polyphosphoinositides, phosphatidic acid, and ceramide-1-phosphate, this is more conveniently accomplished by (31)P NMR. Here, we describe a solid-state (31)P NMR procedure to construct pH titration curves to determine the degree of ionization of phosphomonoester groups in polyphosphoinositides. This procedure can also be used, with suitable sample preparation conditions, for other important signaling lipids. Access to a solid-state, i.e., magic angle spinning, capable NMR spectrometer is assumed. The procedures described here are valid for a Bruker instrument, but can be adapted for other spectrometers as needed.

Synthesis of water suitable as the MEPC.174(58) G8 influent water for testing ballast water management systems.

PubMed

D'Agostino, Fabio; Del Core, Marianna; Cappello, Simone; Mazzola, Salvatore; Sprovieri, Mario

2015-10-01

Here, we describe the methodologies adopted to ensure that natural seawater, used as "influent water" for the land test, complies with the requirement that should be fulfilled to show the efficacy of the new ballast water treatment system (BWTS). The new BWTS was located on the coast of SW Sicily (Italy), and the sampled seawater showed that bacteria and plankton were two orders of magnitude lower than requested. Integrated approaches for preparation of massive cultures of bacteria (Alcanivorax borkumensis and Marinobacter hydrocarbonoclasticus), algae (Tetraselmis suecica), rotifers (Brachionus plicatilis), and crustaceans (Artemia salina) suitable to ensure that 200 m(3) of water fulfilled the international guidelines of MEPC.174(58)G8 are here described. These methodologies allowed us to prepare the "influent water" in good agreement with guidelines and without specific problems arising from natural conditions (seasons, weather, etc.) which significantly affect the concentrations of organisms at sea. This approach also offered the chance to reliably run land tests once every two weeks.

Sample Preparation and Extraction in Small Sample Volumes Suitable for Pediatric Clinical Studies: Challenges, Advances, and Experiences of a Bioanalytical HPLC-MS/MS Method Validation Using Enalapril and Enalaprilat

PubMed Central

Burckhardt, Bjoern B.; Laeer, Stephanie

2015-01-01

In USA and Europe, medicines agencies force the development of child-appropriate medications and intend to increase the availability of information on the pediatric use. This asks for bioanalytical methods which are able to deal with small sample volumes as the trial-related blood lost is very restricted in children. Broadly used HPLC-MS/MS, being able to cope with small volumes, is susceptible to matrix effects. The latter restrains the precise drug quantification through, for example, causing signal suppression. Sophisticated sample preparation and purification utilizing solid-phase extraction was applied to reduce and control matrix effects. A scale-up from vacuum manifold to positive pressure manifold was conducted to meet the demands of high-throughput within a clinical setting. Faced challenges, advances, and experiences in solid-phase extraction are exemplarily presented on the basis of the bioanalytical method development and validation of low-volume samples (50 μL serum). Enalapril, enalaprilat, and benazepril served as sample drugs. The applied sample preparation and extraction successfully reduced the absolute and relative matrix effect to comply with international guidelines. Recoveries ranged from 77 to 104% for enalapril and from 93 to 118% for enalaprilat. The bioanalytical method comprising sample extraction by solid-phase extraction was fully validated according to FDA and EMA bioanalytical guidelines and was used in a Phase I study in 24 volunteers. PMID:25873972

Avoiding drying-artifacts in transmission electron microscopy: Characterizing the size and colloidal state of nanoparticles

PubMed Central

Michen, Benjamin; Geers, Christoph; Vanhecke, Dimitri; Endes, Carola; Rothen-Rutishauser, Barbara; Balog, Sandor; Petri-Fink, Alke

2015-01-01

Standard transmission electron microscopy nanoparticle sample preparation generally requires the complete removal of the suspending liquid. Drying often introduces artifacts, which can obscure the state of the dispersion prior to drying and preclude automated image analysis typically used to obtain number-weighted particle size distribution. Here we present a straightforward protocol for prevention of the onset of drying artifacts, thereby allowing the preservation of in-situ colloidal features of nanoparticles during TEM sample preparation. This is achieved by adding a suitable macromolecular agent to the suspension. Both research- and economically-relevant particles with high polydispersity and/or shape anisotropy are easily characterized following our approach (http://bsa.bionanomaterials.ch), which allows for rapid and quantitative classification in terms of dimensionality and size: features that are major targets of European Union recommendations and legislation. PMID:25965905

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.

Retention of Polyphenolic Species in Spray-Dried Blackberry Extract Using Mannitol as a Thermoprotectant

PubMed Central

Eldridge, Joshua A.; Repko, Debra

2014-01-01

Abstract The purpose of these studies was to determine if a Büchi Mini Spray Dryer B-290 (Büchi Corporation, New Castle, DE, USA) could be used to prepare blackberry extract powders containing mannitol as a thermoprotectant without extensively degrading anthocyanins and polyphenols in the resulting powders. Three blackberry puree extract samples were each prepared by sonication of puree in 30/70% ethanol/water containing 0.003% HCl. Blackberry puree extract sample 1 (S1) contained no mannitol, while blackberry puree extract sample 2 (S2) contained 3.0:1 (w/w) mannitol:berry extract, and blackberry puree extract sample 3 (S3) contained 6.3:1 (w/w) mannitol:berry extract. The levels of anthocyanins and polyphenols in reconstituted spray-dried powders produced from S1–S3 were compared to solutions of S1–S3 that were held at 4°C as controls. All extract samples could be spray-dried using the Büchi Mini Spray Dryer B-290. S1, with no mannitol, showed a 30.8% decrease in anthocyanins and a 24.1% decrease in polyphenols following spray-drying. However, S2 had a reduction in anthocyanins of only 13.8%, while polyphenols were reduced by only 6.1%. S3, with a ratio of mannitol to berry extract of 6.3:1, exhibited a 12.5% decrease in anthocyanins while the decrease in polyphenols after spray-drying was not statistically significant (P=.16). Collectively, these data indicate that a Büchi Mini Spray Dryer B-290 is a suitable platform for producing stable berry extract powders, and that mannitol is a suitable thermoprotectant that facilitates retention of thermosensitive polyphenolic species in berry extracts during spray-drying. PMID:24892214

Detection of enterotoxigenic Clostridium perfringens in meat samples by using molecular methods.

PubMed

Kaneko, Ikuko; Miyamoto, Kazuaki; Mimura, Kanako; Yumine, Natsuko; Utsunomiya, Hirotoshi; Akimoto, Shigeru; McClane, Bruce A

2011-11-01

To prevent food-borne bacterial diseases and to trace bacterial contamination events to foods, microbial source tracking (MST) methods provide important epidemiological information. To apply molecular methods to MST, it is necessary not only to amplify bacterial cells to detection limit levels but also to prepare DNA with reduced inhibitory compounds and contamination. Isolates carrying the Clostridium perfringens enterotoxin gene (cpe) on the chromosome or a plasmid rank among the most important food-borne pathogens. Previous surveys indicated that cpe-positive C. perfringens isolates are present in only ∼5% of nonoutbreak food samples and then only at low numbers, usually less than 3 cells/g. In this study, four molecular assays for the detection of cpe-positive C. perfringens isolates, i.e., ordinary PCR, nested PCR, real-time PCR, and loop-mediated isothermal amplification (LAMP), were developed and evaluated for their reliability using purified DNA. For use in the artificial contamination of meat samples, DNA templates were prepared by three different commercial DNA preparation kits. The four molecular assays always detected cpe when >10³ cells/g of cpe-positive C. perfringens were present, using any kit. Of three tested commercial DNA preparation kits, the InstaGene matrix kit appeared to be most suitable for the testing of a large number of samples. By using the InstaGene matrix kit, the four molecular assays efficiently detected cpe using DNA prepared from enrichment culture specimens of meat samples contaminated with low numbers of cpe-positive C. perfringens vegetative cells or spores. Overall, the current study developed molecular assay protocols for MST to detect the contamination of foods with low numbers of cells, and at a low frequency, of cpe-positive C. perfringens isolates.

The dosimetric properties of phosphate glass systems prepared by different chemical nanomaterials.

PubMed

Abdelhalim, Mohamed Anwar K; Al-Shamrani, Bandar Mora

2016-12-01

The synthesis and characterization of glass systems were carried out using prepared nanocrystals injected into a glass matrix as a thermoluminescence (TL) activator using the melt-quenching method. Sample 1 was prepared as [40P 2 O 5 50BaO:2.5MgO, 2.5Na 2 O, 5TiO 2 ], sample 2 as [37.5P 2 O 5 37.5CaO:25TiO 2 ] and sample 3 as [50P 2 O 5 -50Li 2 O]. Formation of the synthesized compound was confirmed by studying the X-ray diffraction (XRD) patterns and scanning electron microscopy (SEM) images. An annealing procedure was carried out for 1 h at 400 °C. The glow curve position and shape shifted dramatically and linearly to the higher temperature values on increasing the heating rate. A heating rate of 30 °C/s was the most suitable for obtaining a high TL response. Samples 2 and 3 have the highest TL response, which approached the effective atomic number (Z eff ) of natural bone. The observed TL sensitivity of the prepared samples 2 and 3 is less than that of commercially available 'TLD-200 chips' and LiF:Mg,Ti (TLD-100) phosphor. Sample [37.5P 2 O 5 37.5CaO:25TiO 2 ] would be useful in personal and environmental dosimetry for measuring high doses of gamma radiation. Sample [50P 2 O 5 -50Li 2 O] is a good dosimeter, although it requires the addition of an appropriate transitional metal (activator) to overcome the problem of high fading. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Decision support for the selection of reference sites using 137Cs as a soil erosion tracer

NASA Astrophysics Data System (ADS)

Arata, Laura; Meusburger, Katrin; Bürge, Alexandra; Zehringer, Markus; Ketterer, Michael E.; Mabit, Lionel; Alewell, Christine

2017-08-01

The classical approach of using 137Cs as a soil erosion tracer is based on the comparison between stable reference sites and sites affected by soil redistribution processes; it enables the derivation of soil erosion and deposition rates. The method is associated with potentially large sources of uncertainty with major parts of this uncertainty being associated with the selection of the reference sites. We propose a decision support tool to Check the Suitability of reference Sites (CheSS). Commonly, the variation among 137Cs inventories of spatial replicate reference samples is taken as the sole criterion to decide on the suitability of a reference inventory. Here we propose an extension of this procedure using a repeated sampling approach, in which the reference sites are resampled after a certain time period. Suitable reference sites are expected to present no significant temporal variation in their decay-corrected 137Cs depth profiles. Possible causes of variation are assessed by a decision tree. More specifically, the decision tree tests for (i) uncertainty connected to small-scale variability in 137Cs due to its heterogeneous initial fallout (such as in areas affected by the Chernobyl fallout), (ii) signs of erosion or deposition processes and (iii) artefacts due to the collection, preparation and measurement of the samples; (iv) finally, if none of the above can be assigned, this variation might be attributed to turbation processes (e.g. bioturbation, cryoturbation and mechanical turbation, such as avalanches or rockfalls). CheSS was exemplarily applied in one Swiss alpine valley where the apparent temporal variability called into question the suitability of the selected reference sites. In general we suggest the application of CheSS as a first step towards a comprehensible approach to test for the suitability of reference sites.

Cross Section High Resolution Imaging of Polymer-Based Materials

NASA Astrophysics Data System (ADS)

Delaportas, D.; Aden, P.; Muckle, C.; Yeates, S.; Treutlein, R.; Haq, S.; Alexandrou, I.

This paper describes a methodology for preparing cross sections of organic layers suitable for transmission electron microscopy (TEM) at high resolution. Our principal aim is to prepare samples that are tough enough to allow the slicing into sub-150 nm sections. We also need strong contrast at the organic layer area to make it identifiable during TEM. Our approach is to deposit organic layers on flexible substrates and prepare thin cross sections using ultra-microtomy. We sandwich the organic layer between two metal thin films in order to isolate it and improve contrast. Our methodology is used to study the microstructure of polymer/nanotube composites, allowing us to accurately measure the organic layer thickness, determine nanotube dispersion and assess the effect of nanotube clustering on film structural stability.

Microwave synthesis and electrochemical characterization of Mn/Ni mixed oxide for supercapacitor application

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

Prasankumar, T.; Jose, Sujin P., E-mail: sujamystica@yahoo.com; Ilangovan, R.

Nanostructured Mn/Ni mixed metal oxide was synthesized at ambient temperature by facile microwave irradiation technique. The crystal structure and surface morphology were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. X-ray diffraction analysis confirmed the formation of Mn/Ni mixed oxide in rhombohedral phase and the grain size calculated was found to be 87 nm. The irregular spherical morphology of the prepared sample was exhibited by the SEM images. The characteristic peaks of FTIR at about 630 cm{sup −1} and 749 cm{sup −1} were attributed to the Mn-O and Ni-O stretching vibrations respectively. The presence of both Mn and Ni inmore » the prepared sample was validated by the EDS spectra which in turn confirmed the formation of mixed oxide. Cyclic voltammetry and galvanostatic chargedischarge measurements were employed to investigate the electrochemical performance of the mixed oxide. The cyclic voltammetry curves demonstrated good capacitive performance of the sample in the potential window −0.2V to 0.9V. The charge discharge study revealed the suitability of the prepared mixed oxide for the fabrication of supercapacitor electrode.« less

Robust superhydrophobic needle-like nanostructured ZnO surfaces prepared without post chemical-treatment

NASA Astrophysics Data System (ADS)

Velayi, Elmira; Norouzbeigi, Reza

2017-12-01

Robust superhydrophobic ZnO surfaces with micro/nano hybrid hierarchical structures were synthesized on the stainless steel mesh by a facile single-step chemical bath deposition (CBD) method without using further low surface energy materials. The Taguchi L16 experimental design was applied to evaluate the effects of reaction time, type and concentration of the additive, type of the chelating agent, and the molar ratio of the chelating agent to the initial zinc (II) ions. The prepared sample at the optimal conditions exhibited a sustainable and time-independent superhydrophobic behavior with the water contact angle (WCA) of 162.8° ± 2.5° and contact angle hysteresis (CAH) of 1.8° ± 0.5°. The XRD, SEM, TEM and FTIR analyses were used to characterize the prepared samples. Surface characterization using scanning electron microscopy (SEM) indicated accumulation of micro/nano branched ZnO needles on the substrate with the average diameters of ∼85 nm. After 20 abrasion cycles the optimum sample indicated an excellent mechanical robustness via exposure to the pressure of 4.7 kPa. A suitable chemical resistance to the acidic and basic droplets with the pH range of 4 and 9 was observed.

Rheology and stability kinetics of bare silicon nanoparticle inks for low-cost direct printing

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

More, Priyesh V.; Jeong, Sunho; Seo, Yeong-Hui

2013-12-16

Highly dispersed and stable silicon nanoparticles ink is formulated for its application in direct printing or printable electronics. These dispersions are prepared from free-standing silicon nanoparticles which are not capped with any organic ligand, making it suitable for electronic applications. Silicon nanoparticles dispersions are prepared by suspending the nanoparticles in benzonitrile or ethanol by using polypropylene glycol (PPG) as a binder. All the samples show typical shear thinning behavior while the dispersion samples show low viscosities signifying good quality dispersion. Such thinning behavior favors in fabrication of dense films with spin-coating or patterns with drop casting. The dispersion stability ismore » monitored by turbiscan measurements showing good stability for one week. A low-cost direct printing method for dispersion samples is also demonstrated to obtain micro-sized patterns. Low electrical resistivity of resulting patterns, adjustable viscosity and good stability makes these silicon nanoparticles dispersions highly applicable for direct printing process.« less

Community-Level Physiological Profiling of Microbial Communities in Constructed Wetlands: Effects of Sample Preparation.

PubMed

Button, Mark; Weber, Kela; Nivala, Jaime; Aubron, Thomas; Müller, Roland Arno

2016-03-01

Community-level physiological profiling (CLPP) using BIOLOG® EcoPlates™ has become a popular method for characterizing and comparing the functional diversity, functional potential, and metabolic activity of heterotrophic microbial communities. The method was originally developed for profiling soil communities; however, its usage has expanded into the fields of ecotoxicology, agronomy, and the monitoring and profiling of microbial communities in various wastewater treatment systems, including constructed wetlands for water pollution control. When performing CLPP on aqueous samples from constructed wetlands, a wide variety of sample characteristics can be encountered and challenges may arise due to excessive solids, color, or turbidity. The aim of this study was to investigate the impacts of different sample preparation methods on CLPP performed on a variety of aqueous samples covering a broad range of physical and chemical characteristics. The results show that using filter paper, centrifugation, or settling helped clarify samples for subsequent CLPP analysis, however did not do so as effectively as dilution for the darkest samples. Dilution was able to provide suitable clarity for the darkest samples; however, 100-fold dilution significantly affected the carbon source utilization patterns (CSUPs), particularly with samples that were already partially or fully clear. Ten-fold dilution also had some effect on the CSUPs of samples which were originally clear; however, the effect was minimal. Based on these findings, for this specific set of samples, a 10-fold dilution provided a good balance between ease of use, sufficient clarity (for dark samples), and limited effect on CSUPs. The process and findings outlined here can hopefully serve future studies looking to utilize CLPP for functional analysis of microbial communities and also assist in comparing data from studies where different sample preparation methods were utilized.

Electroactive polyurethane/siloxane derived from castor oil as a versatile cardiac patch, part I: Synthesis, characterization, and myoblast proliferation and differentiation.

PubMed

Baheiraei, Nafiseh; Gharibi, Reza; Yeganeh, Hamid; Miragoli, Michele; Salvarani, Nicolò; Di Pasquale, Elisa; Condorelli, Gianluigi

2016-03-01

Tissue-engineered cardiac patch aims at regenerating an infarcted heart by improving cardiac function and providing mechanical support to the diseased myocardium. In order to take advantages of electroactivity, a new synthetic method was developed for the introduction of an electroactive oligoaniline into the backbone of prepared patches. For this purpose, a series of electroactive polyurethane/siloxane films containing aniline tetramer (AT) was prepared through sol-gel reaction of trimethoxysilane functional intermediate polyurethane prepolymers made from castor oil and poly(ethylene glycol). Physicochemical, mechanical, and electrical conductivity of samples were evaluated and the recorded results were correlated to their structural characteristics. The optimized films were proved to be biodegradable and have tensile properties suitable for cardiac patch application. The embedded AT moieties in the backbone of the prepared samples preserved their electroactivity with the electrical conductivity in the range of 10 -4 S/cm. The prepared films were compatible with proliferation of C2C12 and had potential for enhancing myotube formation even without external electrical stimulation. © 2015 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 104A: 775-787, 2016. © 2015 Wiley Periodicals, Inc.

A Highly Flexible, Automated System Providing Reliable Sample Preparation in Element- and Structure-Specific Measurements.

PubMed

Vorberg, Ellen; Fleischer, Heidi; Junginger, Steffen; Liu, Hui; Stoll, Norbert; Thurow, Kerstin

2016-10-01

Life science areas require specific sample pretreatment to increase the concentration of the analytes and/or to convert the analytes into an appropriate form for the detection and separation systems. Various workstations are commercially available, allowing for automated biological sample pretreatment. Nevertheless, due to the required temperature, pressure, and volume conditions in typical element and structure-specific measurements, automated platforms are not suitable for analytical processes. Thus, the purpose of the presented investigation was the design, realization, and evaluation of an automated system ensuring high-precision sample preparation for a variety of analytical measurements. The developed system has to enable system adaption and high performance flexibility. Furthermore, the system has to be capable of dealing with the wide range of required vessels simultaneously, allowing for less cost and time-consuming process steps. However, the system's functionality has been confirmed in various validation sequences. Using element-specific measurements, the automated system was up to 25% more precise compared to the manual procedure and as precise as the manual procedure using structure-specific measurements. © 2015 Society for Laboratory Automation and Screening.

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.

Immunosuppressant therapeutic drug monitoring by LC-MS/MS: workflow optimization through automated processing of whole blood samples.

PubMed

Marinova, Mariela; Artusi, Carlo; Brugnolo, Laura; Antonelli, Giorgia; Zaninotto, Martina; Plebani, Mario

2013-11-01

Although, due to its high specificity and sensitivity, LC-MS/MS is an efficient technique for the routine determination of immunosuppressants in whole blood, it involves time-consuming manual sample preparation. The aim of the present study was therefore to develop an automated sample-preparation protocol for the quantification of sirolimus, everolimus and tacrolimus by LC-MS/MS using a liquid handling platform. Six-level commercially available blood calibrators were used for assay development, while four quality control materials and three blood samples from patients under immunosuppressant treatment were employed for the evaluation of imprecision. Barcode reading, sample re-suspension, transfer of whole blood samples into 96-well plates, addition of internal standard solution, mixing, and protein precipitation were performed with a liquid handling platform. After plate filtration, the deproteinised supernatants were submitted for SPE on-line. The only manual steps in the entire process were de-capping of the tubes, and transfer of the well plates to the HPLC autosampler. Calibration curves were linear throughout the selected ranges. The imprecision and accuracy data for all analytes were highly satisfactory. The agreement between the results obtained with manual and those obtained with automated sample preparation was optimal (n=390, r=0.96). In daily routine (100 patient samples) the typical overall total turnaround time was less than 6h. Our findings indicate that the proposed analytical system is suitable for routine analysis, since it is straightforward and precise. Furthermore, it incurs less manual workload and less risk of error in the quantification of whole blood immunosuppressant concentrations than conventional methods. © 2013.

Habitat modeling for brown trout population in alpine region of Slovenia with focus on determination of preference functions, fuzzy rules and fuzzy sets

NASA Astrophysics Data System (ADS)

Santl, Saso; Carf, Masa; Preseren, Tanja; Jenic, Aljaz

2013-04-01

Water withdrawals and consequently reduction of discharges in river streams for different water uses (hydro power, irrigation, etc.) usually impoverish habitat suitability for naturally present river fish fauna. In Slovenia reduction of suitable habitats resulting from water abstractions frequently impacts local brown trout (Salmo truta) populations. This is the reason for establishment of habitat modeling which can qualitatively and quantitatively support decision making for determination of the environmental flow and other mitigation measures. Paper introduces applied methodology for habitat modeling where input data preparation and elaboration with required accuracy has to be considered. For model development four (4) representative and heterogeneous sampling sites were chosen. Two (2) sampling sections were located within the sections with small hydropower plants and were considered as sections affected by water abstractions. The other two (2) sampling sections were chosen where there are no existing water abstractions. Precise bathymetric mapping for chosen river sections has been performed. Topographic data and series of discharge and water level measurements enabled establishment of calibrated hydraulic models, which provide data on water velocities and depths for analyzed discharges. Brief field measurements were also performed to gather required data on dominant and subdominant substrate size and cover type. Since the accuracy of fish distribution on small scale is very important for habitat modeling, a fish sampling method had to be selected and modified for existing river microhabitats. The brown trout specimen's locations were collected with two (2) different sampling methods. A method of riverbank observation which is suitable for adult fish in pools and a method of electro fishing for locating small fish and fish in riffles or hiding in cover. Ecological and habitat requirements for fish species vary regarding different fish populations as well as eco and hydro morphological types of streams. Therefore, if habitat modeling for brown trout in Slovenia should be applied, it is necessary to determine preference requirements for the locally present brown trout populations. For efficient determination of applied preference functions and linked fuzzy sets/rules, beside expert determination, calibration according to field sampling must also be performed. After this final step a model is prepared for the analysis to support decision making in the field of environmental flow and other mitigation measures determination.

Direct Compositional Characterization of (U,Th)O2 Powders, Microspheres, and Pellets Using TXRF.

PubMed

Dhara, Sangita; Prabhat, Parimal; Misra, N L

2015-10-20

A total reflection X-ray fluorescence (TXRF) analysis method for direct compositional characterization of sintered and green (U,Th)O2 samples in different forms (e.g., pellets, powders, and microspheres) without sample dissolution has been developed for the first time. The methodology involves transfer of only a few nanograms of the sample on the TXRF sample support by gently rubbing the samples on supports or taking their tiny uniform slurry in collodion on the sample support, drying them to make thin film, and measuring the TXRF spectra of the specimens thus prepared. This approach minimizes the matrix effects. Uranium determinations from the TXRF spectra of such specimens were made with respect to thorium, considering it as an internal standard. Samples having uranium atom percent (at%) from 0 to 100 in (U,Th)O2 were analyzed for uranium in comparison to thorium. The results showed an average precision of 2.6% (RSD, 2σ, n = 8). The TXRF-determined results deviated from expected values within 5%. The TXRF results were compared with those of biamperometry with good agreement. The lattice parameters of the solid solutions were calculated using their XRD patterns. A good correlation between lattice parameters and TXRF-determined U at% and between TXRF-determined U at% and expected U at%, calculated on the basis of preparation of (U,Th)O2 solid solutions, was obtained. The developed method is capable of analyzing (U,Th)O2 samples directly with almost negligible sample preparation and is well suited for radioactive samples. The present study suggests that this method can be extended for the determination of U,Th and Pu in other nuclear fuel materials (e.g., nitrides, carbides, etc.) in the form of pellets, powders, and microspheres after suitable modifications in sample handling procedure.

Assessment of different sample preparation routes for mass spectrometric monitoring and imaging of lipids in bone cells via ToF-SIMS

PubMed Central

Schaepe, Kaija; Kokesch-Himmelreich, Julia; Rohnke, Marcus; Wagner, Alena-Svenja; Schaaf, Thimo; Wenisch, Sabine; Janek, Jürgen

2015-01-01

In ToF-SIMS analysis, the experimental outcome from cell experiments is to a great extent influenced by the sample preparation routine. In order to better judge this critical influence in the case of lipid analysis, a detailed comparison of different sample preparation routines is performed—aiming at an optimized preparation routine for systematic lipid imaging of cell cultures. For this purpose, human mesenchymal stem cells were analyzed: (a) as chemically fixed, (b) freeze-dried, and (c) frozen-hydrated. For chemical fixation, different fixatives, i.e., glutaraldehyde, paraformaldehyde, and a mixture of both, were tested with different postfixative handling procedures like storage in phosphate buffered saline, water or critical point drying. Furthermore, secondary lipid fixation via osmium tetroxide was taken into account and the effect of an ascending alcohol series with and without this secondary lipid fixation was evaluated. Concerning freeze-drying, three different postprocessing possibilities were examined. One can be considered as a pure cryofixation technique while the other two routes were based on chemical fixation. Cryofixation methods known from literature, i.e., freeze-fracturing and simple frozen-hydrated preparation, were also evaluated to complete the comparison of sample preparation techniques. Subsequent data evaluation of SIMS spectra in both, positive and negative, ion mode was performed via principal component analysis by use of peak sets representative for lipids. For freeze-fracturing, these experiments revealed poor reproducibility making this preparation route unsuitable for systematic investigations and statistic data evaluation. Freeze-drying after cryofixation showed improved reproducibility and well preserved lipid contents while the other freeze-drying procedures showed drawbacks in one of these criteria. In comparison, chemical fixation techniques via glutar- and/or paraformaldehyde proved most suitable in terms of reproducibility and preserved lipid contents, while alcohol and osmium treatment led to the extraction of lipids and are therefore not recommended. PMID:25791294

Assessment of different sample preparation routes for mass spectrometric monitoring and imaging of lipids in bone cells via ToF-SIMS.

PubMed

Schaepe, Kaija; Kokesch-Himmelreich, Julia; Rohnke, Marcus; Wagner, Alena-Svenja; Schaaf, Thimo; Wenisch, Sabine; Janek, Jürgen

2015-03-19

In ToF-SIMS analysis, the experimental outcome from cell experiments is to a great extent influenced by the sample preparation routine. In order to better judge this critical influence in the case of lipid analysis, a detailed comparison of different sample preparation routines is performed-aiming at an optimized preparation routine for systematic lipid imaging of cell cultures. For this purpose, human mesenchymal stem cells were analyzed: (a) as chemically fixed, (b) freeze-dried, and (c) frozen-hydrated. For chemical fixation, different fixatives, i.e., glutaraldehyde, paraformaldehyde, and a mixture of both, were tested with different postfixative handling procedures like storage in phosphate buffered saline, water or critical point drying. Furthermore, secondary lipid fixation via osmium tetroxide was taken into account and the effect of an ascending alcohol series with and without this secondary lipid fixation was evaluated. Concerning freeze-drying, three different postprocessing possibilities were examined. One can be considered as a pure cryofixation technique while the other two routes were based on chemical fixation. Cryofixation methods known from literature, i.e., freeze-fracturing and simple frozen-hydrated preparation, were also evaluated to complete the comparison of sample preparation techniques. Subsequent data evaluation of SIMS spectra in both, positive and negative, ion mode was performed via principal component analysis by use of peak sets representative for lipids. For freeze-fracturing, these experiments revealed poor reproducibility making this preparation route unsuitable for systematic investigations and statistic data evaluation. Freeze-drying after cryofixation showed improved reproducibility and well preserved lipid contents while the other freeze-drying procedures showed drawbacks in one of these criteria. In comparison, chemical fixation techniques via glutar- and/or paraformaldehyde proved most suitable in terms of reproducibility and preserved lipid contents, while alcohol and osmium treatment led to the extraction of lipids and are therefore not recommended.

Influence of the cooling rate and the blend ratio on the physical stability of co-amorphous naproxen/indomethacin.

PubMed

Beyer, Andreas; Grohganz, Holger; Löbmann, Korbinian; Rades, Thomas; Leopold, Claudia S

2016-12-01

Co-amorphization represents a promising approach to increase the physical stability and dissolution rate of amorphous active pharmaceutical ingredients (APIs) as an alternative to polymer glass solutions. For amorphous and co-amorphous systems, it is reported that the preparation method and the blend ratio play major roles with regard to the resulting physical stability. Therefore, in the present study, co-amorphous naproxen-indomethacin (NAP/IND) was prepared by melt-quenching at three different cooling rates and at ten different NAP/IND blend ratios. The samples were analyzed using XRPD and FTIR, both directly after preparation and during storage to investigate their physical stabilities. All cooling methods led to fully amorphous samples, but with significantly different physical stabilities. Samples prepared by fast cooling had a higher degree of crystallinity after 300d of storage than samples prepared by intermediate cooling and slow cooling. Intermediate cooling was subsequently used to prepare co-amorphous NAP/IND at different blend ratios. In a previous study, it was postulated that the equimolar (0.5:0.5) co-amorphous blend of NAP/IND is most stable. However, in the present study the physically most stable blend was found for a NAP/IND ratio of 0.6:0.4, which also represents the eutectic composition of the crystalline NAP/γ-IND system. This indicates that the eutectic point may be of major importance for the stability of binary co-amorphous systems. Slight deviations from the optimal naproxen molar fraction led to significant recrystallization during storage. Either naproxen or γ-indomethacin recrystallized until a naproxen molar fraction of about 0.6 in the residual co-amorphous phase was reached again. In conclusion, the physical stability of co-amorphous NAP/IND may be significantly improved, if suitable preparation conditions and the optimal phase composition are chosen. Copyright © 2016 Elsevier B.V. All rights reserved.

Liquid precursor for deposition of copper selenide and method of preparing the same

DOEpatents

Curtis, Calvin J.; Miedaner, Alexander; Franciscus Antonius Maria Van Hest, Marinus; Ginley, David S.; Hersh, Peter A.; Eldada, Louay; Stanbery, Billy J.

2015-09-08

Liquid precursors containing copper and selenium suitable for deposition on a substrate to form thin films suitable for semiconductor applications are disclosed. Methods of preparing such liquid precursors and methods of depositing a precursor on a substrate are also disclosed.

Laboratory analytical methods for the determination of the hydrocarbon status of soils (a review)

NASA Astrophysics Data System (ADS)

Pikovskii, Yu. I.; Korotkov, L. A.; Smirnova, M. A.; Kovach, R. G.

2017-10-01

Laboratory analytical methods suitable for the determination of the hydrocarbon status of soils (a specific soil characteristic involving information on the total content and qualitative features of soluble (bitumoid) carbonaceous substances and individual hydrocarbons (polycyclic aromatic hydrocarbons, alkanes, etc.) in bitumoid, as well as the composition and content of hydrocarbon gases) have been considered. Among different physicochemical methods of study, attention is focused on the methods suitable for the wide use. Luminescence-bituminological analysis, low-temperature spectrofluorimetry (Shpolskii spectroscopy), infrared (IR) spectroscopy, gas chromatography, chromatography-mass spectrometry, and some other methods have been characterized, as well as sample preparation features. Advantages and limitations of each of these methods are described; their efficiency, instrumental complexity, analysis duration, and accuracy are assessed.

Easily recycled Bi2O3 photocatalyst coatings prepared via ball milling followed by calcination

NASA Astrophysics Data System (ADS)

Cheng, Lijun; Hu, Xumin; Hao, Liang

2017-06-01

Bi2O3 photocatalyst coatings derived from Bi coatings were first prepared by a two-step method, namely ball milling followed by the calcination process. The as-prepared samples were characterized by XRD, SEM, XPS and UV-Vis spectra, respectively. The results showed that monoclinic Bi2O3 coatings were obtained after sintering Bi coatings at 673 or 773 K, while monoclinic and triclinic mixed phase Bi2O3 coatings were obtained at 873 or 973 K. The topographies of the samples were observably different, which varied from flower-like, irregular, polygonal to nanosized particles with the increase in calcination temperature. Photodegradation of malachite green under simulated solar irradiation for 180 min showed that the largest degradation efficiency of 86.2% was achieved over Bi2O3 photocatalyst coatings sintered at 873 K. The Bi2O3 photocatalyst coatings, encapsulated with Al2O3 ball with an average diameter around 1 mm, are quite easily recycled, which provides an alternative visible light-driven photocatalyst suitable for practical water treatment application.

Preparation of electromechanically active silicone composites and some evaluations of their suitability for biomedical applications.

PubMed

Iacob, Mihail; Bele, Adrian; Patras, Xenia; Pasca, Sorin; Butnaru, Maria; Alexandru, Mihaela; Ovezea, Dragos; Cazacu, Maria

2014-10-01

Some films based on electromechanically active polymer composites have been prepared. Polydimethylsiloxane-α,ω-diols (PDMSs) having different molecular masses (Mv=60 700 and Mv=44 200) were used as matrix in which two different active fillers were incorporated: titanium dioxide in situ generated from its titanium isopropoxide precursor and silica particles functionalized with polar aminopropyl groups on surface. A reference sample based on simple crosslinked PDMS was also prepared. The composites processed as films were investigated to evaluate their ability to act as efficient electromechanical actuators for potential biomedical application. Thus, the surface morphology of interest for electrodes compliance was analysed by atomic force microscopy. Mechanical and dielectric characteristics were evaluated by tensile tests and dielectric spectroscopy, respectively. Electromechanical actuation responses were measured by interferometry. The biocompatibility of the obtained materials has been verified through tests in vitro and, for valuable films, in vivo. The experimental, clinical and anatomopathological evaluation of the in vivo tested samples did not reveal significant pathological modifications. Copyright © 2014 Elsevier B.V. All rights reserved.

Infrared spectroscopy and upconversion luminescence behaviour of erbium doped yttrium (III) oxide phosphor

NASA Astrophysics Data System (ADS)

Dubey, Vikas; Tiwari, Ratnesh; Tamrakar, Raunak Kumar; Rathore, Gajendra Singh; Sharma, Chitrakant; Tiwari, Neha

2014-11-01

The paper reports upconversion luminescence behaviour and infra-red spectroscopic pattern of erbium doped yttrium (III) oxide phosphor. Sample was synthesized by solid state reaction method with variable concentration or erbium (0.5-2.5 mol%). The conventional solid state method is suitable for large scale production and eco-friendly method. The prepared sample was characterized by X-ray diffraction (XRD) technique. From structural analysis by XRD technique shows cubic structure of prepared sample with variable concentration of erbium and no impurity phase were found when increase the concentration of Er3+. Particle size was calculated by Scherer's formula and it varies from 67 nm to 120 nm. The surface morphology of prepared phosphor was determined by field emission gun scanning electron microscopy (FEGSEM) technique. The surface morphology of the sample shows good connectivity with grains as well as some agglomerates formation occurs in sample. The functional group analysis was done by Fourier transform infra-red technique (FTIR) analysis which confirm the formation of Y2O3:Er3+ phosphor was prepared. The results indicated that the Y2O3:Er3+ phosphors might have high upconversion efficiency because of their low vibrational energy. Under 980 nm laser excitation sample shows intense green emission at 555 nm and orange emission at 590 nm wavelength. For green emission transition occurs 2H11/2 → 4I15/2, 4S3/2 → 4I15/2 for upconversion emissions. Excited state absorption and energy transfer process were discussed as possible upconversion mechanisms. The near infrared luminescence spectra was recorded. The upconversion luminescence intensity increase with increasing the concentration or erbium up to 2 mol% after that luminescence intensity decreases due to concentration quenching occurs. Spectrophotometric determinations of peaks are evaluated by Commission Internationale de I'Eclairage (CIE) technique. From CIE technique the dominant peak of from PL spectra shows intense green emission so the prepared phosphor is may be useful for green light emitting diode (GLED) application.

Preparation and characterization of the silicon clathrate NaxSi{136} (x -> 0)

NASA Astrophysics Data System (ADS)

Ammar, A.; Cros, C.; Pouchard, M.; Jaussaud, N.; Bassat, J.-M.; Villeneuve, G.; Reny, E.

2005-03-01

The type-II silicon clathrate, NaxSi{136}, having a residual sodium content as low as 37 ppm (x = 0.0062) has been prepared by thermal decomposition of NaSi under high vacuum in the temperature range 340-420 ° C followed by subsequent treatments under high vacuum, and completed by several treaments with iodine at 300-350 ° C. The final sample was characterized by XRD, chemical analysis and EPR spectroscopy. This latter technique proved to be particularly suitable to the characterization of highly diluted sodium atoms in the open host lattice of a type II clathrate of silicon and the quantitaive determination of the residual sodium content

Lab-on-a-chip modules for detection of highly pathogenic bacteria: from sample preparation to detection

NASA Astrophysics Data System (ADS)

Julich, S.; Kopinč, R.; Hlawatsch, N.; Moche, C.; Lapanje, A.; Gärtner, C.; Tomaso, H.

2014-05-01

Lab-on-a-chip systems are innovative tools for the detection and identification of microbial pathogens in human and veterinary medicine. The major advantages are small sample volume and a compact design. Several fluidic modules have been developed to transform analytical procedures into miniaturized scale including sampling, sample preparation, target enrichment, and detection procedures. We present evaluation data for single modules that will be integrated in a chip system for the detection of pathogens. A microfluidic chip for purification of nucleic acids was established for cell lysis using magnetic beads. This assay was evaluated with spiked environmental aerosol and swab samples. Bacillus thuringiensis was used as simulant for Bacillus anthracis, which is closely related but non-pathogenic for humans. Stationary PCR and a flow-through PCR chip module were investigated for specific detection of six highly pathogenic bacteria. The conventional PCR assays could be transferred into miniaturized scale using the same temperature/time profile. We could demonstrate that the microfluidic chip modules are suitable for the respective purposes and are promising tools for the detection of bacterial pathogens. Future developments will focus on the integration of these separate modules to an entire lab-on-a-chip system.

Liquid precursor for deposition of indium selenide and method of preparing the same

DOEpatents

Curtis, Calvin J.; Miedaner, Alexander; van Hest, Marinus Franciscus Antonius Maria; Ginley, David S.; Hersh, Peter A.; Eldada, Louay; Stanbery, Billy J.

2015-09-22

Liquid precursors containing indium and selenium suitable for deposition on a substrate to form thin films suitable for semiconductor applications are disclosed. Methods of preparing such liquid precursors and method of depositing a liquid precursor on a substrate are also disclosed.

Ozonation as an effective way to stabilize new kinds of fermentation media used in biotechnological production of liquid fuel additives.

PubMed

Dziugan, Piotr; Balcerek, Maria; Binczarski, Michal J; Kregiel, Dorota; Kucner, Marcin; Kunicka-Styczynska, Alina; Pielech-Przybylska, Katarzyna; Smigielski, Krzysztof; Witonska, Izabela A

2016-01-01

Intermediates from processing sugar beets are considered an attractive feedstock for ethanol fermentation due to their high fermentable sugar content. In particular, medium prepared from raw sugar beet juice seems to be suitable for use in fermentation processes, but it is microbiologically unstable and requires sterilization. This study investigates the effect of ozone treatment on the activity of microbial cells from Bacillus subtilis, Leuconostoc mesenteroides, Geobacillus stearothermophilus, Candida vini, and Aspergillus brasiliensis in raw sugar beet juice. Raw sugar beet juice contaminated with 10(5) cfu/mL of the microbial strains was treated with gaseous ozone (ozone concentration in the oxygen stream 0.1 g O3/L O2, flow rate 6 L/h, 10-30 min, 18-20 °C). The number of microflora decreased to 0 cfu/mL after 30 min of ozone treatment in all studied samples. Medium prepared from raw sugar beet juice and sterilized by ozonation is suitable for use in fermentation processes.

Quantification of vicine and convicine in faba bean seeds using hydrophilic interaction liquid chromatography.

PubMed

Purves, Randy W; Khazaei, Hamid; Vandenberg, Albert

2018-02-01

Faba bean (Vicia faba L.) provides environmental and health benefits; however, the presence of the pyrimidine glycosides vicine and convicine (v-c) in its seeds limits consumption. Low v-c genotypes have been introduced, but the convicine levels in these genotypes have not been quantified. To improve detection, the polar nature of v-c was exploited by implementing hydrophilic interaction liquid chromatography (HILIC). A sample preparation method using a two-step extraction was developed for use with UV and/or tandem mass spectrometry (SRM) detection. The HILIC-UV method was suitable for over three orders of magnitude, covering the range of v-c concentrations in faba bean seeds across all genotypes tested. The linear range of HILIC-SRM was slightly less (∼3 orders of magnitude), but improved sensitivity and selectivity make it more suitable for quantifying low v-c samples. The analysis of 13 genotypes suggests that v-c concentrations in faba bean seeds may be independent quantitative traits. Copyright © 2017 Elsevier Ltd. All rights reserved.

Extractive procedure for uranium determination in water samples by liquid scintillation counting.

PubMed

Gomez Escobar, V; Vera Tomé, F; Lozano, J C; Martín Sánchez, A

1998-07-01

An extractive procedure for uranium determination using liquid scintillation counting with the URAEX cocktail is described. Interference from radon and a strong influence of nitrate ion were detected in this procedure. Interference from radium, thorium and polonium emissions were very low when optimal operating conditions were reached. Quenching effects were considered and the minimum detectable activity was evaluated for different sample volumes. Isotopic analysis of samples can be performed using the proposed method. Comparisons with the results obtained with the general procedure used in alpha spectrometry with passivated implanted planar silicon detectors showed good agreement. The proposed procedure is thus suitable for uranium determination in water samples and can be considered as an alternative to the laborious conventional chemical preparations needed for alpha spectrometry methods using semiconductor detectors.

Electromechanical properties of polyamide/lycra fabric treated with PEDOT:PSS

NASA Astrophysics Data System (ADS)

Tadesse, M. G.; Mengistie, D. A.; Loghin, C.; Chen, Y.; Wang, L.; Catalin, D.; Müller, C.; Nierstrasz, V.

2017-10-01

One of the challenges in smart textiles is to develop suitable multifunctional materials that can address simultaneously several characteristics such as durability, stretchability, lightweight, and conductivity. Conductive polymers which showed success in different technological fields like polymer solar cells and light emitting diodes are promising in many smart textile applications. In this work, we treated a common polyamide/lycra knitted fabric with PEDOT:PSS for stretchable e-textiles. PEDOT:PSS, with DMSO as a conductivity enhancer and different ratios of water-based polyurethane dispersions as a binder, was applied to the fabric with simple immersion and coating applications. The effect of different application methods and binder ratio on the surface resistance of the fabric was monitored with four point probe electrical surface resistance measurement systems. Samples prepared by immersion technique are more uniform and have higher conductivity than those prepared by a coating technique. SEM images showed that PEDOT:PSS is incorporated into the structure in the immersion method while in the coating it is majorly present on the surface of the fabric. The tensile measurement showed that the acidic PEDOT:PSS and polyurethane dispersion coating has no adverse effect on the tensile strength of the fabric. The coated samples can be stretched up to 700% while still reasonably conductive. The resistance increases only by a small amount when samples were stretched cyclically by stretching 100%. Generally, samples prepared by the immersion method maintained better conductivity while stretching than those by a coating method. The washing fastness of the samples was also assessed.

Synthesis of lithium superionic conductor by growth of a nanoglass within mesoporous silica SBA-15 template

NASA Astrophysics Data System (ADS)

Chatterjee, Soumi; Miah, Milon; Saha, Shyamal Kumar; Chakravorty, Dipankar

2018-04-01

Nanodimensional silica based glasses containing alkali ions have recently been grown using suitable templates. These have shown electrical properties drastically different from those of their bulk counterpart. We have synthesized silicophosphate glasses having lithium ions with concentrations of 15-35 mole% Li2O within mesoporous silica SBA-15 (Santa Barbara amorphous-15) comprising of pores of diameter ~5 nm. The nanoglasses are characterized by electrical conductivities 5-6 orders of magnitude higher than those of the corresponding bulk glasses. These properties are attributed to the presence of a larger free volume in the nanoglasses as compared to their bulk states. The nanocomposites with 35 mole% Li2O exhibit an electrical conductivity of ~3 × 10-4 S · cm-1 at around room temperature. The activation energy for Li+ ion migration has been estimated from the conductivity-temperature variation to be 0.078 eV. These nanocomposites are believed to be ideally suited for the fabrication of solid state lithium ion batteries. We have also explored the efficiency of silicophosphate glass powders as possible electrode materials. Glass of composition 70SiO2/30P2O5 was prepared by using Pluronic P-123 tri-block copolymer along with suitable precursor sols. Cyclic voltammetric and galvanostatic charge/discharge measurements were carried out on the samples prepared in combination with suitable conductive fillers using a two-electrode system. These exhibited a high specific capacitance of 356 F g-1 making them ideally suitable as electrode materials for making a lithium ion solid state battery system.

Practical method for the definition of chromatographic peak parameters in preparative liquid chromatography.

PubMed

Jin, Gaowa; Guo, Zhimou; Xiao, Yuansheng; Yan, Jingyu; Dong, Xuefang; Shen, Aijin; Wang, Chaoran; Liang, Xinmiao

2016-10-01

A practical method was established for the definition of chromatographic parameters in preparative liquid chromatography. The parameters contained both the peak broadening level under different amounts of sample loading and the concentration distribution of the target compound in the elution. The parameters of the peak broadening level were defined and expressed as a matrix, which consisted of sample loading, the forward broadening and the backward broadening levels. The concentration distribution of the target compound was described by the heat map of the elution profile. The most suitable stationary phase should exhibit the narrower peak broadening and it was best to broaden to both sides to compare to the peak under analytical conditions. Besides, the concentration distribution of the target compounds should be focused on the middle of the elution. The guiding principles were validated by purification of amitriptyline from the mixture of desipramine and amitriptyline. On the selected column, when the content of the impurity desipramine was lower than 0.1%, the recovery of target compound was much higher than the other columns even when the sample loading was as high as 8.03 mg/cm 3 . The parameters and methods could be used for the evaluation and selection of stationary phases in preparative chromatography. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Gas chromatographic detection of some nitro explosive compounds in soil samples after solid-phase microextraction with carbon ceramic copper nanoparticle fibers.

PubMed

Farhadi, Khalil; Bochani, Shayesteh; Hatami, Mehdi; Molaei, Rahim; Pirkharrati, Hossein

2014-07-01

In this research, a new solid-phase microextraction fiber based on carbon ceramic composites with copper nanoparticles followed by gas chromatography with flame ionization detection was applied for the extraction and determination of some nitro explosive compounds in soil samples. The proposed method provides an overview of trends related to synthesis of solid-phase microextraction sorbents and their applications in preconcentration and determination of nitro explosives. The sorbents were prepared by mixing of copper nanoparticles with a ceramic composite produced by mixture of methyltrimethoxysilane, graphite, methanol, and hydrochloric acid. The prepared sorbents were coated on copper wires by dip-coating method. The prepared nanocomposites were evaluated statistically and provided better limits of detection than the pure carbon ceramic. The limit of detection of the proposed method was 0.6 μg/g with a linear response over the concentration range of 2-160 μg/g and square of correlation coefficient >0.992. The new proposed fiber has been demonstrated to be a suitable, inexpensive, and sensitive candidate for extraction of nitro explosive compounds in contaminated soil samples. The constructed fiber can be used more than 100 times without the need for surface generation. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The development and validation of measures to assess cooking skills and food skills.

PubMed

Lavelle, Fiona; McGowan, Laura; Hollywood, Lynsey; Surgenor, Dawn; McCloat, Amanda; Mooney, Elaine; Caraher, Martin; Raats, Monique; Dean, Moira

2017-09-02

With the increase use of convenience food and eating outside the home environment being linked to the obesity epidemic, the need to assess and monitor individuals cooking and food skills is key to help intervene where necessary to promote the usage of these skills. Therefore, this research aimed to develop and validate a measure for cooking skills and one for food skills, that are clearly described, relatable, user-friendly, suitable for different types of studies, and applicable across all sociodemographic levels. Two measures were developed in light of the literature and expert opinion and piloted for clarity and ease of use. Following this, four studies were undertaken across different cohorts (including a sample of students, both 'Food preparation novices' and 'Experienced food preparers', and a nationally representative sample) to assess temporal stability, psychometrics, internal consistency reliability and construct validity of both measures. Analysis included T-tests, Pearson's correlations, factor analysis, and Cronbach's alphas, with a significance level of 0.05. Both measures were found to have a significant level of temporal stability (P < 0.001). Factor analysis revealed three factors with eigenvalues over 1, with two items in a third factor outside the two suggested measures. The internal consistency reliability for the cooking skills confidence measure ranged from 0.78 to 0.93 across all cohorts. The food skills confidence measure's Cronbach's alpha's ranged from 0.85 to 0.94. The two measures also showed a high discriminate validity as there were significant differences (P < 0.05 for cooking skills confidence and P < 0.01 for food skills confidence) between Food preparation novices' and 'Experienced food preparers.' The cooking skills confidence measure and the food skills confidence measure have been shown to have a very satisfactory reliability, validity and are consistent over time. Their user-friendly applicability make both measures highly suitable for large scale cross-sectional, longitudinal and intervention studies to assess or monitor cooking and food skills levels and confidence.

A PEG-Based Hydrogel for Effective Wound Care Management

PubMed Central

Chen, Sen-Lu; Fu, Ru-Huei; Liao, Shih-Fei; Liu, Shih-Ping; Lin, Shinn-Zong; Wang, Yu-Chi

2018-01-01

It is extremely challenging to achieve strong adhesion in soft tissues while minimizing toxicity, tissue damage, and other side effects caused by wound sealing materials. In this study, flexible synthetic hydrogel sealants were prepared based on polyethylene glycol (PEG) materials. PEG is a synthetic material that is nontoxic and inert and, thus, suitable for use in medical products. We evaluated the in vitro biocompatibility tests of the dressings to assess cytotoxicity and irritation, sensitization, pyrogen toxicity, and systemic toxicity following the International Organization for Standardization 10993 standards and the in vivo effects of the hydrogel samples using Coloskin liquid bandages as control samples for potential in wound closure. PMID:29637814

An Efficient Protocol for Preparation of Gallic Acid from Terminalia bellirica (Gaertn.) Roxb by Combination of Macroporous Resin and Preparative High-Performance Liquid Chromatography.

PubMed

Zou, Denglang; Chen, Tao; Chen, Chen; Li, Hongmei; Liu, Yongling; Li, Yulin

2016-08-01

In this article, macroporous resin column chromatography and preparative high-performance liquid chromatography were applied for preparation of gallic acid from Terminalia bellirica (Gaertn.) Roxb. In the first step, six kinds of resins were investigated by adsorption and desorption tests and AB-8 macroporous resin was selected for the enrichment of gallic acid. As a result, 20 g of gallic acid at a purity of 71% could be separated from 100 g of crude extract in which the content of gallic acid was 16.7% and the recovery of gallic acid reached 85.0%. In the second step, preparative high-performance liquid chromatography was selected to purify gallic acid. As a result, 640 mg of gallic acid at a purity of 99.1% was obtained from 1 g of sample in 35 min. The results demonstrated that macroporous resin coupled with preparative high-performance liquid chromatography was suitable for preparation of gallic acid from T. bellirica (Gaertn.) Roxb. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

The International Standard for Oxytetracycline

PubMed Central

Humphrey, J. H.; Lightbown, J. W.; Mussett, M. V.; Perry, W. L. M.

1955-01-01

The first attempt to set up an international standard for oxytetracycline, using oxytetracycline hydrochloride, failed because of difficulties in obtaining a preparation whose moisture content was uniform after distribution into ampoules. A preparation of dihydrate of oxytetracycline base was obtained instead, and was compared in an international collaborative assay with a sample of oxytetracycline hydrochloride, which was the current working standard of Chas. Pfizer & Co., Inc., USA. The results of the collaborative assay showed that the potency of the dihydrate was uniform, and that it was a suitable preparation for use as the International Standard. Evidence was obtained, however, that the reference preparation at the time of examination was less potent than had been originally supposed, and that it was hydrated. The potency of the proposed international standard was recalculated after allowance for water in the reference preparation, and the resulting biological potency agreed well with that to be expected on the basis of the physicochemical properties of the preparation. It was agreed, therefore, that the recalculated values should be used, and the preparation of oxytetracycline base dihydrate used in the collaborative assay is established as the International Standard for Oxytetracycline with a potency of 900 International Units per mg. PMID:13284563

Rapid and reliable determination of the halogenating peroxidase activity in blood samples.

PubMed

Flemmig, Jörg; Schwarz, Pauline; Bäcker, Ingo; Leichsenring, Anna; Lange, Franziska; Arnhold, Jürgen

2014-12-15

By combining easy and fast leukocyte enrichment with aminophenyl-fluorescein (APF) staining we developed a method to quickly and specifically address the halogenating activity of the immunological relevant blood heme peroxidases myeloperoxidase and eosinophil peroxidase, respectively. For leukocyte enrichment a two-fold hypotonic lysis procedure of the blood with Millipore water was chosen which represents a cheap, fast and reliable method to diminish the amount of erythrocytes in the samples. This procedure is shown to be suitable both to human and murine blood micro-samples, making it also applicable to small animal experiments with recurring blood sampling. As all types of leukocytes are kept in the sample during the preparation, they can be analysed separately after discrimination during the flow cytometry analysis. This also holds for all heme peroxidase-containing cells, namely neutrophils, eosinophils and monocytes. Moreover additional parameters (e.g. antibody staining) can be combined with the heme peroxidase activity determination to gain additional information about the different immune cell types. Based on previous results we applied APF for specifically addressing the halogenating activity of leukocyte peroxidases in blood samples. This dye is selectively oxidized by the MPO and EPO halogenation products hypochlorous and hypobromous acid. This approach may provide a suitable tool to gain more insights into the immune-physiological role of the halogenating activity of heme peroxidases. Copyright © 2014 Elsevier B.V. All rights reserved.

25 CFR 63.16 - Who conducts the background investigation and prepares the determination of suitability for...

Code of Federal Regulations, 2010 CFR

2010-04-01

... 25 Indians 1 2010-04-01 2010-04-01 false Who conducts the background investigation and prepares the determination of suitability for employment? 63.16 Section 63.16 Indians BUREAU OF INDIAN AFFAIRS, DEPARTMENT OF THE INTERIOR TRIBAL GOVERNMENT INDIAN CHILD PROTECTION AND FAMILY VIOLENCE PREVENTION Minimum...

Synthesis and characterization of α-NaYF{sub 4}: Yb, Er nanoparticles by reverse microemulsion method

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

Gunaseelan, M.; Senthilselvan, J., E-mail: jsselvan@hotmail.com

2016-05-06

A simple and cost effective reverse microemulsion system was newly designed to synthesis NaYF{sub 4}:20%Yb,2%Er upconverting luminescent nanoparticles. XRD results confirms the cubic structure of NaYF{sub 4} nanophosphor in the as prepared condition without any other impurity phases. The as-prepared sample itself having highly crystalline nanoparticle with well dispersed uniform morphology is the advantage of this reverse microemulsion process. HRTEM images of as prepared and calcined samples revealed spherical nanoclusters morphology with size of ~210 nm and ~245 nm respectively. The characteristic absorption wavelength that occurs at 980 nm due to transition of energy levels {sup 2}F{sub 5/2} to {sup 2}F{sub 7/2} formore » Yb{sup 3+} rare earth ion in as prepared and calcined upconversion nanoparticle confirms the presence of Yb{sup 3+} by UV-Visible spectroscopy which can act as a sensitizer for photonic upconversion. Therefore the absorption at NIR region and emission spectrum at visible region suggests that NaYF{sub 4}:20%Yb,2%Er is suitable for upcoversion process, due to its optical property and chemical stability this material also be useful for bio imaging applications.« less

CoPt/TiN films nanopatterned by RF plasma etching towards dot-patterned magnetic media

NASA Astrophysics Data System (ADS)

Szívós, János; Pothorszky, Szilárd; Soltys, Jan; Serényi, Miklós; An, Hongyu; Gao, Tenghua; Deák, András; Shi, Ji; Sáfrán, György

2018-03-01

CoPt thin films as possible candidates for Bit Patterned magnetic Media (BPM) were prepared and investigated by electron microscopy techniques and magnetic measurements. The structure and morphology of the Direct Current (DC) sputtered films with N incorporation were revealed in both as-prepared and annealed state. Nanopatterning of the samples was carried out by means of Radio Frequency (RF) plasma etching through a Langmuir-Blodgett film of silica nanospheres that is a fast and high throughput technique. As a result, the samples with hexagonally arranged 100 nm size separated dots of fct-phase CoPt were obtained. The influence of the order of nanopatterning and anneling on the nanostructure formation was revealed. The magnetic properties of the nanopatterned fct CoPt films were investigated by Vibrating Sample Magnetometer (VSM) and Magnetic Force Microscopy (MFM). The results show that CoPt thin film nanopatterned by means of the RF plasma etching technique is promising candidate to a possible realization of BPM. Furthermore, this technique is versatile and suitable for scaling up to technological and industrial applications.

Urchin-like gold nanoparticle-based immunochromatographic strip test for rapid detection of fumonisin B1 in grains.

PubMed

Ren, Wenjie; Huang, Zhibing; Xu, Yang; Li, Yanping; Ji, Yanwei; Su, Baowei

2015-09-01

An immunochromatographic strip (ICS) using urchin-like gold nanoparticles (UGNs) for sensitive detection of fumonisin B1 (FB1) was developed to meet the requirement for rapidly monitoring FB1 in grain samples. The sensitivity of the ICS was 5.0 ng/mL, which represents a fourfold increase in sensitivity over conventional strip preparation using colloidal gold as the antibody-labeled probe. Analysis of FB1 in grain samples showed that data obtained from the strip tests were in a good agreement with those obtained from HPLC and enzyme-linked immunosorbent assays (ELISAs). This qualitative test did not require any specialized equipment, and the detection time was less than 5 min, which is suitable for on-site testing of FB1 in grain samples. Overall, to our knowledge, this is the first report of using a UGN as the antibody-labeled probe for sensitive detection of FB1 in grains using an ICS. Graphical Abstract Preparation of ICS using conventional colloidal gold and urchin-like gold nanoparticle, respectively.

A recombinase polymerase amplification assay for rapid detection of Crimean-Congo Haemorrhagic fever Virus infection.

PubMed

Bonney, Laura C; Watson, Robert J; Afrough, Babak; Mullojonova, Manija; Dzhuraeva, Viktoriya; Tishkova, Farida; Hewson, Roger

2017-10-01

Crimean-Congo Haemorrhagic fever Virus (CCHFV) is a rapidly emerging vector-borne pathogen and the cause of a virulent haemorrhagic fever affecting large parts of Europe, Africa, the Middle East and Asia. An isothermal recombinase polymerase amplification (RPA) assay was successfully developed for molecular detection of CCHFV. The assay showed rapid (under 10 minutes) detection of viral extracts/synthetic virus RNA of all 7 S-segment clades of CCHFV, with high target specificity. The assay was shown to tolerate the presence of inhibitors in crude preparations of mock field samples, indicating that this assay may be suitable for use in the field with minimal sample preparation. The CCHFV RPA was successfully used to screen and detect CCHFV positives from a panel of clinical samples from Tajikistan. The assay is a rapid, isothermal, simple-to-perform molecular diagnostic, which can be performed on a light, portable real-time detection device. It is ideally placed therefore for use as a field-diagnostic or in-low resource laboratories, for monitoring of CCHF outbreaks at the point-of-need, such as in remote rural regions in affected countries.

Polymer monolithic capillary microextraction on-line coupled with inductively coupled plasma-mass spectrometry for the determination of trace Au and Pd in biological samples

NASA Astrophysics Data System (ADS)

Liu, Xiaolan; He, Man; Chen, Beibei; Hu, Bin

2014-11-01

A novel method based on on-line polymer monolithic capillary microextraction (CME)-inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of trace Au and Pd in biological samples. For this purpose, poly(glycidyl methacrylate-ethylene dimethacrylate) monolith was prepared and functionalized with mercapto groups. The prepared monolith exhibited good selectivity to Au and Pd, and good resistance to strong acid with a long life span. Factors affecting the extraction efficiency of CME, such as sample acidity, sample flow rate, eluent conditions and coexisting ion interference were investigated in detail. Under the optimal conditions, the limits of detection (LODs, 3σ) were 5.9 ng L- 1 for Au and 8.3 ng L- 1 for Pd, and the relative standard deviations (RSDs, c = 50 ng L-1, n = 7) were 6.5% for Au and 1.1% for Pd, respectively. The developed method was successfully applied to the determination of Au and Pd in human urine and serum samples with the recovery in the range of 84-118% for spiked samples. The developed on-line polymer monolithic CME-ICP-MS method has the advantages of rapidity, simplicity, low sample/reagent consumption, high sensitivity and is suitable for the determination of trace Au and Pd in biological samples with limited amount available and complex matrix.

Chemical vapor deposition growth

NASA Technical Reports Server (NTRS)

Ruth, R. P.; Manasevit, H. M.; Kenty, J. L.; Moudy, L. A.; Simpson, W. I.; Yang, J. J.

1976-01-01

The chemical vapor deposition (CVD) method for the growth of Si sheet on inexpensive substrate materials is investigated. The objective is to develop CVD techniques for producing large areas of Si sheet on inexpensive substrate materials, with sheet properties suitable for fabricating solar cells meeting the technical goals of the Low Cost Silicon Solar Array Project. Specific areas covered include: (1) modification and test of existing CVD reactor system; (2) identification and/or development of suitable inexpensive substrate materials; (3) experimental investigation of CVD process parameters using various candidate substrate materials; (4) preparation of Si sheet samples for various special studies, including solar cell fabrication; (5) evaluation of the properties of the Si sheet material produced by the CVD process; and (6) fabrication and evaluation of experimental solar cell structures, using standard and near-standard processing techniques.

Use of microgravity to improve the efficiency and power output of Nd-doped laser glasses

NASA Technical Reports Server (NTRS)

Ray, Chandra S.

1992-01-01

The objectives of this research are to: (1) obtain further evidence and understand the science for the reported improvement in chemical homogeneity in glasses prepared in microgravity; and (2) study the feasibility of improving the optical and fluorescence properties, particularly, the limit for Nd(+3) concentration quenching and threshold energy for laser action for laser glasses prepared in microgravity. Attention was directed to ground based investigation whose primary purpose was to determine the suitability and conditions for processing these laser glasses in space. This report describes that the scientific and technical information required for planning flight experiments for these glasses have been obtained, and the preparation for handling and analyzing post flight samples have also been taken. Instruments required for measuring the fluorescence properties of interest have been constructed. The optical and fluorescence properties for the glasses have been measured and made available for comparative property analysis.

YAlO3:Ce3+ powders: Synthesis, characterization, thermoluminescence and optical studies

NASA Astrophysics Data System (ADS)

Parganiha, Yogita; Kaur, Jagjeet; Dubey, Vikas; Shrivastava, Ravi

2015-09-01

Yttrium aluminum perovskite (YAP) is a promising high temperature ceramic material, known for its mechanical, structural and optical properties. YAP's also known as an ideal host material for solid-state lasers and phosphors. In this work, Ce3+ doped YAlO3 phosphors were synthesized by solid state reaction method, which is very suitable technique for large scale production. A prepared phosphor was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Scanning electron microscopy (SEM), Photoluminescence spectra and Thermoluminescence (TL) glow curve study. The starting reagents used for sample preparation are Y2O3, Al2O3 and CeO2, boric acid used as a flux. Ratio of Y:Al was 1:1 which shows perovskite structure confirmed by the X-ray diffraction (XRD) study. The entire prepared sample was studied by PL excitation and emission spectra. Prominent peak at 446 nm (blue emission) which shows broad emission spectra of photoluminescence. It proves that prepared phosphor can act as a single host for blue emission of light and can be used for display applications. Commission Internationale de I'Eclairage (CIE) techniques proves the blue emission of light (x = .148, y = .117). TL glow curve analysis of prepared phosphor shows the prominent peak at 189 °C for the variable UV exposure time and high temperature peak shows the more stability and less fading in the prepared phosphor. Kinetic data of prepared phosphor were evaluated by peak shape method for variable UV exposure time (5-25 min).

Poly(aryl ethers) and related polysiloxane copolymer molecular coatings: Preparation and radiation degradation

NASA Technical Reports Server (NTRS)

Mcgrath, J. E.

1982-01-01

The radiation degradation of poly(arylene ether sulfones) and related materials is studied. These basic studies are important both as a means to developing stronger, more stable matrix resins for composite materials, as well as to improve the data base in regard to chemical structure-physical property relationships. Thirty homo and copolymers were synthesized, at least partially characterized and, in several cases suitable film casting techniques were developed. Four samples were chosen for initial radiation degradation. Poly(dimethyl siloxane) soft bocks/segments can preferentially migrate to the surface of copolymer films. Since siloxanes are utilized as thermal control coatings, this form of 'molecular' coating is of interest. The chemistry for preparing such copolymers with any of the polymers described was demonstrated.

White light emission and effect of annealing on the Ho{sup 3+}–Yb{sup 3+} codoped BaCa{sub 2}Al{sub 8}O{sub 15} phosphor

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

Kumari, Astha; Rai, Vineet Kumar, E-mail: vineetkrrai@yahoo.co.in

Graphical abstract: The upconversion emission spectra of the Ho{sup 3+}/Yb{sup 3+} doped/codoped BaCa{sub 2}Al{sub 8}O{sub 15} phosphors with different doping concentrations of Ho{sup 3+}/Yb{sup 3+} ions along with UC emission spectrum of the white light emitting phosphor annealed at 800 °C. - Highlights: • BaCa{sub 2}Al{sub 8}O{sub 15} phosphors codoped with Ho{sup 3+}–Yb{sup 3+} have been prepared by combustion method. • Phosphor annealed at 800 °C, illuminate an intense white light upon NIR excitation. • The sample annealed at higher temperatures emits in the pure green region. • The colour emitted persists in the white region even at high pumpmore » power density. • Developed phosphor is suitable for making upconverters and WLEDs. - Abstract: The BaCa{sub 2}Al{sub 8}O{sub 15} (BCAO) phosphors codoped with suitable Ho{sup 3+}–Yb{sup 3+} dopant concentration prepared by combustion method illuminate an intense white light upon near infrared diode laser excitation. The structural analysis of the phosphors and the detection of impurity contents have been performed by using the X-Ray Diffraction, FESEM and FTIR analysis. The purity of white light emitted from the sample has been confirmed by the CIE chromaticity diagram. Also, the white light emitted from the sample persists with the variation of pump power density. The phosphors emit upconversion (UC) emission bands in the blue, green and red region (three primary colours required for white light emission) along with one more band in the near infrared region of the electromagnetic spectrum. On annealing the white light emitting sample at higher temperatures, the sample starts to emit green colour and also the intensity of green and red UC emission bands get enhanced largely.« less

Multilayer mounting enables long-term imaging of zebrafish development in a light sheet microscope.

PubMed

Kaufmann, Anna; Mickoleit, Michaela; Weber, Michael; Huisken, Jan

2012-09-01

Light sheet microscopy techniques, such as selective plane illumination microscopy (SPIM), are ideally suited for time-lapse imaging of developmental processes lasting several hours to a few days. The success of this promising technology has mainly been limited by the lack of suitable techniques for mounting fragile samples. Embedding zebrafish embryos in agarose, which is common in conventional confocal microscopy, has resulted in severe growth defects and unreliable results. In this study, we systematically quantified the viability and mobility of zebrafish embryos mounted under more suitable conditions. We found that tubes made of fluorinated ethylene propylene (FEP) filled with low concentrations of agarose or methylcellulose provided an optimal balance between sufficient confinement of the living embryo in a physiological environment over 3 days and optical clarity suitable for fluorescence imaging. We also compared the effect of different concentrations of Tricaine on the development of zebrafish and provide guidelines for its optimal use depending on the application. Our results will make light sheet microscopy techniques applicable to more fields of developmental biology, in particular the multiview long-term imaging of zebrafish embryos and other small organisms. Furthermore, the refinement of sample preparation for in toto and in vivo imaging will promote other emerging optical imaging techniques, such as optical projection tomography (OPT).

A simple design for microwave assisted digestion vessel with low reagent consumption suitable for food and environmental samples

NASA Astrophysics Data System (ADS)

Gholami, Mehrdad; Behkami, Shima; Zain, Sharifuddin Md.; Bakirdere, Sezgin

2016-11-01

The objective of this work is to prepare a cost-effective, low reagent consumption and high performance polytetrafluoroethylene (PTFE) vessel that is capable to work in domestic microwave for digesting food and environmental samples. The designed vessel has a relatively thicker wall compared to that of commercial vessels. In this design, eight vessels are placed in an acrylonitrile butadiene styrene (ABS) holder to keep them safe and stable. This vessel needs only 2.0 mL of HNO3 and 1.0 mL H2O2 to digest 100 mg of biological sample. The performance of this design is then evaluated with an ICP-MS instrument in the analysis of the several NIST standard reference material of milk 1849a, rice flour 1568b, spinach leave 1570a and Peach Leaves 1547 in a domestic microwave oven with inverter technology. Outstanding agreement to (SRM) values are observed by using the suggested power to time microwave program, which simulates the reflux action occurring in this closed vessel. Taking into account the high cost of commercial microwave vessels and the volume of chemicals needed for various experiments (8-10 mL), this simple vessel is cost effective and suitable for digesting food and environmental samples.

Clusters of Monoisotopic Elements for Calibration in (TOF) Mass Spectrometry

NASA Astrophysics Data System (ADS)

Kolářová, Lenka; Prokeš, Lubomír; Kučera, Lukáš; Hampl, Aleš; Peňa-Méndez, Eladia; Vaňhara, Petr; Havel, Josef

2017-03-01

Precise calibration in TOF MS requires suitable and reliable standards, which are not always available for high masses. We evaluated inorganic clusters of the monoisotopic elements gold and phosphorus (Au n +/Au n - and P n +/P n -) as an alternative to peptides or proteins for the external and internal calibration of mass spectra in various experimental and instrumental scenarios. Monoisotopic gold or phosphorus clusters can be easily generated in situ from suitable precursors by laser desorption/ionization (LDI) or matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). Their use offers numerous advantages, including simplicity of preparation, biological inertness, and exact mass determination even at lower mass resolution. We used citrate-stabilized gold nanoparticles to generate gold calibration clusters, and red phosphorus powder to generate phosphorus clusters. Both elements can be added to samples to perform internal calibration up to mass-to-charge ( m/z) 10-15,000 without significantly interfering with the analyte. We demonstrated the use of the gold and phosphorous clusters in the MS analysis of complex biological samples, including microbial standards and total extracts of mouse embryonic fibroblasts. We believe that clusters of monoisotopic elements could be used as generally applicable calibrants for complex biological samples.

Utilisation of construction and demolition waste as cemented paste backfill material for underground mine openings.

PubMed

Yılmaz, Tekin; Ercikdi, Bayram; Deveci, Hacı

2018-09-15

This study presents the utilisation of finely ground construction and demolition waste (CDW) as partial replacement (5-15 wt.%) to sulphide tailings on the short- and long-term strength, durability (i.e. no loss of strength) and microstructural properties of cemented paste backfill (CPB) over a curing period of 360 days. The CPB samples containing CDW were prepared at binder dosages of 7.5 and 8.5 wt.%, while control samples (full tailings) were only produced at 8.5 wt.% binder dosage. A total of 108 CPB samples were subjected to the unconfined compressive strength (UCS), acid/sulphate (pH, SO 4 2- ) and microstructure (MIP, XRD etc.) tests. Despite its limited contribution to the resistance of CPB to acid and sulphate attack, the use of CDW as partial replacement (5-15 wt.%) to sulphide tailings enhanced the strength properties of CPB samples by decreasing the total and macro porosity. The UCSs and pH values of CPB samples increased with increasing the CDW content in CPB mixtures, while the generation of sulphate ions (SO4 2- ) decreased irrespective of the binder dosages. Compared with control samples prepared at 8.5 wt.% binder dosage, 5.3-19.5% higher UCS values were obtained for the CPB samples containing 15 wt.% CDW prepared even at 7.5 wt.% binder dosage. Mercury intrusion porosimetry (MIP) analyses proved the beneficial effect of the use of CDW on the microstructural properties (i.e. total porosity) of CPB. These findings suggest that CDW materials can be suitably used as backfill material in the mining industry to fill underground voids created during the ore production. This offers safe disposal and hence environmentally sound management of CDW. Copyright © 2018 Elsevier Ltd. All rights reserved.

Effect of the preparation of lime putties on their properties.

PubMed

Navrátilová, Eva; Tihlaříková, Eva; Neděla, Vilém; Rovnaníková, Pavla; Pavlík, Jaroslav

2017-12-08

In the study of lime as the basic component of historical mortars and plasters, four lime putties prepared from various kinds of lime of various granulometry and by various ways of preparation were evaluated. The rheological properties and micro-morphologic changes, growing of calcite crystals, and rate of carbonation were monitored. The lime putty prepared from lump lime achieves the best rheological properties, yield stress 214.7 Pa and plastic viscosity 2.6 Pa·s. The suitability of this lime putty was checked by testing the development of calcium hydroxide and calcite crystals using scanning electron microscopy and environmental scanning electron microscopy. The disordered crystals of calcium hydroxide exhibit better carbonation resulting in the large crystals of calcite; therefore, the mortar prepared from the lump lime has the highest flexural strength and compressive strength 0.8/2.5 MPa, its carbonation is the fastest and exhibits the longest durability. Also, thanks to the micro-morphological characterization of samples in their native state by means of environmental scanning electron microscopy, the new way of lime putty preparation by mixing was proven. The preparation consists in the mechanical crash of the lime particles immediately after hydration. This enables the properties of putty prepared from lump lime to be nearly reached.

Preparation and Characterization of Microencapsulated Phase Change Materials for Use in Building Applications.

PubMed

Giro-Paloma, Jessica; Al-Shannaq, Refat; Fernández, Ana Inés; Farid, Mohammed M

2015-12-26

A method for preparing and characterizing microencapsulated phase change materials (MPCM) was developed. A comparison with a commercial MPCM is also presented. Both MPCM contained paraffin wax as PCM with acrylic shell. The melting temperature of the PCM was around 21 °C, suitable for building applications. The M-2 (our laboratory made sample) and Micronal ® DS 5008 X (BASF) samples were characterized using SEM, DSC, nano-indentation technique, and Gas Chromatography/Mass spectrometry (GC-MS). Both samples presented a 6 μm average size and a spherical shape. Thermal energy storage (TES) capacities were 111.73 J·g -1 and 99.3 J·g -1 for M-2 and Micronal ® DS 5008 X, respectively. Mechanical characterization of the samples was performed by nano-indentation technique in order to determine the elastic modulus ( E ), load at maximum displacement ( P m ), and displacement at maximum load ( h m ), concluding that M-2 presented slightly better mechanical properties. Finally, an important parameter for considering use in buildings is the release of volatile organic compounds (VOC's). This characteristic was studied at 65 °C by CG-MS. Both samples showed VOC's emission after 10 min of heating, however peaks intensity of VOC's generated from M-2 microcapsules showed a lower concentration than Micronal ® DS 5008 X.

Determination of trace/ultratrace rare earth elements in environmental samples by ICP-MS after magnetic solid phase extraction with Fe3O4@SiO2@polyaniline-graphene oxide composite.

PubMed

Su, Shaowei; Chen, Beibei; He, Man; Hu, Bin; Xiao, Zuowei

2014-02-01

A novel Fe3O4@SiO2@polyaniline-graphene oxide composite (MPANI-GO) was prepared through a simple noncovalent method and applied to magnetic solid phase extraction (MSPE) of trace rare earth elements (REEs) in tea leaves and environmental water samples followed by inductively coupled plasma mass spectrometry (ICP-MS) detection. The prepared MPANI-GO was characterized by transmission electron microscopy and vibrating sample magnetometer. Various parameters affecting MPANI-GO MSPE of REEs have been investigated. Under the optimized conditions, the limits of detection (LODs, 3σ) for REEs were in the range of 0.04-1.49 ng L(-1) and the relative standard deviations (RSDs, c=20 ng L(-1), n=7) were 1.7-6.5%. The accuracy of the proposed method was validated by analyzing a Certified Reference Material of GBW 07605 tea leaves. The method was also successfully applied for the determination of trace REEs in tea leaves and environmental water samples. The developed MPANI-GO MSPE-ICP-MS method has the advantages of simplicity, rapidity, high sensitivity, high enrichment factor and is suitable for the analysis of trace REEs in samples with complex matrix. © 2013 Elsevier B.V. All rights reserved.

Characterization of Neutron Transmutation Doped (NTD) Ge for low temperature sensor development

NASA Astrophysics Data System (ADS)

Mathimalar, S.; Singh, V.; Dokania, N.; Nanal, V.; Pillay, R. G.; Pal, S.; Ramakrishnan, S.; Shrivastava, A.; Maheshwari, Priya; Pujari, P. K.; Ojha, S.; Kanjilal, D.; Jagadeesan, K. C.; Thakare, S. V.

2015-02-01

Development of NTD Ge sensors has been initiated for low temperature (mK) thermometry in The India-based TIN detector (TIN.TIN). NTD Ge sensors are prepared by thermal neutron irradiation of device grade Ge samples at Dhruva reactor, BARC, Mumbai. Detailed measurements have been carried out in irradiated samples for estimating the carrier concentration and fast neutron induced defects. The Positron Annihilation Lifetime Spectroscopy (PALS) measurements indicated monovacancy type defects for all irradiated samples, while Channeling studies employing RBS with 2 MeV alpha particles, revealed no significant defects in the samples exposed to fast neutron fluence of ∼ 4 ×1016 /cm2 . Both PALS and Channeling studies have shown that vacuum annealing at 600 °C for ∼ 2 h is sufficient to recover the damage in the irradiated samples, thereby making them suitable for the sensor development.

Headspace solid-phase microextraction (HS-SPME) and liquid-liquid extraction (LLE): comparison of the performance in classification of ecstasy tablets. Part 2.

PubMed

Bonadio, Federica; Margot, Pierre; Delémont, Olivier; Esseiva, Pierre

2008-11-20

Headspace solid-phase microextraction (HS-SPME) is assessed as an alternative to liquid-liquid extraction (LLE) currently used for 3,4-methylenedioxymethampethamine (MDMA) profiling. Both methods were compared evaluating their performance in discriminating and classifying samples. For this purpose 62 different seizures were analysed using both extraction techniques followed by gas chromatography-mass spectroscopy (GC-MS). A previously validated method provided data for HS-SPME, whereas LLE data were collected applying a harmonized methodology developed and used in the European project CHAMP. After suitable pre-treatment, similarities between sample pairs were studied using the Pearson correlation. Both methods enable to distinguish between samples coming from the same pre-tabletting batches and samples coming from different pre-tabletting batches. This finding emphasizes the use of HS-SPME as an effective alternative to LLE, with additional advantages such as sample preparation and a solvent-free process.

Surface chemistry and catalytic performance of amorphous NiB/Hβ catalyst for n-hexane isomerization

NASA Astrophysics Data System (ADS)

Chen, Jinshe; Cai, Tingting; Jing, Xiaohui; Zhu, Lijun; Zhou, Yulu; Xiang, Yuzhi; Xia, Daohong

2016-12-01

The amorphous NiB nanoparticles were synthesized and a novel type of NiB/Hβ catalyst was prepared for the isomerization of n-hexane. The optimum preparation conditions were investigated and the effect of preparation conditions on the surface chemistry information of catalysts was characterized by XRD, N2 sorption studies, XPS, TPD and other related means. It was demonstrated that the loading amounts of NiB have effect on textural properties and the acid properties of surface. The loading amounts of NiB were also related to the amount of strong Lewis acid sites and the ratios of weak acid to strong acid of samples. Meanwhile, calcination temperatures of samples were closely associated with the structure of active components that function as metal centers. When the loading amount of NiB was 5 wt.% and calcination temperature was 200 °C, the catalyst had proper surface acidity sites and metal active sites to provide suitable synergistic effects. The mechanism for n-hexane isomerization was also investigated and the existence of unique structure of Bsbnd Nisbnd H was proved, which could provide good hydrogenation-dehydrogenation functions.

Application of inductively coupled plasma sector field mass spectrometry for low-level environmental americium-241 analysis.

PubMed

Varga, Zsolt

2007-03-28

An improved and novel sample preparation method for (241)Am analysis by inductively coupled plasma sector field mass spectrometry has been developed. The procedure involves a selective CaF(2) pre-concentration followed by an extraction chromatographic separation using TRU resin. The achieved absolute detection limit of 0.86 fg (0.11 mBq) is comparable to that of alpha spectrometry (0.1 mBq) and suitable for low-level environmental measurements. Analysis of different kinds of environmental standard reference materials (IAEA-384--Fangataufa lagoon sediment, IAEA-385--Irish Sea sediment and IAEA-308--Mixed seaweed from the Mediterranean Sea) and alpha spectrometry were used to validate the procedure. The chemical recovery of sample preparation ranged between 72 and 94%. The results obtained are in good agreement with reference values and those measured by alpha spectrometry. The proposed method offers a rapid and less labor-intensive possibility for environmental (241)Am analysis than the conventionally applied radioanalytical techniques.

Sampling silica and ferrihydrite colloids with fiberglass wicks under unsaturated conditions.

PubMed

Shira, Jason M; Williams, Barbara C; Flury, Markus; Czigány, Szabolcs; Tuller, Markus

2006-01-01

The suitability of passive capillary samplers (PCAPS) for collection of representative colloid samples under partially saturated conditions was evaluated by investigating the transport of negatively and positively charged colloids in fiberglass wicks. A synthetic pore water solution was used to suspend silica microspheres (330 nm in diameter) and ferrihydrite (172 nm in diameter) for transport experiments on fiberglass wicks. Breakthrough curves were collected for three unsaturated flow rates with silica microspheres and one unsaturated flow rate with ferrihydrite colloids. A moisture characteristic curve, relating tensiometer measurements of matric potential to moisture content, was developed for the fiberglass wick. Results indicate that retention of the silica and the ferrihydrite on the wick occurred; that is, the wicks did not facilitate quantitative sampling of the colloids. For silica microspheres, 90% of the colloids were transmitted through the wicks. For ferrihydrite, 80 to 90% of the colloids were transmitted. The mechanisms responsible for the retention of the colloids on the fiberglass wicks appeared to be physicochemical attachment and not thin-film, triple-phase entrapment, or mechanical straining. Visualization of pathways by iron staining indicates that flow is preferential at the center of twisted bundles of filaments. Although axial preferential flow in PCAPS may enhance their hydraulic suitability for sampling mobile colloids, we conclude that without specific preparation to reduce attachment or retention, fiberglass wicks should only be used for qualitative sampling of pore water colloids.

Selection of a suitable method for the preparation of polymeric nanoparticles: multi-criteria decision making approach.

PubMed

Krishnamoorthy, Kannan; Mahalingam, Manikandan

2015-03-01

The present study is aimed to select the suitable method for preparation of camptothecin loaded polymeric nanoparticles by utilizing the multi-criteria decision making method. Novel approaches of drug delivery by formulation using nanotechnology are revolutionizing the future of medicine. Recent years have witnessed unprecedented growth of research and application in the area of nanotechnology. Nanoparticles have become an important area of research in the field of drug delivery because they have the ability to deliver a wide range of drug to varying areas of body. Despite of extensive research and development, polymeric nanoparticles are frequently used to improve the therapeutic effect of drugs. A number of techniques are available for the preparation of polymeric nanoparticles. The Analytical Hierarchy Process (AHP) is a method for decision making, which are derived from individual judgements for qualitative factors, using the pair-wise comparison matrix. In AHP, a decision hierarchy is constructed with a goal, criteria and alternatives. The model uses three main criteria 1) Instrument, 2) Process and Output and 3) Cost. In addition, there are eight sub-criteria's as well as eight alternatives. Pair-wise comparison matrixes are used to obtain the overall priority weight and ranking for the selection of suitable method. Nanoprecipitation technique is the most suitable method for the preparation of camptothecin loaded polymeric nanoparticles with the highest overall priority weight of 0.297 CONCLUSION: In particular, the result indicates that the priority weights obtained from AHP could be defined as a multiple output for finding out the most suitable method for preparation of camptothecin loaded polymeric nanoparticles.

Same-day breast cancer surgery: a qualitative study of women's lived experiences.

PubMed

Greenslade, M Victoria; Elliott, Barbara; Mandville-Anstey, Sue Ann

2010-03-01

To understand the experiences of women having same-day breast cancer surgery and make recommendations to assist healthcare professionals effect change to enhance quality of care. Thematic analysis of audiotaped interviews. Outpatient departments of two city hospitals on the east coast of Canada. Purposive sample of 13 women who had undergone same-day breast cancer surgery. A constructivist approach with in-depth interviews and comparative analysis to develop and systemically organize data into four major interrelated themes and a connecting essential thread. Women's experiences with same-day breast cancer surgery. The themes of preparation, timing, supports, and community health nursing intervention were of paramount importance for effective coping and recovery. Women who had a positive experience with same-day breast cancer surgery also reported having adequate preparation, appropriate timing of preparation, strong support systems, and sufficient community health nursing intervention. Those reporting a negative experience encountered challenges in one or more of the identified theme areas. Same-day surgery is a sign of the times, and the approach to it is changing. Healthcare systems need to be responsive to such changes. Although same-day surgery for breast cancer is not suitable for every patient, women undergoing this type of surgery should be assessed individually to determine whether it is appropriate for them. Women undergoing breast cancer surgery should be screened for same-day surgery suitability. Those having same-day breast cancer surgery should be prepared adequately with timely education. Most importantly, such women should receive community health nursing follow-up for assessment, continuing education, and psychosocial support.

Comparison of sample preparation techniques and data analysis for the LC-MS/MS-based identification of proteins in human follicular fluid.

PubMed

Lehmann, Roland; Schmidt, André; Pastuschek, Jana; Müller, Mario M; Fritzsche, Andreas; Dieterle, Stefan; Greb, Robert R; Markert, Udo R; Slevogt, Hortense

2018-06-25

The proteomic analysis of complex body fluids by liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis requires the selection of suitable sample preparation techniques and optimal parameter settings in data analysis software packages to obtain reliable results. Proteomic analysis of follicular fluid, as a representative of a complex body fluid similar to serum or plasma, is difficult as it contains a vast amount of high abundant proteins and a variety of proteins with different concentrations. However, the accessibility of this complex body fluid for LC-MS/MS analysis is an opportunity to gain insights into the status, the composition of fertility-relevant proteins including immunological factors or for the discovery of new diagnostic and prognostic markers for, for example, the treatment of infertility. In this study, we compared different sample preparation methods (FASP, eFASP and in-solution digestion) and three different data analysis software packages (Proteome Discoverer with SEQUEST, Mascot and MaxQuant with Andromeda) combined with semi- and full-tryptic databank search options to obtain a maximum coverage of the follicular fluid proteome. We found that the most comprehensive proteome coverage is achieved by the eFASP sample preparation method using SDS in the initial denaturing step and the SEQUEST-based semi-tryptic data analysis. In conclusion, we have developed a fractionation-free methodical workflow for in depth LC-MS/MS-based analysis for the standardized investigation of human follicle fluid as an important representative of a complex body fluid. Taken together, we were able to identify a total of 1392 proteins in follicular fluid. © 2018 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

Beyond-use dating of lidocaine alone and in two "magic mouthwash" preparations.

PubMed

Kirk, Loren Madden; Brown, Stacy D; Luu, Yao; Ogle, Amanda; Huffman, Jessica; Lewis, Paul O

2017-05-01

Beyond-use dating (BUD) of lidocaine alone and in two "magic mouthwash" preparations stored in amber oral syringes at room temperature was determined. Two formulations of mouthwash containing oral topical lidocaine 2% (viscous), diphenhydramine 2.5 mg/mL, and aluminum hydroxide-magnesium hydroxide-simethicone were prepared in 1:1:1 and 1:2.5:2.5 ratios, divided into 3-mL samples, and stored in unit-dose oral amber syringes. Unit-dose single-product lidocaine samples were also prepared to serve as controls and stored in oral amber syringes. The lidocaine concentrations in these samples were measured periodically for 90 days. A stability-indicating high-performance liquid chromatographic method was developed and validated for system suitability, accuracy, repeatability, intermediate precision, specificity, linearity, and robustness. Based on the calculated percentages versus the initial concentration and the results from an analysis of variance comparing the two formulations, a BUD of 21 days is deemed appropriate for both magic mouthwash formulations. Based on the stability data, published safety concerns, and lack of efficacy in combination, packaging and dispensing lidocaine separately from other ingredients are recommended when administering magic mouthwash mixtures. Utilizing a 90-day BUD, lidocaine can be packaged separately from other magic mouthwash ingredients in individual dosage units and applied to the oral cavity using the swish-and-spit method. The delivery of the diphenhydramine and aluminum hydroxide-magnesium hydroxide-simethicone could be separated, allowing for a swish-and-swallow method of administration. A BUD of 21 days is recommended for lidocaine prepared with diphenhydramine and aluminum hydroxide-magnesium hydroxide-simethicone in ratios of 1:1:1 and 1:2.5:2.5 and stored at room temperature in amber oral plastic syringes. Copyright © 2017 by the American Society of Health-System Pharmacists, Inc. All rights reserved.

Towards a phenotypic screening strategy for emerging β-lactamases in Gram-negative bacilli.

PubMed

Willems, Elise; Verhaegen, Jan; Magerman, Koen; Nys, Sita; Cartuyvels, Reinoud

2013-02-01

The purpose of this manuscript was to review recent literature and guidelines regarding phenotypic detection of emerging β-lactamases [extended-spectrum β-lactamases (ESBLs), AmpC β-lactamases and carbapenemases] in Gram-negative bacilli (GNB) in order to formulate recommendations on best practice to screen for them. We conclude that chromogenic ESBL screening agar plates are suitable to screen for ESBL-producing Enterobacteriaceae directly from clinical samples. Furthermore, ceftazidime (CAZ) and ceftriaxone or cefotaxime (CTX) are the indicator antimicrobial agents of choice for ESBL detection in GNB. In non-inducible Enterobacteriaceae, the combined double-disk synergy test (CDDST) with at least CTX and CAZ and additionally cefepime as indicators is the preferred ESBL confirmation assay. The two most suitable ESBL confirmation strategies in AmpC co-producing Enterobacteriaceae are adapted CDDSTs: (i) with addition of 3-aminophenylboronic acid to CTX and CAZ disks; and (ii) with addition of cloxacillin (CLOX) to Mueller-Hinton agar. Reduced cefoxitin susceptibility and decreased susceptibility to cefotetan are regarded as suitable screening tests for plasmid-mediated and derepressed AmpC production. A CLOX-based CDDST with CTX and CAZ as indicators is considered to be the best AmpC confirmation assay. Finally, in Enterobacteriaceae isolates we suggest to screen for carbapenemases with a 0.5 μg/mL meropenem screening breakpoint. For class A carbapenemase confirmation, the home-prepared as well as the commercially available boronic acid-based CDDST can be considered. For metallo-β-lactamase confirmation, ethylene diamine tetra-acetic-acid-based home-prepared assays are recommended. The most suitable method (CDDST or DDST) and indicator antimicrobial agent(s) vary depending on the bacterial genus. Copyright © 2012 Elsevier B.V. and the International Society of Chemotherapy. All rights reserved.

Multilaboratory trial for determination of ceftiofur residues in bovine and swine kidney and muscle, and bovine milk.

PubMed

Hornish, Rex E; Hamlow, Philip J; Brown, Scott A

2003-01-01

A multilaboratory trial for determining ceftiofur-related residues in bovine and swine kidney and muscle, and bovine milk was conducted following regulatory guidelines of the U.S. Food and Drug Administration, Center for Veterinary Medicine. The methods convert all desfuroylceftiofur-related residues containing the intact beta-lactam ring to desfuroylceftiofur acetamide to establish ceftiofur residues in tissues. Four laboratories analyzed 5 sets of samples for each tissue. Each sample set consisted of a control/blank sample and 3 control samples fortified with ceftiofur at 0.5 Rm, Rm, and 2 Rm, respectively, where Rm is the U.S. tolerance assigned for ceftiofur residue in each tissue/matrix: 0.100 microg/mL for milk, 8.0 microg/g for kidney (both species), 1.0 microg/g for bovine muscle, and 2.0 microg/g for swine muscle. Each sample set also contained 2 samples of incurred-residue tissues (one > Rm and one < Rm) from animals treated with ceftiofur hydrochloride. All laboratories completed the method trial after a familiarization phase and test of system suitability in which they demonstrated > 80% recovery in pretrial fortified test samples. Results showed that the methods met all acceptable performance criteria for recovery, accuracy, and precision. Although sample preparation was easy, solid-phase extraction cartridge performance must be carefully evaluated before samples are processed. The liquid chromatography detection system was easily set up; however, the elution profile may require slight modifications. The procedures could clearly differentiate between violative (> Rm) and nonviolative (< Rm) ceftiofur residues. Participating laboratories found the procedures suitable for ceftiofur residue determination.

Detection of cytomegalovirus (CMV) DNA in EDTA whole-blood samples: evaluation of the quantitative artus CMV LightCycler PCR kit in conjunction with automated sample preparation.

PubMed

Michelin, Birgit D A; Hadzisejdic, Ita; Bozic, Michael; Grahovac, Maja; Hess, Markus; Grahovac, Blazenka; Marth, Egon; Kessler, Harald H

2008-04-01

Whole blood has been found to be a reliable matrix for the detection and quantitation of cytomegalovirus (CMV) DNA. In this study, the performance of the artus CMV LightCycler (LC) PCR kit in conjunction with automated sample preparation on a BioRobot EZ1 workstation was evaluated. The accuracy, linearity, analytical sensitivity, and inter- and intra-assay variations were determined. A total of 102 clinical EDTA whole-blood samples were investigated, and results were compared with those obtained with the in vitro diagnostics (IVD)/Conformité Européene (CE)-labeled CMV HHV6,7,8 R-gene quantification kit. When the accuracy of the new kit was tested, seven of eight results were found to be within +/-0.5 log(10) unit of the expected panel results. Determination of linearity resulted in a quasilinear curve over more than 5 log units. The lower limit of detection of the assay was determined to be 139 copies/ml in EDTA whole blood. The interassay variation ranged from 15 to 58%, and the intra-assay variation ranged from 7 to 35%. When clinical samples were tested and the results were compared with those of the routinely used IVD/CE-labeled assay, 53 samples tested positive and 13 samples tested negative by both of the assays. One sample was found to be positive with the artus CMV LC PCR kit only, and 35 samples tested positive with the routinely used assay only. The majority of discrepant results were found with low-titer samples. In conclusion, use of the artus CMV LC PCR kit in conjunction with automated sample preparation on the BioRobot EZ1 workstation may be suitable for the detection and quantitation of CMV DNA in EDTA whole blood in the routine low-throughput laboratory; however, low-positive results may be missed by this assay.

[Study on the appropriate parameters of automatic full crown tooth preparation for dental tooth preparation robot].

PubMed

Yuan, F S; Wang, Y; Zhang, Y P; Sun, Y C; Wang, D X; Lyu, P J

2017-05-09

Objective: To further study the most suitable parameters for automatic full crown preparation using oral clinical micro robot. Its purpose is to improve the quality of automated tooth preparing for the system and to lay the foundation for clinical application. Methods: Twenty selected artificial resin teeth were used as sample teeth. The micro robot automatic tooth preparation system was used in dental clinic to control the picosecond laser beam to complete two dimensional cutting on the resin tooth sample according to the motion planning path. Using the laser scanning measuring microscope, each layer of cutting depth values was obtained and the average value was calculated. The monolayer cutting depth was determined. The three-dimensional (3D) data of the target resin teeth was obtained using internal scanner, and the CAD data of full-crown tooth preparation was designed by CAD self-develged software. According to the depth of the single layer, 11 complete resin teeth in phantom head were automatically prepared by the robot controlling the laser focused spot in accordance with the layer-cutting way. And the accuracy of resin tooth preparation was evaluated with the software. Using the same method, monolayer cutting depth parameter for cutting dental hard tissue was obtained. Then 15 extracted mandibular and maxillary first molars went through automatic full crown tooth preparation. And the 3D data of tooth preparations were obtained with intra oral scanner. The software was used to evaluate the accuracy of tooth preparation. Results: The results indicated that the single cutting depth of cutting resin teeth and in vitro teeth by picosecond laser were (60.0±2.6) and (45.0±3.6) μm, respectively. Using the tooth preparation robot, 11 artificial resin teeth and 15 complete natural teeth were automatically prepared, and the average time were (13.0±0.7), (17.0±1.8) min respectively. Through software evaluation, the average preparation depth of the occlusal surface of 11 resin teeth was approximately (2.089±0.026) mm, the error was about (0.089±0.026) mm; the average convergence angle was about 6.56°±0.30°, the error was about 0.56°±0.30°. Compared with the target preparation shape, the average shape error of the 11 resin tooth preparations was about 0.02-0.11 mm. And the average preparation depth of the occlusal surface of 15 natural teeth was approximately (2.097±0.022) mm, the error was about (0.097±0.022) mm; the average convergence angle was about 6.98°±0.35°, the error was about 0.98°±0.35°. Compared with the target preparation shape, the average shape error of the 15 natural tooth preparations was about 0.05-0.17 mm. Conclusions: The experimental results indicate that the automatic tooth preparation for resin teeth and the teeth were completed according to the specific parameters of the single cutting depth by the micro robot controlling picosecond laser respectively, its preparation accuracy met the clinical needs. And the suitability of the parameter was confirmed.

Pharmacokinetic behavior of intravitreal triamcinolone acetonide prepared by a hospital pharmacy.

PubMed

Oishi, Masako; Maeda, Shinichiro; Hashida, Noriyasu; Ohguro, Nobuyuki; Tano, Yasuo; Kurokawa, Nobuo

2008-01-01

We developed a new hospital pharmaceutical preparation of triamcinolone acetonide (TA) for intravitreal injections using sodium hyaluronate as the vehicle. The purpose of this study was to compare the pharmacokinetic behavior of this hospital pharmacy preparation of TA (HPP-TA) to that of a commercial preparation of TA (CP-TA) in rats. We injected the two preparations of TA into the vitreous humor of male Wistar rats. The rats were killed between days 1 and 21, and the concentration of TA in the vitreous was measured by high-performance liquid chromatography to determine the pharmacokinetic parameters. We also examined the microscopic appearance of the TA particles in these preparations. The elimination half-life was 6.08 days for the CP-TA and 5.78 days for the HPP-TA. A two-compartment model was suitable to approximate the pharmacokinetic behavior of HPP-TA in the vitreous body, but this model was not suitable for CP-TA, because its pharmacokinetic behavior was not sufficiently stable. The particle size of CP-TA was largest, followed by TA powder and HPP-TA. Many particles were agglutinated in the CP-TA preparation, whereas the TA particles were fine and dispersed in the HPP-TA medium. The TA particle size and the suspension medium are likely important factors in the preparation of a safe and stable suspension of TA. HPP-TA satisfied these requirements and should be suitable for clinical use.

A hybrid approach to device integration on a genetic analysis platform

NASA Astrophysics Data System (ADS)

Brennan, Des; Jary, Dorothee; Kurg, Ants; Berik, Evgeny; Justice, John; Aherne, Margaret; Macek, Milan; Galvin, Paul

2012-10-01

Point-of-care (POC) systems require significant component integration to implement biochemical protocols associated with molecular diagnostic assays. Hybrid platforms where discrete components are combined in a single platform are a suitable approach to integration, where combining multiple device fabrication steps on a single substrate is not possible due to incompatible or costly fabrication steps. We integrate three devices each with a specific system functionality: (i) a silicon electro-wetting-on-dielectric (EWOD) device to move and mix sample and reagent droplets in an oil phase, (ii) a polymer microfluidic chip containing channels and reservoirs and (iii) an aqueous phase glass microarray for fluorescence microarray hybridization detection. The EWOD device offers the possibility of fully integrating on-chip sample preparation using nanolitre sample and reagent volumes. A key challenge is sample transfer from the oil phase EWOD device to the aqueous phase microarray for hybridization detection. The EWOD device, waveguide performance and functionality are maintained during the integration process. An on-chip biochemical protocol for arrayed primer extension (APEX) was implemented for single nucleotide polymorphism (SNiP) analysis. The prepared sample is aspirated from the EWOD oil phase to the aqueous phase microarray for hybridization. A bench-top instrumentation system was also developed around the integrated platform to drive the EWOD electrodes, implement APEX sample heating and image the microarray after hybridization.

Extemporaneous (magistral) preparation of oral medicines for children in European hospitals.

PubMed

Brion, F; Nunn, A J; Rieutord, A

2003-04-01

To evaluate methods of preparation of oral medicines in European children's hospitals when drugs prescribed are unlicensed or off-label, and to determine whether such extemporaneously prepared medicines are available as suitable, authorized products in other countries. A questionnaire was distributed to 41 hospital pharmacists in 18 European countries, requesting information on the most frequent extemporaneously prepared oral liquid, powder and capsule medicines, and on their formulation and stability. Information was gathered on the availability of suitable authorized forms of these medicines in other European countries, the USA and Australia. 21 questionnaires from 16 countries returned showed that the methods of extemporaneous preparation vary in different European countries with, for example, liquid preparations predominating in England and Sweden, capsules in France and Spain, and powders in Finland and Italy. The top 20 preparations are made in many different strengths and formulations. The same drug may be prepared in liquid, capsule or powder form, depending on the country. Many of the extemporaneous preparations were available as suitable authorized paediatric medicines in other countries. The quality of information available on formulation and stability was limited, and there was concern about the availability and quality of chemical ingredients. Preparation of children's oral medicines is subject to much variation in hospitals throughout Europe and there is little harmonization of formulations or information on stability of products. The European Union could be the focus for improving the availability of appropriate authorized medicines for children and ensuring that when extemporaneous preparation is necessary it is of a common high standard.

Preparation of novel alumina nanowire solid-phase microextraction fiber coating for ultra-selective determination of volatile esters and alcohols from complicated food samples.

PubMed

Zhang, Zhuomin; Ma, Yunjian; Wang, Qingtang; Chen, An; Pan, Zhuoyan; Li, Gongke

2013-05-17

A novel alumina nanowire (ANW) solid-phase microextraction (SPME) fiber coating was prepared by a simple and rapid anodization-chemical etching method for ultra-selective determination of volatile esters and alcohols from complicated food samples. Preparation conditions for ANW SPME fiber coating including corrosion solution concentration and corrosion time were optimized in detail for better surface morphology and higher surface area based on scanning electron microscope (SEM). Under the optimum conditions, homogeneous alumina nanowire structure of ANW SPME fiber coating was achieved with the average thickness of 20 μm around. Compared with most of commercial SPME fiber coatings, ANW SPME fiber coatings achieved the higher extraction capacity and special selectivity for volatile esters and alcohols. Finally, an efficient gas sampling technique based on ANW SPME fiber coating as the core was established and successfully applied for the ultra-selective determination of trace volatile esters and alcohols from complicated banana and fermented glutinous rice samples coupled with gas chromatography/mass spectrometry (GC/MS) detection. It was interesting that 25 esters and 2 alcohols among 30 banana volatile organic compounds (VOCs) identified and 4 esters and 7 alcohols among 13 identified VOCs of fermented glutinous rice were selectively sampled by ANW SPME fiber coatings. Furthermore, new analytical methods for the determination of some typical volatile esters and alcohols from banana and fermented glutinous rice samples at specific storage or brewing phases were developed and validated. Good recoveries for banana and fermented glutinous rice samples were achieved in range of 108-115% with relative standard deviations (RSDs) of 2.6-6.7% and 80.0-91.8% with RSDs of 0.3-1.3% (n=3), respectively. This work proposed a novel and efficient gas sampling technique of ANW SPME which was quite suitable for ultra-selectively sampling trace volatile esters and alcohols from complicated food samples. Copyright © 2013 Elsevier B.V. All rights reserved.

A simplified and efficient method for the analysis of fatty acid methyl esters suitable for large clinical studies.

PubMed

Masood, Athar; Stark, Ken D; Salem, Norman

2005-10-01

Conventional sample preparation for fatty acid analysis is a complicated, multiple-step process, and gas chromatography (GC) analysis alone can require >1 h per sample to resolve fatty acid methyl esters (FAMEs). Fast GC analysis was adapted to human plasma FAME analysis using a modified polyethylene glycol column with smaller internal diameters, thinner stationary phase films, increased carrier gas linear velocity, and faster temperature ramping. Our results indicated that fast GC analyses were comparable to conventional GC in peak resolution. A conventional transesterification method based on Lepage and Roy was simplified to a one-step method with the elimination of the neutralization and centrifugation steps. A robotics-amenable method was also developed, with lower methylation temperatures and in an open-tube format using multiple reagent additions. The simplified methods produced results that were quantitatively similar and with similar coefficients of variation as compared with the original Lepage and Roy method. The present streamlined methodology is suitable for the direct fatty acid analysis of human plasma, is appropriate for research studies, and will facilitate large clinical trials and make possible population studies.

The monolithic carbon aerogels and aerogel composites for electronics and thermal protection applications

NASA Astrophysics Data System (ADS)

Lu, Sheng; Guo, Hui; Zhou, Yugui; Liu, Yuanyuan; Jin, Zhaoguo; Liu, Bin; Zhao, Yingmin

2017-09-01

Monolithic carbon aerogels have been prepared by condensation polymerization and high temperature pyrolysis. The morphology of carbon aerogels are characterized by SEM. The pore structure is characterized by N2 adsorption-desorption technique. Monolithic carbon aerogels are mesoporous nanomaterials. Carbon fiber reinforced carbon aerogel composites are prepared by in-situ sol-gel process. Fiber reinforced carbon aerogel composites are of high mechanical strength. The thermal response of the fiber reinforced aerogel composite samples are tested in an arc plasma wind tunnel. Carbon aerogel composites show good thermal insulation capability and high temperature resistance in inert atmosphere even at ultrahigh temperature up to 1800 °C. The results show that they are suitable for applications in electrodes for supercapacitors/ Lithium-ion batteries and aerospace thermal protection area.

Preparation of a Carbon Doped Tissue-Mimicking Material with High Dielectric Properties for Microwave Imaging Application

PubMed Central

Lan, Siang-Wen; Weng, Min-Hang; Yang, Ru-Yuan; Chang, Shoou-Jinn; Chung, Yaoh-Sien; Yu, Tsung-Chih; Wu, Chun-Sen

2016-01-01

In this paper, the oil-in-gelatin based tissue-mimicking materials (TMMs) doped with carbon based materials including carbon nanotube, graphene ink or lignin were prepared. The volume percent for gelatin based mixtures and oil based mixtures were both around 50%, and the doping amounts were 2 wt %, 4 wt %, and 6 wt %. The effect of doping material and amount on the microwave dielectric properties including dielectric constant and conductivity were investigated over an ultra-wide frequency range from 2 GHz to 20 GHz. The coaxial open-ended reflection technology was used to evaluate the microwave dielectric properties. Six measured values in different locations of each sample were averaged and the standard deviations of all the measured dielectric properties, including dielectric constant and conductivity, were less than one, indicating a good uniformity of the prepared samples. Without doping, the dielectric constant was equal to 23 ± 2 approximately. Results showed with doping of carbon based materials that the dielectric constant and conductivity both increased about 5% to 20%, and the increment was dependent on the doping amount. By proper selection of doping amount of the carbon based materials, the prepared material could map the required dielectric properties of special tissues. The proposed materials were suitable for the phantom used in the microwave medical imaging system. PMID:28773678

Quantification of Bone Growth Rate Variability in Rats Exposed to Micro- (near zero G) and Macrogravity (2G)

NASA Technical Reports Server (NTRS)

Bromage, Timothy G.; Doty, Stephen B.; Smolyar, Igor; Holton, Emily

1996-01-01

Our stated primary objective is to quantify the growth rate variability of rat lamellar bone exposed to micro and macrogravity (2G). The primary significance of the proposed work is that an elegant method will be established that unequivocally characterizes the morphological consequences of gravitational factors on developing bone. The integrity of this objective depends upon our successful preparation of thin sections suitable for imaging individual bone lamellae, and our imaging and quantitation of growth rate variability in populations of lamellae from individual bone samples.

Module Degradation Mechanisms Studied by a Multi-Scale Approach

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

Johnston, Steve; Al-Jassim, Mowafak; Hacke, Peter

2016-11-21

A key pathway to meeting the Department of Energy SunShot 2020 goals is to reduce financing costs by improving investor confidence through improved photovoltaic (PV) module reliability. A comprehensive approach to further understand and improve PV reliability includes characterization techniques and modeling from module to atomic scale. Imaging techniques, which include photoluminescence, electroluminescence, and lock-in thermography, are used to locate localized defects responsible for module degradation. Small area samples containing such defects are prepared using coring techniques and are then suitable and available for microscopic study and specific defect modeling and analysis.

Development of molecular tests for the detection of ILAR and latent viruses in fruit trees.

PubMed

Roussel, S; Kummert, J; Dutrecq, O; Lepoivre, P; Jijakli, M H

2004-01-01

The detection throughout the year of latent and ILAR viruses in fruit tress by classical serological tests appear to be unreliable. We have developed RT-PCR tests for a reliable detection of latent and ILAR viruses in fruit trees. These assays were then simplified to allow the direct use of crude plant extracts instead of total RNA preparations, and the analyses of pooled samples. In this way, such RT-PCR protocols are suitable for a routine diagnosis of latent and ILAR viruses in fruit tree certification.

Selection of a Suitable Method for the Preparation of Polymeric Nanoparticles: Multi-Criteria Decision Making Approach

PubMed Central

Krishnamoorthy, Kannan; Mahalingam, Manikandan

2015-01-01

Purpose: The present study is aimed to select the suitable method for preparation of camptothecin loaded polymeric nanoparticles by utilizing the multi-criteria decision making method. Novel approaches of drug delivery by formulation using nanotechnology are revolutionizing the future of medicine. Recent years have witnessed unprecedented growth of research and application in the area of nanotechnology. Nanoparticles have become an important area of research in the field of drug delivery because they have the ability to deliver a wide range of drug to varying areas of body. Methods: Despite of extensive research and development, polymeric nanoparticles are frequently used to improve the therapeutic effect of drugs. A number of techniques are available for the preparation of polymeric nanoparticles. The Analytical Hierarchy Process (AHP) is a method for decision making, which are derived from individual judgements for qualitative factors, using the pair-wise comparison matrix. In AHP, a decision hierarchy is constructed with a goal, criteria and alternatives. Results: The model uses three main criteria 1) Instrument, 2) Process and Output and 3) Cost. In addition, there are eight sub-criteria’s as well as eight alternatives. Pair-wise comparison matrixes are used to obtain the overall priority weight and ranking for the selection of suitable method. Nanoprecipitation technique is the most suitable method for the preparation of camptothecin loaded polymeric nanoparticles with the highest overall priority weight of 0.297 Conclusion: In particular, the result indicates that the priority weights obtained from AHP could be defined as a multiple output for finding out the most suitable method for preparation of camptothecin loaded polymeric nanoparticles. PMID:25789220

Sources and preparation of data for assessing trends in concentrations of pesticides in streams of the United States, 1992–2010

USGS Publications Warehouse

Martin, Jeffrey D.; Eberle, Michael; Nakagaki, Naomi

2011-01-01

This report updates a previously published water-quality dataset of 44 commonly used pesticides and 8 pesticide degradates suitable for a national assessment of trends in pesticide concentrations in streams of the United States. Water-quality samples collected from January 1992 through September 2010 at stream-water sites of the U.S. Geological Survey (USGS) National Water-Quality Assessment (NAWQA) Program and the National Stream Quality Accounting Network (NASQAN) were compiled, reviewed, selected, and prepared for trend analysis. The principal steps in data review for trend analysis were to (1) identify analytical schedule, (2) verify sample-level coding, (3) exclude inappropriate samples or results, (4) review pesticide detections per sample, (5) review high pesticide concentrations, and (6) review the spatial and temporal extent of NAWQA pesticide data and selection of analytical methods for trend analysis. The principal steps in data preparation for trend analysis were to (1) select stream-water sites for trend analysis, (2) round concentrations to a consistent level of precision for the concentration range, (3) identify routine reporting levels used to report nondetections unaffected by matrix interference, (4) reassign the concentration value for routine nondetections to the maximum value of the long-term method detection level (maxLT-MDL), (5) adjust concentrations to compensate for temporal changes in bias of recovery of the gas chromatography/mass spectrometry (GCMS) analytical method, and (6) identify samples considered inappropriate for trend analysis. Samples analyzed at the USGS National Water Quality Laboratory (NWQL) by the GCMS analytical method were the most extensive in time and space and, consequently, were selected for trend analysis. Stream-water sites with 3 or more water years of data with six or more samples per year were selected for pesticide trend analysis. The selection criteria described in the report produced a dataset of 21,988 pesticide samples at 212 stream-water sites. Only 21,144 pesticide samples, however, are considered appropriate for trend analysis.

An Improved LC-MS/MS Method for Simultaneous Determination of the Eleven Bioactive Constituents for Quality Control of Radix Angelicae Pubescentis and Its Related Preparations

PubMed Central

Li, Jin; Zhang, Qiu-Hong; He, Jun; Liu, Er-wei; Gao, Xiu-mei; Chang, Yan-xu

2015-01-01

An improved LC-MS/MS method was developed for simultaneous determination of eleven bioactive constituents of Radix Angelicae Pubescentis and its related preparations. It was the first report on the quantification of bioactive constituents in different preparations of Radix Angelicae Pubescentis by LC-MS/MS analytical method. These samples were separated with an Agilent Zorbax Extend reversed-phase C18 column (1.8 μm, 4.6 × 100 mm) by linear gradient elution using aqueous ammonium acetate and acetonitrile as mobile phase. The flow rate was 0.3 mL min−1. The eleven bioactive constituents showed good regression (R > 0.990) within test ranges and the recoveries were in the range of 87.1–110%. The limit of detections and quantifications for most of the major constituents were less than 0.5 and 1.0 ng mL−1, respectively. All results indicated that the developed method could be readily utilized as a suitable quality control method for Radix Angelicae Pubescentis and related preparations. PMID:26078992

Observation of asphalt binder microstructure with ESEM.

PubMed

Mikhailenko, P; Kadhim, H; Baaj, H; Tighe, S

2017-09-01

The observation of asphalt binder with the environmental scanning electron microscope (ESEM) has shown the potential to observe asphalt binder microstructure and its evolution with binder aging. A procedure for the induction and identification of the microstructure in asphalt binder was established in this study and included sample preparation and observation parameters. A suitable heat-sampling asphalt binder sample preparation method was determined for the test and several stainless steel and Teflon sample moulds developed, finding that stainless steel was the preferable material. The magnification and ESEM settings conducive to observing the 3D microstructure were determined through a number of observations to be 1000×, although other magnifications could be considered. Both straight run binder (PG 58-28) and an air blown oxidised binder were analysed; their structures being compared for their relative size, abundance and other characteristics, showing a clear evolution in the fibril microstructure. The microstructure took longer to appear for the oxidised binder. It was confirmed that the fibril microstructure corresponded to actual characteristics in the asphalt binder. Additionally, a 'bee' micelle structure was found as a transitional structure in ESEM observation. The test methods in this study will be used for more comprehensive analysis of asphalt binder microstructure. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Improvement in the performance of external quality assessment in Korean HIV clinical laboratories using unrecalcified human plasma.

PubMed

Wang, Jin-Sook; Kee, Mee-Kyung; Choi, Byeong-Sun; Kim, Chan-Wha; Kim, Hyon-Suk; Kim, Sung Soon

2012-01-01

The external quality assessment schemes (EQAS) organizer provides a suitable program to monitor and improve the quality of human immunodeficiency virus (HIV) testing laboratories with EQAS panels prepared under various conditions. The aim of the current study was to investigate the effects of human plasma samples on the EQAS results of HIV obtained from hospital-based clinical laboratories. From 2007 to 2009, HIV EQAS panels consisted of four to six samples that consisted of undiluted positive and negative samples and were provided to laboratories twice per year. Up until the first half EQAS in 2008, EQAS panel materials were obtained by converting acid citrate dextrose treated plasma to serum via chemical treatment with CaCl2. Beginning with the second EQAS in 2008, all materials were prepared without the defibrination process. Approximately 300 HIV clinical laboratories participated in this program. The overall performance of clinical laboratories was shown to be improved when using unrecalcified plasma panels compared with recalcified panels. Significant differences were observed in EIA analyses of plasma for both positive (p<0.001) and negative (p<0.001) samples between the recalcified and unrecalcified groups. Our finding suggested that defibrination status of EQAS panels might affect the results of anti-HIV EQAS of Korean HIV testing laboratories.

Dip-coated ZrO2-Y2O3 coatings tested in molten salts for CSP applications

NASA Astrophysics Data System (ADS)

Pérez, Francisco Javier; Encinas-Sánchez, Víctor; Lasanta, María Isabel; de Miguel, María Teresa; García-Martín, Gustavo

2017-06-01

In the present work, the behaviour of ZrO2 - Y2O3 coatings in contact with molten salts at 500 °C has been studied. The coatings were prepared by sol-gel and deposited by dip-coating on AISI 304 specimens previously prepared by sanding and polishing. The behaviour in contact with molten salt was studied through static corrosion tests by the immersion of the coated samples in an alkali-nitrate mixture with a composition of 60 wt.% NaNO3/40 wt.% KNO3 (commonly known as Solar Salt). Prior to test, the deposited coatings were characterized using Scanning Electron Microscopy and X-Ray Diffraction, showing a compacted, homogeneous and uniform aspect and t-YSZ as main component. After corrosion tests, the samples were characterized via gravimetric, Scanning Electron Microscopy and X-Ray Diffraction. The results show a good behaviour of the coated samples compared with the bare coupon samples. However after 1000 h of testing m-ZrO2 appears in the composition,. At this preliminary study, results confirm the suitability of ZrO2 - Y2O3 coatings in solar applications after those working hours, although it is necessary to optimize the coating and study its behaviour at longer times.

Processing, Mechanical and Optical Properties of Additive-Free ZrC Ceramics Prepared by Spark Plasma Sintering.

PubMed

Musa, Clara; Licheri, Roberta; Orrù, Roberto; Cao, Giacomo; Sciti, Diletta; Silvestroni, Laura; Zoli, Luca; Balbo, Andrea; Mercatelli, Luca; Meucci, Marco; Sani, Elisa

2016-06-18

In the present study, nearly fully dense monolithic ZrC samples are produced and broadly characterized from microstructural, mechanical and optical points of view. Specifically, 98% dense products are obtained by Spark Plasma Sintering (SPS) after 20 min dwell time at 1850 °C starting from powders preliminarily prepared by Self-propagating High-temperature Synthesis (SHS) followed by 20 min ball milling. A prolonged mechanical treatment up to 2 h of SHS powders does not lead to appreciable benefits. Vickers hardness of the resulting samples (17.5 ± 0.4 GPa) is reasonably good for monolithic ceramics, but the mechanical strength (about 250 MPa up to 1000 °C) could be further improved by suitable optimization of the starting powder characteristics. The very smoothly polished ZrC specimen subjected to optical measurements displays high absorption in the visible-near infrared region and low thermal emittance at longer wavelengths. Moreover, the sample exhibits goodspectral selectivity (2.1-2.4) in the 1000-1400 K temperature range. These preliminary results suggest that ZrC ceramics produced through the two-step SHS/SPS processing route can be considered as attractive reference materials for the development of innovative solar energy absorbers.

Influence of nickel substitution on crystal structure and magnetic properties of strontium ferrite preparation via sol-gel auto-combustion route

NASA Astrophysics Data System (ADS)

Roohani, Ebrahim; Arabi, Hadi; Sarhaddi, Reza

2018-01-01

In this research, SrFe12-xNixO19 (x = 0 - 1) hexagonal ferrites were prepared by sol-gel auto-combustion method. Effect of Ni substitution on structural, morphological and magnetic properties of nanoparticles was investigated by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM), respectively. The XRD results confirmed that all samples with x ≤ 0.5 have single phase M-type strontium ferrite structure, whereas for the SrFe12-xNixO19 samples with x > 0.5, the spinel NiFe2O4 phase has also appeared. The lattice parameters and crystallite sizes of the powders were concluded from the XRD data and Williamson-Hall method. Magnetic analyses showed that the coercivity of powders decreased from 5672 Oe to 639 Oe while the saturation magnetization increased from 74 emu/g to 81 emu/g with nickel substitution. The results of this study suggest that the strontium hexaferrites doped with Ni are suitable for applications in high density magnetic recording media as well as microwave devices because of their promising magnetic properties.

Influence of CeO2 addition on the preparation of foamed glass-ceramics from high-titanium blast furnace slag

NASA Astrophysics Data System (ADS)

Zhou, Hong-ling; Feng, Ke-qin; Chen, Chang-hong; Yan, Zi-di

2018-06-01

Foamed glass-ceramics doped with cerium oxide (CeO2) were successfully prepared from high-titanium blast furnace slag by one-step sintering. The influence of CeO2 addition (1.5wt%-3.5wt%) on the crystalline phases, microstructure, and properties of foamed glass-ceramics was studied. Results show that CeO2 improves the stability of the glass phase and changes the two-dimensional crystallization mechanism into three-dimensional one. XRD analysis indicates the presence of Ca(Mg, Fe)Si2O6 and Ca(Ti, Mg, Al)(Si, Al)2O6 in all sintered samples. Added with CeO2, TiCeO4 precipitates, and crystallinity increases, leading to increased thickness of pore walls and uniform pores. The comprehensive properties of foamed glass-ceramics are better than that of samples without CeO2. In particular, the sample added with a suitable amount of CeO2 (2.5wt%) exhibits bulk density that is similar to and compressive strength (14.9 MPa) that is more than twice of foamed glass-ceramics without CeO2.

Advantages of automation in plasma sample preparation prior to HPLC/MS/MS quantification: application to the determination of cilazapril and cilazaprilat in a bioequivalence study.

PubMed

Kolocouri, Filomila; Dotsikas, Yannis; Apostolou, Constantinos; Kousoulos, Constantinos; Soumelas, Georgios-Stefanos; Loukas, Yannis L

2011-01-01

An HPLC/MS/MS method characterized by complete automation and high throughput was developed for the determination of cilazapril and its active metabolite cilazaprilat in human plasma. All sample preparation and analysis steps were performed by using 2.2 mL 96 deep-well plates, while robotic liquid handling workstations were utilized for all liquid transfer steps, including liquid-liquid extraction. The whole procedure was very fast compared to a manual procedure with vials and no automation. The method also had a very short chromatographic run time of 1.5 min. Sample analysis was performed by RP-HPLC/MS/MS with positive electrospray ionization using multiple reaction monitoring. The calibration curve was linear in the range of 0.500-300 and 0.250-150 ng/mL for cilazapril and cilazaprilat, respectively. The proposed method was fully validated and proved to be selective, accurate, precise, reproducible, and suitable for the determination of cilazapril and cilazaprilat in human plasma. Therefore, it was applied to a bioequivalence study after per os administration of 2.5 mg tablet formulations of cilazapril.

A recombinase polymerase amplification assay for rapid detection of Crimean-Congo Haemorrhagic fever Virus infection

PubMed Central

Afrough, Babak; Mullojonova, Manija; Dzhuraeva, Viktoriya; Tishkova, Farida; Hewson, Roger

2017-01-01

Background Crimean-Congo Haemorrhagic fever Virus (CCHFV) is a rapidly emerging vector-borne pathogen and the cause of a virulent haemorrhagic fever affecting large parts of Europe, Africa, the Middle East and Asia. Methodology/principle findings An isothermal recombinase polymerase amplification (RPA) assay was successfully developed for molecular detection of CCHFV. The assay showed rapid (under 10 minutes) detection of viral extracts/synthetic virus RNA of all 7 S-segment clades of CCHFV, with high target specificity. The assay was shown to tolerate the presence of inhibitors in crude preparations of mock field samples, indicating that this assay may be suitable for use in the field with minimal sample preparation. The CCHFV RPA was successfully used to screen and detect CCHFV positives from a panel of clinical samples from Tajikistan. Conclusions/significance The assay is a rapid, isothermal, simple-to-perform molecular diagnostic, which can be performed on a light, portable real-time detection device. It is ideally placed therefore for use as a field-diagnostic or in-low resource laboratories, for monitoring of CCHF outbreaks at the point-of-need, such as in remote rural regions in affected countries. PMID:29028804

Multicomponent analysis of fat- and water-soluble vitamins and auxiliary substances in multivitamin preparations by qNMR.

PubMed

Eiff, Julia; Monakhova, Yulia B; Diehl, Bernd W K

2015-04-01

A nuclear magnetic resonance (NMR) spectroscopic method was tested to control 12 vitamins and accompanying substances in multivitamin preparations. The limits of detection (LODs) and limits of quantification (LOQs) varied in the 9.0-77.0 mg/kg and in the 34.5-93.5 mg/kg range, respectively. The coefficients of variation (CVs) ranged between 0.9% and 12%. The (1)H NMR spectra showed linearity for the 140-260 mg sample weight (R(2) > 0.918). The NMR spectra of multivitamin preparations showed the presence of different degradation products of ascorbic acid. The NMR method was applied to 13 different multivitamin preparations including tablets, capsules, and effervescent tablets with average recovery rates between 85% and 132%. A number of accompanying substances (citric acid, mannitol, saccharin, cyclamate, sum of steviol glycosides, and butylhydroxytoluene) were additionally identified and quantified. NMR was found to be suitable for the simultaneous qualitative measurement of water- and fat-soluble vitamins and accompanying substances and shows some promise for quantitative determination of at least 5 vitamins (B1, B3, B5, B6, and E) in multivitamin preparations.

Preparation of nitrogen-doped carbon tubes

DOEpatents

Chung, Hoon Taek; Zelenay, Piotr

2015-12-22

A method for synthesizing nitrogen-doped carbon tubes involves preparing a solution of cyanamide and a suitable transition metal-containing salt in a solvent, evaporating the solvent to form a solid, and pyrolyzing the solid under an inert atmosphere under conditions suitable for the production of nitrogen-doped carbon tubes from the solid. Pyrolyzing for a shorter period of time followed by rapid cooling resulted in a tubes with a narrower average diameter.

Quality changes of chicken meat jerky with different sweeteners during storage.

PubMed

Wongwiwat, Pirinya; Wattanachant, Saowakon

2015-12-01

Chicken meat jerky with high sugar content is popular intermediate-moisture meat product in Asia. Different types of sugar, sucrose and mixed sugar (sucrose: fructose: sorbitol 70: 15: 15), were evaluated to improve the quality of product. Quality changes of chicken meat jerky stored in vacuum and aerobic (33 and 75 %relative humidity, %RH) conditions were studied for suitable condition to extend shelf-life of product. The samples were determined the physical and chemical characteristics, as well as sensory evaluation during storage at room temperature. The moisture content and water activity (aw) of samples stored in 33 %RH conditions was continuously diminished during storage that related to harder texture and unacceptable quality in sensory evaluation. All samples stored in vacuum and 75 %RH condition demonstrated the lower shear force value than that stored in 33%RH condition (p < 0.05). Samples stored in vacuum condition had the lowest lipid oxidation (p < 0.05.) which corresponding to the highest scores in less rancidity and overall acceptance attributes. All samples stored in vacuum condition also had the highest acceptability in all sensory attributes (taste, rancidity, color and overall acceptance) followed by 75 %RH storage condition (p < 0.05). Samples prepared with mixed sugar could improve color and retard rancidity in chicken jerky meat product. Sample prepared with mixed sugar kept in vacuum condition had the lowest lipid oxidation and highest sensory score in overall acceptance attributes along the extended storage.

Preparation of thermo and pH-responsive polymer@Au/Fe3O4 core/shell nanoparticles as a carrier for delivery of anticancer agent

NASA Astrophysics Data System (ADS)

Ghorbani, Marjan; Hamishehkar, Hamed; Arsalani, Naser; Entezami, Ali Akbar

2015-07-01

In this work, a thermo and pH-responsive poly- N-isopropylacrylamide-co-itaconic acid containing thiol side groups were successfully synthesized to prepare Doxorubicin-loaded polymer@Au/Fe3O4 core/shell nanoparticles (DOX-NPs). Copolymer and NPs were fully characterized by FT-IR, HNMR, photo-correlation spectroscopy, SEM, X-ray diffraction, vibrating-sample magnetometer, thermal gravimetric analysis, and UV-Vis spectroscopy. The stimuli-responsive characteristics of NPs were evaluated by in vitro release study in simulated cancerous environment. The biocompatibility and cytotoxic properties of NPs and DOX-NPs are explored by MTT method. The prepared NPs with the size of 50 nm showed paramagnetic characteristics with suitable and stable dispersion at physiological medium and high loading capacity (up to 55 %) of DOX. DOX-NPs yielded a pH- and temperature-triggered release of entrapped drugs at tumor tissue environment (59 % of DOX release) compared to physiological condition (20 % of DOX release) during 48 h. In vitro cytotoxicity studies indicated that the NPs showed no cytotoxicity on A549 cells at different amounts after incubation for 72 h confirming its suitability as a drug carrier. DOX-NPs, on the other hand, caused an efficient anticancer performance as verified by MTT assay test. It was concluded that developed NPs by us in this study may open the possibilities for targeted delivery of DOX to the cancerous tissues.

Compounded Apixaban Suspensions for Enteral Feeding Tubes.

PubMed

Caraballo, Maria L; Donmez, Seda; Nathan, Kobi; Zhao, Fang

2017-07-01

Objective: There is limited information on compounded apixaban formulations for administration via enteral feeding tubes. This study was designed to identify a suitable apixaban suspension formulation that is easy to prepare in a pharmacy setting, is compatible with commonly used feeding tubes, and has a beyond-use date of 7 days. Methods: Apixaban suspensions were prepared from commercially available 5-mg Eliquis tablets. Several vehicles and compounding methods were screened for ease of preparation, dosage accuracy, and tube compatibility. Two tubing types, polyurethane and polyvinyl chloride, with varying lengths and diameters, were included in the study. They were mounted on a peg board during evaluation to mimic the patient body position. A 7-day stability study of the selected formulation was also conducted. Results: Vehicles containing 40% to 60% Ora-Plus in water all exhibited satisfactory flowability through the tubes. The mortar/pestle compounding method was found to produce more accurate and consistent apixaban suspensions than the pill crusher or crushing syringe method. The selected formulation, 0.25 mg/mL apixaban in 50:50 Ora-Plus:water, was compatible with both tubing types, retaining >98% drug in posttube samples. The stability study also confirmed that this formulation was stable physically and chemically over 7 days of storage at room temperature. Conclusions: A suitable apixaban suspension formulation was identified for administration via enteral feeding tubes. The formulation consisted of 0.25 mg/mL apixaban in 50:50 Ora-Plus:water. The stability study results supported a beyond-use date of 7 days at room temperature.

Preparing a poster.

PubMed

White, Adrian; White, Leon

2003-06-01

Well prepared posters are an effective means to communicate a simple message and stimulate discussion. A good poster requires considerable effort in identifying the vital ingredients and rejecting any superfluous material. The conventional structure for papers and abstracts is a suitable basis for posters on many subjects, with modification if necessary. Suitable topics include clinical trials, surveys, qualitative studies and case reports. Suggestions are made for contents that should be considered for each section. Careful planning of size, shape, flow and content will save time in preparation, and several technical graphical points are made, which may improve the attractiveness and readability of the poster.

Effect of two-stage sintering on dielectric properties of BaTi0.9Zr0.1O3 ceramics

NASA Astrophysics Data System (ADS)

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

2011-09-01

The effect of two-stage sintering on the dielectric properties of BaTi0.9Zr0.1O3 ceramics prepared by solid state route was investigated and is presented here. It has been found that under suitable two-stage sintering conditions, dense BaTi0.9Zr0.1O3 ceramics with improved electrical properties can be synthesized. The density was found to have a value of 5.49 g cc-1 for normally sintered samples, whereas in the case of the two-stage sintered sample it was 5.85 g cc-1. Dielectric measurements were done as a function of frequency and temperature. A small decrease in the Curie temperature was observed with modification in dielectric loss for two-stage sintered ceramic samples.

RNA sample preparation applied to gene expression profiling for the horse biological passport.

PubMed

Bailly-Chouriberry, Ludovic; Baudoin, Florent; Cormant, Florence; Glavieux, Yohan; Loup, Benoit; Garcia, Patrice; Popot, Marie-Agnès; Bonnaire, Yves

2017-09-01

The improvement of doping control is an ongoing race. Techniques to fight doping are usually based on the direct detection of drugs or their metabolites by analytical methods such as chromatography hyphenated to mass spectrometry after ad hoc sample preparation. Nowadays, omic methods constitute an attractive development and advances have been achieved particularly by application of molecular biology tools for detection of anabolic androgenic steroids (AAS), erythropoiesis-stimulating agent (ESA), or to control human growth hormone misuses. These interesting results across different animal species have suggested that modification of gene expression offers promising new methods of improving the window of detection of banned substances by targeting their effects on blood cell gene expression. In this context, the present study describes the possibility of using a modified version of the dedicated Human IVD (in vitro Diagnostics) PAXgene® Blood RNA Kit for horse gene expression analysis in blood collected on PAXgene® tubes applied to the horse biological passport. The commercial kit was only approved for human blood samples and has required an optimization of specific technical requirements for equine blood samples. Improvements and recommendations were achieved for sample collection, storage and RNA extraction procedure. Following these developments, RNA yield and quality were demonstrated to be suitable for downstream gene expression analysis by qPCR techniques. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Preparation and Characterization of Microencapsulated Phase Change Materials for Use in Building Applications

PubMed Central

Giro-Paloma, Jessica; Al-Shannaq, Refat; Fernández, Ana Inés; Farid, Mohammed M.

2015-01-01

A method for preparing and characterizing microencapsulated phase change materials (MPCM) was developed. A comparison with a commercial MPCM is also presented. Both MPCM contained paraffin wax as PCM with acrylic shell. The melting temperature of the PCM was around 21 °C, suitable for building applications. The M-2 (our laboratory made sample) and Micronal® DS 5008 X (BASF) samples were characterized using SEM, DSC, nano-indentation technique, and Gas Chromatography/Mass spectrometry (GC-MS). Both samples presented a 6 μm average size and a spherical shape. Thermal energy storage (TES) capacities were 111.73 J·g−1 and 99.3 J·g−1 for M-2 and Micronal® DS 5008 X, respectively. Mechanical characterization of the samples was performed by nano-indentation technique in order to determine the elastic modulus (E), load at maximum displacement (Pm), and displacement at maximum load (hm), concluding that M-2 presented slightly better mechanical properties. Finally, an important parameter for considering use in buildings is the release of volatile organic compounds (VOC’s). This characteristic was studied at 65 °C by CG-MS. Both samples showed VOC’s emission after 10 min of heating, however peaks intensity of VOC’s generated from M-2 microcapsules showed a lower concentration than Micronal® DS 5008 X. PMID:28787812

Fast X-Ray Fluorescence Microtomography of Hydrated Biological Samples

PubMed Central

Lombi, Enzo; de Jonge, Martin D.; Donner, Erica; Kopittke, Peter M.; Howard, Daryl L.; Kirkham, Robin; Ryan, Chris G.; Paterson, David

2011-01-01

Metals and metalloids play a key role in plant and other biological systems as some of them are essential to living organisms and all can be toxic at high concentrations. It is therefore important to understand how they are accumulated, complexed and transported within plants. In situ imaging of metal distribution at physiological relevant concentrations in highly hydrated biological systems is technically challenging. In the case of roots, this is mainly due to the possibility of artifacts arising during sample preparation such as cross sectioning. Synchrotron x-ray fluorescence microtomography has been used to obtain virtual cross sections of elemental distributions. However, traditionally this technique requires long data acquisition times. This has prohibited its application to highly hydrated biological samples which suffer both radiation damage and dehydration during extended analysis. However, recent advances in fast detectors coupled with powerful data acquisition approaches and suitable sample preparation methods can circumvent this problem. We demonstrate the heightened potential of this technique by imaging the distribution of nickel and zinc in hydrated plant roots. Although 3D tomography was still impeded by radiation damage, we successfully collected 2D tomograms of hydrated plant roots exposed to environmentally relevant metal concentrations for short periods of time. To our knowledge, this is the first published example of the possibilities offered by a new generation of fast fluorescence detectors to investigate metal and metalloid distribution in radiation-sensitive, biological samples. PMID:21674049

A novel hybridization approach for detection of citrus viroids.

PubMed

Murcia, N; Serra, P; Olmos, A; Duran-Vila, N

2009-04-01

Citrus plants are natural hosts of several viroid species all belonging to the family Pospiviroidae. Previous attempts to detect viroids from field-grown species and cultivars yielded erratic results unless analyses were performed using Etrog citron a secondary bio-amplification host. To overcome the use of Etrog citron a number of RT-PCR approaches have been proposed with different degrees of success. Here we report the suitability of an easy to handle northern hybridization protocol for viroid detection of samples collected from field-grown citrus species and cultivars. The protocol involves: (i) Nucleic acid preparations from bark tissue samples collected from field-grown trees regardless of the growing season and storage conditions; (ii) Separation in 5% PAGE or 1% agarose, blotting to membrane and fixing; (iii) Hybridization with viroid-specific DIG-labelled probes and detection with anti-DIG-alkaline phosphatase conjugate and autoradiography with the CSPD substrate. The method has been tested with viroid-infected trees of sweet orange, lemon, mandarin, grapefruit, sour orange, Swingle citrumello, Tahiti lime and Mexican lime. This novel hybridization approach is extremely sensitive, easy to handle and shortens the time needed for reliable viroid indexing tests. The suitability of PCR generated DIG-labelled probes and the sensitivity achieved when the samples are separated and blotted from non-denaturing gels are discussed.

Preparation and characterization of Fe3O4-Pt nanoparticles

NASA Astrophysics Data System (ADS)

Andrade, Ângela Leão; Cavalcante, Luis Carlos Duarte; Fabris, José Domingos; Pereira, Márcio César; Ardisson, José Domingos; Domingues, Rosana Zacarias

2017-11-01

Pt and Pt-based nanomaterials are active anticancer drugs for their ability to inhibit the division of living cells. Nanoparticles of magnetite containing variable proportions of platinum were prepared in the laboratory. The magnetite nanoparticles with platinum (Pt-Fe3O4) were obtained by reducing the Fe3+ of the maghemite ( γ Fe2O3) mixed with platinum (II) acetylacetonate and sucrose in two inversely coupled ceramic crucibles and heated in a furnace at 400 °C for 20 min. The formed carbon during this preparation acts to chemically reduce the ferric iron in maghemite. Moreover, its residual layer on the particle surface prevents the forming magnetite from oxidizing in air and helps retain the platinum in the solid mixture. The produced Pt-magnetite samples were characterized by 57Fe-Mössbauer spectroscopy, powder X-ray diffraction, scanning electron microscopy, and magnetization measurements. Measurements of AC magnetic-field-induced heating properties of the obtained nanocomposites, in aqueous solution, showed that they are suitable as a hyperthermia agent for biological applications.

Fusion Bead Procedure for Nuclear Forensics Employing Synthetic Enstatite to Dissolve Uraniferous and Other Challenging Materials Prior to Laser Ablation Inductively Coupled Plasma Mass Spectrometry.

PubMed

Reading, David G; Croudace, Ian W; Warwick, Phillip E

2017-06-06

There is an increasing demand for rapid and effective analytical tools to support nuclear forensic investigations of seized or suspect materials. Some methods are simply adapted from other scientific disciplines and can effectively be used to rapidly prepare complex materials for subsequent analysis. A novel sample fusion method is developed, tested, and validated to produce homogeneous, flux-free glass beads of geochemical reference materials (GRMs), uranium ores, and uranium ore concentrates (UOC) prior to the analysis of 14 rare earth elements (REE) via laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The novelty of the procedure is the production of glass beads using 9 parts high purity synthetic enstatite (MgSiO 3 ) as the glass former with 1 part of sample (sample mass ∼1.5 mg). The beads are rapidly prepared (∼10 min overall time) by fusing the blended mixture on an iridium strip resistance heater in an argon-purged chamber. Many elements can be measured in the glass bead, but the rare earth group in particular is a valuable series in nuclear forensic studies and is well-determined using LA-ICP-MS. The REE data obtained from the GRMs, presented as chondrite normalized patterns, are in very good agreement with consensus patterns. The UOCs have comparable patterns to solution ICP-MS methods and published data. The attractions of the current development are its conservation of sample, speed of preparation, and suitability for microbeam analysis, all of which are favorable for nuclear forensics practitioners and geochemists requiring REE patterns from scarce or valuable samples.

An etched stainless steel wire/ionic liquid-solid phase microextraction technique for the determination of alkylphenols in river water.

PubMed

Cui, Meiyu; Qiu, Jinxue; Li, Zhenghua; He, Miao; Jin, Mingshi; Kim, Jiman; Quinto, Maurizio; Li, Donghao

2015-01-01

In this study, a stainless steel wire/ionic liquid-solid phase microextraction technique was developed for the direct extraction of APs from water samples. Some parameters were optimised, such as selection of the substrate and ILs, extraction time, extraction temperature, stirring rate and sample pH, etc. The experimental data demonstrated that the etched stainless steel wire was a suitable substrate for IL-coated SPME. The coating was prepared by directly depositing the ILs onto the surface of the etched stainless steel wire, which exhibited a porous structure and a high surface area. The [C8MIM][PF6] IL exhibited maximum efficiency with an extraction time of 30 min, and the aqueous sample was maintained at 40 °C and adjusted to pH 2 under stirring conditions. The enrichment factor of the IL coating for the four APs ranged from 1382 to 4779, the detection limits (LOD, S/N=3) of the four APs ranged from 0.01 to 0.04 ng mL(-1) and the RSD values for purified water spiked with APs ranged from 4.0 to 11.8% (n=3). The calibration graphs were linear in the concentration range from 0.5 to 200 ng mL(-1) (R(2)>0.9569). The optimised method was successfully applied for the analysis of real water samples, and the method was suitable for the extraction of APs from water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Voltammetric determination of copper in selected pharmaceutical preparations--validation of the method.

PubMed

Lutka, Anna; Maruszewska, Małgorzata

2011-01-01

It were established and validated the conditions of voltammetric determination of copper in pharmaceutical preparations. The three selected preparations: Zincuprim (A), Wapń, cynk, miedź z wit. C (B), Vigor complete (V) contained different salts and different quantity of copper (II) and increasing number of accompanied ingredients. For the purpose to transfer copper into solution, the samples of powdered tablets of the first and second preparation were undergone extraction and of the third the mineralization procedures. The concentration of copper in solution was determined by differential pulse voltammetry (DP) using comparison with standard technique. In the validation process, the selectivity, accuracy, precision and linearity of DP determination of copper in three preparations were estimated. Copper was determined within the concentration range of 1-9 ppm (1-9 microg/mL): the mean recoveries approached 102% (A), 100% (B), 102% (V); the relative standard deviations of determinations (RSD) were 0.79-1.59% (A), 0.62-0.85% (B) and 1.68-2.28% (V), respectively. The mean recoveries and the RSDs of determination satisfied the requirements for the analyte concentration at the level 1-10 ppm. The statistical verification confirmed that the tested voltammetric method is suitable for determination of copper in pharmaceutical preparation.

A modified technique for the preparation of SO2 from sulphates and sulphides for sulphur isotope analyses.

PubMed

Han, L; Tanweer, A; Szaran, J; Halas, S

2002-09-01

A modified technique for the conversion of sulphates and sulphides to SO2 with the mixture of V2O5-SiO2 for sulphur isotopic analyses is described. This technique is more suitable for routine analysis of large number of samples. Modification of the reaction vessel and using manifold inlet system allows to analyse up to 24 samples every day. The modified technique assures the complete yield of SO2, consistent oxygen isotope composition of the SO2 gas and reproducibility of delta34S measurements being within 0.10 per thousand. It is observed, however, oxygen in SO2 produced from sulphides differs in delta18O with respect to that produced from sulphates.

Chemical vapor deposition growth

NASA Technical Reports Server (NTRS)

Ruth, R. P.; Manasevit, H. M.; Campbell, A. G.; Johnson, R. E.; Kenty, J. L.; Moudy, L. A.; Shaw, G. L.; Simpson, W. I.; Yang, J. J.

1978-01-01

The objective was to investigate and develop chemical vapor deposition (CVD) techniques for the growth of large areas of Si sheet on inexpensive substrate materials, with resulting sheet properties suitable for fabricating solar cells that would meet the technical goals of the Low Cost Silicon Solar Array Project. The program involved six main technical tasks: (1) modification and test of an existing vertical-chamber CVD reactor system; (2) identification and/or development of suitable inexpensive substrate materials; (3) experimental investigation of CVD process parameters using various candidate substrate materials; (4) preparation of Si sheet samples for various special studies, including solar cell fabrication; (5) evaluation of the properties of the Si sheet material produced by the CVD process; and (6) fabrication and evaluation of experimental solar cell structures, using impurity diffusion and other standard and near-standard processing techniques supplemented late in the program by the in situ CVD growth of n(+)/p/p(+) sheet structures subsequently processed into experimental cells.

Use of ERTS imagery in air pollution and marine biology studies, tasks 1 through 3

NASA Technical Reports Server (NTRS)

Copeland, G. E.; Ludwick, J. C.; Marshall, H. G. (Principal Investigator); Bandy, A. R.; Fleischer, P.; Hanna, W. J.; Gosink, T. A.; Bowker, D. W.

1972-01-01

There are no author-identified significant results in this report. The general suitability of ERTS imagery in detecting ground originated air pollution has proved to be excellent. The quality and resolution exceeded expectations and has permitted in some instances location of point sources to within a thousand feet. Suitable techniques have not yet been developed for determining or measuring area and line sources of air pollution. A major problem has been cloud cover that has persisted over the area of primary interest, the Chesapeake Bay. Work has been completed on mounting the shipboard transmissometer which will be used for investigations to relate the chlorophyll and suspended sediment content in the waters of the Lower Chesapeake Bay to ERTS-1 imagery. Water sampling, plankton analysis, and preparations for sea collection of water truth along the eastern continental shelf of the U.S. have been completed for use in comparisons with ERTS-1 data.

Comparing different preparation methods to study human fibrin fibers and platelets using TEM.

PubMed

Buys, Antoinette V; Pretorius, Etheresia

2012-06-01

For the study of cellular ultrastructure, the sample needs to be stabilized by fixation, with the ultimate aim to preserve the native tissue organization and to protect the tissue against later stages of preparation. Chemical and freezing fixation are most used, and chemical fixation employs agents that permeate tissues and cells by diffusion and covalently bind with their major biochemical constituents to fix them. Most widely used chemical fixatives are aldehydes, e.g., formaldehyde and glutaraldehyde, which are noncoagulating, crosslinking agents. Cryofixation methods for ultrastructural studies are also popular, and high-pressure freezing immobilizes all cell constituents and arrests biological activity by removing the thermal energy from the system. In the current research, we used platelet-rich plasma (PRP) to study expansive fibrin fibers and platelet ultrastructure to compare the two fixation techniques. We also used thrombin and calcium chloride as a clotting agent to determine the technique most suitable for the formation of extensive fibrin networks. Chemically fixated fibrin fibers were more compact and condensed and also showed a banding pattern on longitudinal sections. High-pressure frozen samples were more dispersed while platelets fixated showed better preserved cellular membranes and organelle structure. PRP coagulated by addition of CaCl(2) showed blood platelets that are noticeably more activated compared with PRP; however, with thrombin, a sharp ultrastructure was seen. We conclude that PRP mixed with thrombin, and freeze substituted, is the most suitable method for the study of extensive fibrin fibers as well as platelets. Copyright © 2011 Wiley Periodicals, Inc.

Potential and limitations of X-Ray micro-computed tomography in arthropod neuroanatomy: A methodological and comparative survey

PubMed Central

Sombke, Andy; Lipke, Elisabeth; Michalik, Peter; Uhl, Gabriele; Harzsch, Steffen

2015-01-01

Classical histology or immunohistochemistry combined with fluorescence or confocal laser scanning microscopy are common techniques in arthropod neuroanatomy, and these methods often require time-consuming and difficult dissections and sample preparations. Moreover, these methods are prone to artifacts due to compression and distortion of tissues, which often result in information loss and especially affect the spatial relationships of the examined parts of the nervous system in their natural anatomical context. Noninvasive approaches such as X-ray micro-computed tomography (micro-CT) can overcome such limitations and have been shown to be a valuable tool for understanding and visualizing internal anatomy and structural complexity. Nevertheless, knowledge about the potential of this method for analyzing the anatomy and organization of nervous systems, especially of taxa with smaller body size (e.g., many arthropods), is limited. This study set out to analyze the brains of selected arthropods with micro-CT, and to compare these results with available histological and immunohistochemical data. Specifically, we explored the influence of different sample preparation procedures. Our study shows that micro-CT is highly suitable for analyzing arthropod neuroarchitecture in situ and allows specific neuropils to be distinguished within the brain to extract quantitative data such as neuropil volumes. Moreover, data acquisition is considerably faster compared with many classical histological techniques. Thus, we conclude that micro-CT is highly suitable for targeting neuroanatomy, as it reduces the risk of artifacts and is faster than classical techniques. J. Comp. Neurol. 523:1281–1295, 2015. © 2015 Wiley Periodicals, Inc. PMID:25728683

Luminescence studies and infrared emission of erbium-doped calcium zirconate phosphor.

PubMed

Tiwari, Neha; Dubey, Vikas

2016-05-01

The near-infrared-to-visible upconversion luminescence behaviour of Er(3+)-doped CaZrO3 phosphor is discussed in this manuscript. The phosphor was prepared by a combustion synthesis technique that is suitable for less-time-taking techniques for nanophosphors. The starting materials used for sample preparation were Ca(NO3)2.4H2O, Zr(NO3)4 and Er(NO3)2, and urea was used as a fuel. The prepared sample was characterized by X-ray diffraction (XRD). The surface morphology of prepared phosphor was determined by field emission gun scanning electron microscopy (FEGSEM). The functional group analysis was determined by Fourier transform infrared (FTIR) spectroscopy. All prepared phosphors with variable Er(3+) concentrations (0.5-2.5 mol%) were studied by photoluminescence analysis. It was found that the excitation spectra of the prepared phosphor showed a sharp excitation peak centred at 980 nm. The emission spectra with variable Er(3+) concentrations showed strong peaks in the 555 nm and 567 nm range, with a dominant peak at 555 nm due to the ((2)H(11/2),(4)S(3/2)) transition and a weaker transition at 567 nm associated with 527 nm. Spectrophotometric determination of the peak was evaluated by the Commission Internationale de I'Eclairage (CIE) method These upconverted emissions were attributed to a two-photon process. The excitation wavelength dependence of the upconverted luminescence, together with its time evolution after infrared pulsed excitation, suggested that energy transfer upconversion processes were responsible for the upconversion luminescence. The upconversion mechanisms were studied in detail through laser power dependence. Excited state absorption and energy transfer processes were discussed as possible upconversion mechanisms. The cross-relaxation process in Er(3+) was also investigated. Copyright © 2015 John Wiley & Sons, Ltd.

GMO detection using a bioluminescent real time reporter (BART) of loop mediated isothermal amplification (LAMP) suitable for field use.

PubMed

Kiddle, Guy; Hardinge, Patrick; Buttigieg, Neil; Gandelman, Olga; Pereira, Clint; McElgunn, Cathal J; Rizzoli, Manuela; Jackson, Rebecca; Appleton, Nigel; Moore, Cathy; Tisi, Laurence C; Murray, James A H

2012-04-30

There is an increasing need for quantitative technologies suitable for molecular detection in a variety of settings for applications including food traceability and monitoring of genetically modified (GM) crops and their products through the food processing chain. Conventional molecular diagnostics utilising real-time polymerase chain reaction (RT-PCR) and fluorescence-based determination of amplification require temperature cycling and relatively complex optics. In contrast, isothermal amplification coupled to a bioluminescent output produced in real-time (BART) occurs at a constant temperature and only requires a simple light detection and integration device. Loop mediated isothermal amplification (LAMP) shows robustness to sample-derived inhibitors. Here we show the applicability of coupled LAMP and BART reactions (LAMP-BART) for determination of genetically modified (GM) maize target DNA at low levels of contamination (0.1-5.0% GM) using certified reference material, and compare this to RT-PCR. Results show that conventional DNA extraction methods developed for PCR may not be optimal for LAMP-BART quantification. Additionally, we demonstrate that LAMP is more tolerant to plant sample-derived inhibitors, and show this can be exploited to develop rapid extraction techniques suitable for simple field-based qualitative tests for GM status determination. We also assess the effect of total DNA assay load on LAMP-BART quantitation. LAMP-BART is an effective and sensitive technique for GM detection with significant potential for quantification even at low levels of contamination and in samples derived from crops such as maize with a large genome size. The resilience of LAMP-BART to acidic polysaccharides makes it well suited to rapid sample preparation techniques and hence to both high throughput laboratory settings and to portable GM detection applications. The impact of the plant sample matrix and genome loading within a reaction must be controlled to ensure quantification at low target concentrations.

Effect of annealing and In content on the properties of electron beam evaporated ZnO films

NASA Astrophysics Data System (ADS)

Mohamed, S. H.; Ali, H. M.; Mohamed, H. A.; Salem, A. M.

2005-08-01

The effect of both annealing and In content on the properties of ZnO films prepared by electron beam evaporation were investigated. The evaporation was carried out at room temperature from bulk samples prepared by sintering technique. X-ray diffraction showed that the structure of ZnO-In{2}O{3} films depends on both the In content and annealing temperature. Amorphous, highly transparent and relatively low resistive films which can be suitable for the usage as transparent electrode of organic light-emitting diode were obtained upon annealing at 300 circC. Partially crystalline, highly transparent and highly resistive films which can be used in piezoelectric applications were obtained upon annealing at 500 circC. For each composition the refractive index has no monotonic variation upon increasing annealing temperature.

Polyvinyl alcohol: an efficient fuel for synthesis of superparamagnetic LSMO nanoparticles for biomedical application.

PubMed

Thorat, N D; Shinde, K P; Pawar, S H; Barick, K C; Betty, C A; Ningthoujam, R S

2012-03-14

La(0.7)Sr(0.3)MnO(3) (LSMO) nanoparticles have been prepared using glycine and polyvinyl alcohol (PVA) as fuels. Their crystal structure, particle morphology and compositions are characterized using X-ray diffraction, transmission electron microscopy, field-emission electron microscopy and energy dispersive analysis of X-ray. They show a pseudo-cubic perovskite structure. The spherical particle sizes of 30 and 20 nm have been obtained from samples prepared by glycine and PVA respectively. The field cooled (FC) and zero field cooled (ZFC) magnetizations have been recorded from 5 to 375 K at 500 Oe and superparamagnetic blocking temperatures (T(B)) of 75 and 30 K are obtained from samples prepared by glycine and PVA respectively. Particle size distribution is observed from dynamic light scattering measurements. Dispersion stability of the particles in water is studied by measuring the Zeta potential with varying the pH of the medium from 1 to 12. Under induction heating experiments, a hyperthermia temperature (42-43 °C) is achieved by both the samples (3-6 mg mL(-1)) at magnetic fields of 167-335 Oe and at a frequency of 267 kHz. The bio-compatibility of the LSMO nanoparticles is studied on the L929 and HeLa cell lines by MTT assay for up to 48 h. The present work reveals the importance of synthesis technique and fuel choice on structural, morphological, magnetic, hyperthermia and biocompatible properties of LSMO and predicts the suitability for biomedical applications.

Extraction tools for identification of chemical contaminants in estuarine and coastal waters to determine toxic pressure on primary producers.

PubMed

Booij, Petra; Sjollema, Sascha B; Leonards, Pim E G; de Voogt, Pim; Stroomberg, Gerard J; Vethaak, A Dick; Lamoree, Marja H

2013-09-01

The extent to which chemical stressors affect primary producers in estuarine and coastal waters is largely unknown. However, given the large number of legacy pollutants and chemicals of emerging concern present in the environment, this is an important and relevant issue that requires further study. The purpose of our study was to extract and identify compounds which are inhibitors of photosystem II activity in microalgae from estuarine and coastal waters. Field sampling was conducted in the Western Scheldt estuary (Hansweert, The Netherlands). We compared four different commonly used extraction methods: passive sampling with silicone rubber sheets, polar organic integrative samplers (POCIS) and spot water sampling using two different solid phase extraction (SPE) cartridges. Toxic effects of extracts prepared from spot water samples and passive samplers were determined in the Pulse Amplitude Modulation (PAM) fluorometry bioassay. With target chemical analysis using LC-MS and GC-MS, a set of PAHs, PCBs and pesticides was determined in field samples. These compound classes are listed as priority substances for the marine environment by the OSPAR convention. In addition, recovery experiments with both SPE cartridges were performed to evaluate the extraction suitability of these methods. Passive sampling using silicone rubber sheets and POCIS can be applied to determine compounds with different structures and polarities for further identification and determination of toxic pressure on primary producers. The added value of SPE lies in its suitability for quantitative analysis; calibration of passive samplers still needs further investigation for quantification of field concentrations of contaminants. Copyright © 2013 Elsevier Ltd. All rights reserved.

AC impedance spectroscopy of NASICON type Na3Fe2(PO4)3 ceramic

NASA Astrophysics Data System (ADS)

Mandal, Biswajit; Thakur, A. K.

2018-05-01

Super ionic conductors (e.g.; A3M2(XO4)3, A=Li, Na) have received attention in applied research due to their interesting electrochemical property and inherently high ionic conductivity [1]. However, structural and compatibility requirements for fast ion transport is stringent and it plays a crucial role. In A3M2(XO4)3, a suitable cage formation in the crystal framework due to corner sharing arrangement of XO4 tetrahedra and MO6 octahedra creates voids that acts as host/guest site for cation transport. In this work, we report Nasicon structure Na3Fe2(PO4)3 (NFP) prepared via sol-gel route mediated by citric acid. Structural analysis confirmed that NFP sample belongs to monoclinic crystal structure having Cc space group (S. G. No 9) with lattice parameters, a=15.106 Å, b=8.722 Å, c=8.775 Å and β=124.96°. Electrical properties of the prepared sample have been studied by AC impedance spectroscopy technique. The AC conductivity results indicated typical signature of ionically conducting system.

Photo-electrochemically synthesized light emtting nanoporous silicon based UV photodetector: influence of current density

NASA Astrophysics Data System (ADS)

Thahe, Asad A.; Bidin, Noriah; Hassan, Z.; Bakhtiar, Hazri; Qaeed, M. A.; Bououdina, Mohamed; Ahmed, Naser M.; Talib, Zainal A.; Al-Azawi, Mohammed A.; Alqaraghuli, Hasan; Uday, M. B.; Hamad Ahmed, Omar

2017-11-01

Nanoporous silicon (n-PSi) with diverse morphologies was prepared on silicon (Si) substrate via photo-electrochemical etching technique. The role of changing current density (15, 30 and 45 mA cm-2) on the structure, morphology and optical properties was determined. As-prepared samples were systematically characterized using XRD, FESEM, AFM and photoluminescence measurements. Furthermore, the achieved n-PSi sample was used to make metal-semiconductor-metal (MSM) UV photodetector. The performance of these photodetectors was evaluated upon exposing to visible light of wavelength 530 nm (power density 1.55 mW cm-2), which exhibited very high sensitivity of 150.26 with a low dark current. The achieved internal photoconductive gain was 2.50, the photoresponse peak was 1.23 A W-1 and the response time was 0.49 s and the recovery time was 0.47 s. Excellent attributes of the fabricated photodetectors suggest that the present approach may provide a cost effective and simple way to obtain n-PSi suitable for sundry applications.

Synthesis of surface molecular imprinted polymers based on carboxyl-modified silica nanoparticles with the selective detection of dibutyl phthalate from tap water samples

NASA Astrophysics Data System (ADS)

Xu, Wanzhen; Zhang, Xiaoming; Huang, Weihong; Luan, Yu; Yang, Yanfei; Zhu, Maiyong; Yang, Wenming

2017-12-01

In this work, the molecular imprinted polymers were synthesized with the low monomer concentrations for dibutyl phthalate (DBP). The polymers were prepared over carboxyl-modified silica nanoparticle, which used methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the cross-linker agent and azoisobutyronitrile as the initiator in the process of preparation. Various measures were used to characterize the structure and morphology in order to get the optimal polymer. The characterization results show that the optimal polymer has suitable features for further adsorption process. And adsorption capacity experiments were evaluated to analyze its adsorption performance, through adsorption isotherms/kinetics, selectivity adsorption and desorption and regeneration experiments. These results showed that the molecular imprinted polymers had a short equilibrium time about 60 min and high stability with 88% after six cycles. Furthermore, the molecular imprinted polymers were successfully applied to remove dibutyl phthalate. The concentration range was 5.0-30.0 μmol L-1, and the limit of detection was 0.06 μmol L-1 in tap water samples.

Metallic contamination of food during preparation and storage: development of methods and some preliminary results.

PubMed

Samsahl, K; Wester, P O

1977-09-01

A chemical procedure for studying trace metals leached from metallic cooking utensils and preserving cans used in the preparation and storage of food has been developed. The method consists in the destruction of the major part of organic matter with HNO3-vapour followed by a complete mineralization of residues with small amounts of HNO3 in Teflon bombs at 150-160 degrees C under a pressure of 3-12 kg/cm2, depending on the amount and composition of the samples. Subsequently, an ion-exchange step removes major components and concentrates the trace elements in a dilute HNO3-solution, suitable for analysis. The ion-exchange separation, which is performed with an automatic ion-exchange separator, is practically free from blank level problems, e.g., typically a mean of less than 2 per cent of the sample levels of the elements being determined. Preliminary results show that large amounts of aluminium are released from vessels to the water during boiling at the same pH-range which exist for most drinking water in Sweden.

Synthesis of N-doped potassium tantalate perovskite material for environmental applications

NASA Astrophysics Data System (ADS)

Rao, Martha Purnachander; Nandhini, Vellangattupalayam Ponnusamy; Wu, Jerry J.; Syed, Asad; Ameen, Fuad; Anandan, Sambandam

2018-02-01

Nitrogen containing potassium tantalate perovskite material has been synthesized by the solvothermal method using urea (CH4N2O) as a nitrogen source. The as-prepared sample was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), diffuse reflectance spectroscopy (DRS), scanning electron microscope (SEM), and energy-dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS). The particle size of nitrogen containing KTaO3 observed from SEM images was found to be 100-150 nm. Doping KTaO3 with nitrogen causes reduction of band gap from 3.5 to 2.54 eV. The incorporation of Nitrogen into the crystal lattice of KTaO3 not only extended the absorption of light from UV (ultraviolet) region to visible region and also enhanced the photocatalytic activity. As prepared nitrogen containing KTaO3 samples exhibit cubic-like morphology and noticed efficient photocatalytic activity towards methylene blue dye degradation under visible light illumination. The intermediates formed during photodegradation were identified by mass spectrometry (GC-MS) and proposed suitable degradation pathway.

Thermal processing of a poorly water-soluble drug substance exhibiting a high melting point: the utility of KinetiSol® Dispersing.

PubMed

Hughey, Justin R; Keen, Justin M; Brough, Chris; Saeger, Sophie; McGinity, James W

2011-10-31

Poorly water-soluble drug substances that exhibit high melting points are often difficult to successfully process by fusion-based techniques. The purpose of this study was to identify a suitable polymer system for meloxicam (MLX), a high melting point class II BCS compound, and investigate thermal processing techniques for the preparation of chemically stable single phase solid dispersions. Thermal and solution based screening techniques were utilized to screen hydrophilic polymers suitable for immediate release formulations. Results of the screening studies demonstrated that Soluplus(®)(SOL) provided the highest degree of miscibility and solubility enhancement. A hot-melt extrusion feasibility study demonstrated that high temperatures and extended residence times were required in order to render compositions amorphous, causing significant degradation of MLX. A design of experiments (DOE) was conducted on the KinetiSol(®) Dispersing (KSD) process to evaluate the effect of processing conditions on the chemical stability and amorphous character of MLX. The study demonstrated that ejection temperature significantly impacted MLX stability. All samples prepared by KSD were substantially amorphous. Dissolution analysis of the KSD processed solid dispersions showed increased dissolution rates and extent of supersaturation over the marketed generic MLX tablets. Copyright © 2011 Elsevier B.V. All rights reserved.

Controlled preparation of Ag–Cu{sub 2}O nanocorncobs and their enhanced photocatalytic activity under visible light

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

Yang, Siyuan; Zhang, Shengsen; College of Science, South China Agricultural University, Guangzhou 510642

Graphical abstract: The corncob-like Ag–Cu{sub 2}O nanostructure with suitably exposed Ag surface exhibited much higher photocatalytic activity than Ag@Cu{sub 2}O nanocables and Cu{sub 2}O nanowires. - Highlights: • Ag–Cu{sub 2}O nanocorncobs have been controllably prepared by a simple synthesis. • The possible formation mechanism of Ag–Cu{sub 2}O has been studied. • Ag–Cu{sub 2}O exhibits noticeable improved photocurrent compared with the pure Cu{sub 2}O NWs. • Ag–Cu{sub 2}O with suitably exposed Ag surface shows much higher photocatalytic activity. - Abstract: Novel corncob-like nano-heterostructured Ag–Cu{sub 2}O photocatalyst has been controllably prepared by adjusting the synthetic parameters, and the possible formation mechanism hasmore » been also studied. The photoelectrochemical and photocatalytic performances demonstrated that the as-prepared Ag–Cu{sub 2}O nanocorncobs exhibited higher photocatalytic activity than both pure Cu{sub 2}O nanowires and cable-like Ag@Cu{sub 2}O nano-composites. It was concluded that Ag–Cu{sub 2}O nanocorncobs with suitably exposed Ag surface not only effectively inhibit the recombination of electron–hole pairs but also suitably increase the active sites of electronic conduction, and thus increasing the photocatalytic activity under visible light irradiation.« less

Structural characterization of Er(3+),Yb(3+)-doped Gd2O3 phosphor, synthesized using the solid-state reaction method, and its luminescence behavior.

PubMed

Tamrakar, Raunak Kumar; Bisen, D P; Brahme, Nameeta

2016-02-01

We report the synthesis and structural characterization of Er(3+),Yb(3+)-doped Gd2O3 phosphor. The sample was prepared using the conventional solid-state reaction method, which is the most suitable method for large-scale production. The prepared phosphor sample was characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), thermoluminescence (TL), photoluminescence (PL) and CIE techniques. For PL studies, the excitation and emission spectra of Gd2O3 phosphor doped with Er(3+) and Yb(3+) were recorded. The excitation spectrum was recorded at a wavelength of 551 nm and showed an intense peak at 276 nm. The emission spectrum was recorded at 276 nm excitation and showed peaks in all blue, green and red regions, which indicate that the prepared phosphor may act as a single host for white light-emitting diode (WLED) applications, as verified by International de I'Eclairage (CIE) techniques. From the XRD data, the calculated average crystallite size of Er(3+) and Yb(3+) -doped Gd2O3 phosphor is ~ 38 nm. A TL study was carried out for the phosphor using UV irradiation. The TL glow curve was recorded for UV, beta and gamma irradiations, and the kinetic parameters were also calculated. In addition, the trap parameters of the prepared phosphor were also studied using computerized glow curve deconvolution (CGCD). Copyright © 2015 John Wiley & Sons, Ltd.

Optimization of the β-Elimination/Michael Addition Chemistry on Reversed-Phase Supports for Mass Spectrometry Analysis of O-Linked Protein Modifications

PubMed Central

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

2013-01-01

We previously adapted the β-elimination/Michael addition chemistry to solid-phase derivatization on reversed-phase supports, and demonstrated the utility of this reaction format to prepare phosphoseryl peptides in unfractionated protein digests for mass spectrometric identification and facile phosphorylation-site determination. Here, we have expanded the use of this technique to β-N-acetylglucosamine peptides, modified at serine/threonine, phosphothreonyl peptides, and phosphoseryl/phosphothreonyl peptides, followed in sequence by proline. The consecutive β-elimination with Michael addition was adapted to optimize the solid-phase reaction conditions for throughput and completeness of derivatization. The analyte remained intact during derivatization and was recovered efficiently from the silica-based, reversed-phase support with minimal sample loss. The general use of the solid-phase approach for enzymatic dephosphorylation was demonstrated with phosphoseryl and phosphothreonyl peptides and was used as an orthogonal method to confirm the identity of phosphopeptides in proteolytic mixtures. The solid-phase approach proved highly suitable to prepare substrates from low-level amounts of protein digests for phosphorylation-site determination by chemical-targeted proteolysis. The solid-phase protocol provides for a simple, robust, and efficient tool to prepare samples for phosphopeptide identification in MALDI mass maps of unfractionated protein digests, using standard equipment available in most biological laboratories. The use of a solid-phase analytical platform is expected to be readily expanded to prepare digest from O-glycosylated- and O-sulfonated proteins for mass spectrometry-based structural characterization. PMID:23997661

Algal autolysate medium to label proteins for NMR in mammalian cells.

PubMed

Fuccio, Carmelo; Luchinat, Enrico; Barbieri, Letizia; Neri, Sara; Fragai, Marco

2016-04-01

In-cell NMR provides structural and functional information on proteins directly inside living cells. At present, the high costs of the labeled media for mammalian cells represent a limiting factor for the development of this methodology. Here we report a protocol to prepare a homemade growth medium from Spirulina platensis autolysate, suitable to express uniformly labeled proteins inside mammalian cells at a reduced cost-per-sample. The human proteins SOD1 and Mia40 were overexpressed in human cells grown in (15)N-enriched S. platensis algal-derived medium, and high quality in-cell NMR spectra were obtained.

Active pharmaceutical ingredients available as substances for extemporaneous preparation in veterinary medicine in the Czech Republic.

PubMed

Sklenář, Zbyněk; Horáčková, Kateřina; Bakhouche, Hana

2014-04-01

In veterinary medicine, extemporaneously prepared drugs can be also used in therapy. In the recent four years the selection of suitable compounds for extemporaneous (magistral) preparation has been expanded and new possibilities for the creation of formulas have appeared. The paper reports on the substances available for compounding that can be used in veterinary medicine, in the pharmacotherapeutic classes antibiotics, antimycotics, antiseptics, corticosteroids, emollients and epithelizing agents, anti-inflammatory drugs, local anesthetics, decongestives, beta-blockers and calcium channel blockers, antiemetics and prokinetics, sedatives and hypnotics. The emphasis has been placed on newly available substances. Examples of suitable magistral formulas are presented that can replace mass-produced drug products which are not readily obtainable. The aim of the paper is to inform pharmacists and veterinarians about new possibilities of drug compounding. compounded preparations extemporaneous preparation compounding of drugs possibilities magistral formulas in veterinary medicine.

Application of Lemongrass Oil-Containing Polylactic Acid Films to the Packaging of Pork Sausages.

PubMed

Yang, Hyun-Ju; Song, Kyung Bin

2016-01-01

Polylactic acid (PLA) is a biodegradable and renewable polymer, which represents a valuable alternative to plastic packaging films, often associated with environmental problems. In this study, we tested the suitability of PLA as a biodegradable packaging film and assessed the antimicrobial activity of lemongrass oil (LO), incorporated into the PLA film in different concentrations. To obtain the optimal physical properties for PLA films, tensile strength, elongation at break, and water vapor permeability were measured under different preparation conditions. In addition, the antimicrobial activity of the LO contained in the PLA film against Listeria monocytogenes was investigated by disc diffusion and viable cell count. Among all concentrations tested, 2% LO was the most suitable in terms of antimicrobial activity and physical properties of the PLA film. Based on these results, we used the PLA film containing 2% LO to pack pork sausages; after 12 d of storage at 4℃, the population of inoculated L. monocytogenes in the sausage samples wrapped with the PLA film containing 2% LO was reduced by 1.47 Log CFU/g compared with the control samples. Our data indicate that PLA films containing 2% LO represent a valuable means for antimicrobial sausage packaging.

Application of Lemongrass Oil-Containing Polylactic Acid Films to the Packaging of Pork Sausages

PubMed Central

2016-01-01

Polylactic acid (PLA) is a biodegradable and renewable polymer, which represents a valuable alternative to plastic packaging films, often associated with environmental problems. In this study, we tested the suitability of PLA as a biodegradable packaging film and assessed the antimicrobial activity of lemongrass oil (LO), incorporated into the PLA film in different concentrations. To obtain the optimal physical properties for PLA films, tensile strength, elongation at break, and water vapor permeability were measured under different preparation conditions. In addition, the antimicrobial activity of the LO contained in the PLA film against Listeria monocytogenes was investigated by disc diffusion and viable cell count. Among all concentrations tested, 2% LO was the most suitable in terms of antimicrobial activity and physical properties of the PLA film. Based on these results, we used the PLA film containing 2% LO to pack pork sausages; after 12 d of storage at 4℃, the population of inoculated L. monocytogenes in the sausage samples wrapped with the PLA film containing 2% LO was reduced by 1.47 Log CFU/g compared with the control samples. Our data indicate that PLA films containing 2% LO represent a valuable means for antimicrobial sausage packaging. PMID:27433114

Flow-injection assay of catalase activity.

PubMed

Ukeda, Hiroyuki; Adachi, Yukiko; Sawamura, Masayoshi

2004-03-01

A novel flow-injection assay (FIA) system with a double line for catalase activity was constructed in which an oxidase is immobilized and the substrate is continuously pumped to reduce the dissolved oxygen and to generate a given level of hydrogen peroxide. The catalase in a sample decomposed the hydrogen peroxide, and thus the increase in dissolved oxygen dependent on the activity was amperometrically monitored using a Clark-type oxygen electrode. Among the examined several oxidases, uricase was most suitable for the continuous formation of hydrogen peroxide from a consideration of the stability and the conversion efficiency. Under the optimum conditions, a linear calibration curve was obtained in the range from 21 to 210 units/mg and the reproducibility (CV) was better than 2% by 35 successive determinations of 210 units/ml catalase preparation. The sampling frequency was about 15 samples/h. The present FIA system was applicable to monitor the inactivation of catalase by glycation.

Image processing for identification and quantification of filamentous bacteria in in situ acquired images.

PubMed

Dias, Philipe A; Dunkel, Thiemo; Fajado, Diego A S; Gallegos, Erika de León; Denecke, Martin; Wiedemann, Philipp; Schneider, Fabio K; Suhr, Hajo

2016-06-11

In the activated sludge process, problems of filamentous bulking and foaming can occur due to overgrowth of certain filamentous bacteria. Nowadays, these microorganisms are typically monitored by means of light microscopy, commonly combined with staining techniques. As drawbacks, these methods are susceptible to human errors, subjectivity and limited by the use of discontinuous microscopy. The in situ microscope appears as a suitable tool for continuous monitoring of filamentous bacteria, providing real-time examination, automated analysis and eliminating sampling, preparation and transport of samples. In this context, a proper image processing algorithm is proposed for automated recognition and measurement of filamentous objects. This work introduces a method for real-time evaluation of images without any staining, phase-contrast or dilution techniques, differently from studies present in the literature. Moreover, we introduce an algorithm which estimates the total extended filament length based on geodesic distance calculation. For a period of twelve months, samples from an industrial activated sludge plant were weekly collected and imaged without any prior conditioning, replicating real environment conditions. Trends of filament growth rate-the most important parameter for decision making-are correctly identified. For reference images whose filaments were marked by specialists, the algorithm correctly recognized 72 % of the filaments pixels, with a false positive rate of at most 14 %. An average execution time of 0.7 s per image was achieved. Experiments have shown that the designed algorithm provided a suitable quantification of filaments when compared with human perception and standard methods. The algorithm's average execution time proved its suitability for being optimally mapped into a computational architecture to provide real-time monitoring.

Monoclonal antibody-based serological assays and immunocapture-RT-PCR for detecting Rice dwarf virus in field rice plants and leafhopper vectors.

PubMed

Wu, Jianxiang; Ni, Yuequn; Liu, Huan; Ding, Ming; Zhou, Xueping

2014-01-01

Rice dwarf virus (RDV) causes Rice dwarf disease, which leads to considerable losses in rice production in Asia. Purified RDV virions were used as the immunogen to prepare monoclonal antibodies (mAbs). Three murine mAbs against RDV were prepared. Plate-trapped antigen enzyme-linked immunosorbent assay (PTA-ELISA), dot enzyme-linked immunosorbent assay (dot-ELISA) and immunocapture-RT-PCR (IC-RT-PCR) were then developed for sensitive, specific, and rapid detection of RDV in rice and leafhopper samples obtained in the field using the mAbs. The PTA-ELISA, dot-ELISA and IC-RT-PCR detected the virus in infected tissue crude extracts diluted at 1:81,920, 1:10,240 and 1:655,360 (w/v, g mL(-1)), in individual viruliferous rice green leafhopper crude extracts diluted at 1:25,600, 1:6400 and 1:3,276,800 (individual leafhopper/μL), respectively. 878 rice field samples and 531 leafhopper field samples from ten provinces of China were screened for the presence of RDV using the two serological assays and the IC-RT-PCR and the results indicated that 37 of the 878 rice samples and 22 of the 531 leafhopper samples were infected by RDV. All positive samples were from Yunnan Province, indicating that RDV is prevalent in this province, but not in the other nine provinces. The dot-ELISA is suitable for routine detection of large-scale rice and leafhopper samples in field surveys. Copyright © 2013 Elsevier B.V. All rights reserved.

Molecularly imprinted polymer/cryogel composites for solid-phase extraction of bisphenol A from river water and wine.

PubMed

Baggiani, Claudio; Baravalle, Patrizia; Giovannoli, Cristina; Anfossi, Laura; Giraudi, Gianfranco

2010-05-01

Superporous monolithic hydrogels (cryogel monoliths) are elastic, sponge-like materials that can be prepared in an aqueous medium through a cryotropic gelation technique. These monoliths show interesting properties for the development of high-throughput solid-phase extraction supports to treat large volumes of aqueous samples. In this work, a cryogel-supported molecularly imprinted solid-phase extraction approach for the endocrine disruptor bisphenol A (BPA) from river water and wine samples is presented. An imprinted polymer with molecular recognition properties for BPA was prepared in acetonitrile by thermal polymerization of a mixture of 4,4'-dihydroxy-2,2-diphenyl-1,1,1,3,3,3-trifluoropropane as a mimic template of BPA, 4-vinylpyridine and trimethylolpropane trimethacrylate in a molar ratio of 1 + 6 + 6. Fine imprinted particles (<10 microm) were embedded in a poly-acrylamide-co-N,N'-methylenbisacrylamide cryogel obtained by ammonium persulfate-induced cryopolymerization at -18 degrees C. The resulting monolithic gel was evaluated for its use as a sorbent support in an off-line solid-phase extraction approach to recover BPA from dilute aqueous samples with minimum pre-loading work-up. The optimized extraction protocol resulted in a reliable MISPE method suitable to selectively extract and preconcentrate BPA from river water and red wine samples, demonstrating the practical feasibility of cryogel-trapped imprinted polymers as solid-phase extraction materials.

4-Substituted-2-Methoxyphenol: Suitable Building Block to Prepare New Bioactive Natural-like Hydroxylated Biphenyls.

PubMed

Dettori, Maria Antonietta; Fabbri, Davide; Pisano, Marina; Rozzo, Carla; Palmieri, Giuseppe; Dess, Alessandro; Dallocchio, Roberto; Delogu, Giovanna

2015-02-01

A small collection of eugenol- and curcumin-analog hydroxylated biphenyls was prepared by straightforward methods starting from natural 4-substituted-2-methoxyphenols and their antitumoral activity was evaluated in vitro . Two curcumin-biphenyl derivatives showed interesting growth inhibitory activities on different malignant melanoma cell lines with IC 50 ranging from 13 to 1 µM. Preliminary molecular modeling studies were carried out to evaluate conformations and dihedral angles suitable for antiproliferative activity in hydroxylated biphenyls bearing a side aliphatic chain.

Synthesis and Purification of Iodoaziridines Involving Quantitative Selection of the Optimal Stationary Phase for Chromatography

PubMed Central

Boultwood, Tom; Affron, Dominic P.; Bull, James A.

2014-01-01

The highly diastereoselective preparation of cis-N-Ts-iodoaziridines through reaction of diiodomethyllithium with N-Ts aldimines is described. Diiodomethyllithium is prepared by the deprotonation of diiodomethane with LiHMDS, in a THF/diethyl ether mixture, at -78 °Cin the dark. These conditions are essential for the stability of the LiCHI2 reagent generated. The subsequent dropwise addition of N-Ts aldimines to the preformed diiodomethyllithium solution affords an amino-diiodide intermediate, which is not isolated. Rapid warming of the reaction mixture to 0 °C promotes cyclization to afford iodoaziridines with exclusive cis-diastereoselectivity. The addition and cyclization stages of the reaction are mediated in one reaction flask by careful temperature control. Due to the sensitivity of the iodoaziridines to purification, assessment of suitable methods of purification is required. A protocol to assess the stability of sensitive compounds to stationary phases for column chromatography is described. This method is suitable to apply to new iodoaziridines, or other potentially sensitive novel compounds. Consequently this method may find application in range of synthetic projects. The procedure involves firstly the assessment of the reaction yield, prior to purification, by 1H NMR spectroscopy with comparison to an internal standard. Portions of impure product mixture are then exposed to slurries of various stationary phases appropriate for chromatography, in a solvent system suitable as the eluent in flash chromatography. After stirring for 30 min to mimic chromatography, followed by filtering, the samples are analyzed by 1H NMR spectroscopy. Calculated yields for each stationary phase are then compared to that initially obtained from the crude reaction mixture. The results obtained provide a quantitative assessment of the stability of the compound to the different stationary phases; hence the optimal can be selected. The choice of basic alumina, modified to activity IV, as a suitable stationary phase has allowed isolation of certain iodoaziridines in excellent yield and purity. PMID:24893769

Microstructure and trapped field of YBCO bulk single-grain superconductors prepared by interior seeding

NASA Astrophysics Data System (ADS)

Radusovska, M.; Diko, P.; Piovarci, S.; Park, S.-D.; Jun, B.-H.; Kim, C.-J.

2017-10-01

The microstructural analyses of YBCO bulk single-grain superconductors grown by interior seeding with taller and shorter upper pellets have shown that a suitable upper pellet height can lower the porosity in the upper part of the sample, produce a more appropriate distribution of pinning centres in the form of Y-211 particles and suppress subgrain formation with a higher crystal misalignment in the c-growth sector (c-GS), which can lead to a higher measured trapped magnetic field and a more uniform cone of the trapped-field profile. The observed bulging of the sample surface at the c-GS can be explained by the edge melt distribution model, which shows that macroscopic mass transport to the growth sector occurs with higher growth rates.

Influence of sample processing on the analysis of carotenoids in maize.

PubMed

Rivera, Sol; Canela, Ramon

2012-09-21

We performed a number of tests with the aim to develop an effective extraction method for the analysis of carotenoid content in maize seed. Mixtures of methanol-ethyl acetate (6:4, v/v) and methanol-tetrahydrofuran (1:1, v/v) were the most effective solvent systems for carotenoid extraction from maize endosperm under the conditions assayed. In addition, we also addressed sample preparation prior to the analysis of carotenoids by liquid chromatography (LC). The LC response of extracted carotenoids and standards in several solvents was evaluated and results were related to the degree of solubility of these pigments. Three key factors were found to be important when selecting a suitable injection solvent: compatibility between the mobile phase and injection solvent, carotenoid polarity and content in the matrix.

Extemporaneous clobazam suspensions for paediatric use prepared from commercially available tablets and pure drug.

PubMed

Buontempo, F; Moretton, M A; Quiroga, E; Chiappetta, D A

2013-01-01

Two clobazam aqueous suspensions for paediatric oral usage (5 mg/ml) were investigated to determinate its physicochemical stability under different storage conditions. Formulations were stored at 4 and 25 °C and the clobazam content was determined by High Performance Liquid Chromatography. Each sample was analyzed by triplicate at different time points (0, 7, 14, 28 and 56 days). Liquid suspensions were successfully formulated from pure drug and commercially available tablets. In both cases, samples showed suitable physical stability. Clobazam was chemically stable in aqueous suspension during the 56 days of the study at the two storage temperatures. All the tried oral liquid formulations can be conserved at 4 and 25 °C at least 56-day period. Copyright © 2013 SEFH. Published by AULA MEDICA. All rights reserved.

Multiplex PCR method for MinION and Illumina sequencing of Zika and other virus genomes directly from clinical samples.

PubMed

Quick, Joshua; Grubaugh, Nathan D; Pullan, Steven T; Claro, Ingra M; Smith, Andrew D; Gangavarapu, Karthik; Oliveira, Glenn; Robles-Sikisaka, Refugio; Rogers, Thomas F; Beutler, Nathan A; Burton, Dennis R; Lewis-Ximenez, Lia Laura; de Jesus, Jaqueline Goes; Giovanetti, Marta; Hill, Sarah C; Black, Allison; Bedford, Trevor; Carroll, Miles W; Nunes, Marcio; Alcantara, Luiz Carlos; Sabino, Ester C; Baylis, Sally A; Faria, Nuno R; Loose, Matthew; Simpson, Jared T; Pybus, Oliver G; Andersen, Kristian G; Loman, Nicholas J

2017-06-01

Genome sequencing has become a powerful tool for studying emerging infectious diseases; however, genome sequencing directly from clinical samples (i.e., without isolation and culture) remains challenging for viruses such as Zika, for which metagenomic sequencing methods may generate insufficient numbers of viral reads. Here we present a protocol for generating coding-sequence-complete genomes, comprising an online primer design tool, a novel multiplex PCR enrichment protocol, optimized library preparation methods for the portable MinION sequencer (Oxford Nanopore Technologies) and the Illumina range of instruments, and a bioinformatics pipeline for generating consensus sequences. The MinION protocol does not require an Internet connection for analysis, making it suitable for field applications with limited connectivity. Our method relies on multiplex PCR for targeted enrichment of viral genomes from samples containing as few as 50 genome copies per reaction. Viral consensus sequences can be achieved in 1-2 d by starting with clinical samples and following a simple laboratory workflow. This method has been successfully used by several groups studying Zika virus evolution and is facilitating an understanding of the spread of the virus in the Americas. The protocol can be used to sequence other viral genomes using the online Primal Scheme primer designer software. It is suitable for sequencing either RNA or DNA viruses in the field during outbreaks or as an inexpensive, convenient method for use in the lab.

Design and development of molecularly imprinted polymers for the selective extraction of deltamethrin in olive oil: An integrated computational-assisted approach.

PubMed

Martins, Nuno; Carreiro, Elisabete P; Locati, Abel; Ramalho, João P Prates; Cabrita, Maria João; Burke, Anthony J; Garcia, Raquel

2015-08-28

This work firstly addresses the design and development of molecularly imprinted systems selective for deltamethrin aiming to provide a suitable sorbent for solid phase (SPE) extraction that will be further used for the implementation of an analytical methodology for the trace analysis of the target pesticide in spiked olive oil samples. To achieve this goal, a preliminary evaluation of the molecular recognition and selectivity of the molecularly imprinted polymers has been performed. In order to investigate the complexity of the mechanistic basis for template selective recognition in these polymeric matrices, the use of a quantum chemical approach has been attempted providing new insights about the mechanisms underlying template recognition, and in particular the crucial role of the crosslinker agent and the solvent used. Thus, DFT calculations corroborate the results obtained by experimental molecular recognition assays enabling one to select the most suitable imprinting system for MISPE extraction technique which encompasses acrylamide as functional monomer and ethylene glycol dimethacrylate as crosslinker. Furthermore, an analytical methodology comprising a sample preparation step based on solid phase extraction has been implemented using this "tailor made" imprinting system as sorbent, for the selective isolation/pre-concentration of deltamethrin from olive oil samples. Molecularly imprinted solid phase extraction (MISPE) methodology was successfully applied for the clean-up of spiked olive oil samples, with recovery rates up to 94%. Copyright © 2015 Elsevier B.V. All rights reserved.

Methodological proposal for the remediation of a site affected by phosphogypsum deposits

NASA Astrophysics Data System (ADS)

Martínez-Sanchez, M. J.; Perez-Sirvent, C.; Bolivar, J. P.; Garcia-Tenorio, R.

2012-04-01

The accumulation of phosphogysum (PY) produces a well known environmental problems. The proposals for the remediation of these sites require multidisciplinary and very specific studies. Since they cover large areas a sampling design specifically outlined for each case is necessary in order the contaminants, transfer pathways and particular processes can be correctly identified. In addition to a suitable sampling of the soil, aquatic medium and biota, appropriate studies of the space-temporal variations by means of control samples are required. Two different stages should be considered: 1.- Diagnostic stage This stage includes preliminary studies, identification of possible sources of radiosotopes, design of the appropriate sampling plan, hydrogeological study, characterization and study of the space-temporal variability of radioisotopes and other contaminants, as well as the risk assessement for health and ecosystems, that depends on the future use of the site. 2.- Remediation proposal stage It comprises the evaluation and comparison of the different procedures for the decontamination/remediation, including models experiments at the laboratory. To this respect, the preparation and detailed study of a small scale pilot project is a task of particular relevance. In this way the suitability of the remediating technology can be checked, and its performance optimized. These two stages allow a technically well-founded proposal to be presented to the Organisms or Institutions in charge of the problem and facilitate decision-making. It both stages be included in a social communication campaign in order the final proposal be accepted by stakeholders.

Multiresidue determination of pesticides in tea by gas chromatography-tandem mass spectrometry.

PubMed

Saito-Shida, Shizuka; Nemoto, Satoru; Teshima, Reiko

2015-01-01

An efficient and reliable GC-MS/MS method for the multiresidue determination of pesticides in tea was developed by modifying the Japanese official multiresidue method. Sample preparation was carefully optimized for the efficient removal of coextracted matrix components. The optimal sample preparation procedure involved swelling of the sample in water; extraction with acetonitrile; removal of water by salting-out; and sequential cleanup by ODS, graphitized carbon black/primary secondary amine (GCB/PSA) and silica gel cartridges prior to GC-MS/MS analysis. The recoveries of 162 pesticides from fortified (at 0.01 mg kg(-1)) green tea, oolong tea, black tea and matcha (powdered green tea) were mostly (95-98% of the tested pesticides) within the range of 70-120%, with relative standard deviations of <20%. Poor recovery of triazole pesticides was considered to be due to low recovery from the silica gel cartridges. The test solutions obtained by the modified method contained relatively small amounts of pigments, caffeine and other matrix components and were cleaner than those obtained by the original Japanese official multiresidue method. No interfering peaks were observed in the blank chromatograms, indicating the high selectivity of the modified method. The overall results suggest that the developed method is suitable for the quantitative analysis of GC-amenable pesticide residues in tea.

Structural morphology of zinc oxide structures with antibacterial application of calamine lotion

NASA Astrophysics Data System (ADS)

Ann, Ling Chuo; Mahmud, Shahrom; Bakhori, Siti Khadijah Mohd; Sirelkhatim, Amna; Mohamad, Dasmawati; Hasan, Habsah; Seeni, Azman; Rahman, Rosliza Abdul

2015-04-01

In this study, we report the structural morphology of a zinc oxide (ZnO) sample and antibacterial application of the ZnO structures in calamine lotion. Antibacterial activities of the calamine lotion towards Staphylococcus aureus and Pseudomonas aeruginosa were investigated. The structural morphology of ZnO sample was studied using a transmission electron microscope (TEM) and a field-emission scanning electron microscope (FESEM). The morphologies of the ZnO structure consisted of many rod and spherical structures. The particle sizes of the sample ranged from 40 nm to 150 nm. A calamine lotion was prepared through mixing the ZnO structures with other constituents in suitable proportion. The energy-dispersive x-ray spectroscopy (EDS) revealed the presence of large amount of ZnO structures whiles the X-ray diffraction (XRD) results showed a good crystalline property of ZnO in the calamine lotion mixture. The morphological structures of ZnO were found to remain unchanged in the calamine lotion mixture through FESEM imaging. In the antibacterial test, prepared calamine lotion exhibited a remarkable bacterial inhibition on Staphylococcus aureus and Pseudomonas aeruginosa after 24 h of treatment. The bactericidal capability of calamine lotion was largely due to the presence of ZnO structures which induce high toxicity and killing effect on the bacteria.

[Evaluation of three methods for forensic diatom test].

PubMed

Wang, Yuzhong; Zhao, Jian; Li, Peng; Hu, Sunlin; Wang, Huipin; Wang, Huijun; Liu, Chao

2015-03-01

To compare the efficacy of three methods for forensic diatom test, namely strong acid digestion-centrifuge enrichment-light microscopy (SD-CE-LM), microwave digestion-membrane filtration-automated scanning electron microscopy (MD-ME-SEM), and microwave digestion-membrane filtration-light microscopy (MD-MF-LM). Sixty samples were randomly divided into 3 groups for diatom test using three methods, and the sample preparation time, degree of digestion and recovery rate of diatoms were compared. The sample preparation time was the shortest with MD-MF-LM and the longest with SD-CE-LM (P<0.05). MD-ME-SEM and MD-MF-LM allowed more thorough tissue digestion than SD-CE-LM. MD-ME-SEM resulted in the highest total recovery rate of diatom, followed by MD-MF-LM and then by SD-CE-LM (P<0.05); the recover rate of different diatom species was the highest with MD-ME-SEM, followed by MD-MF-LM and SD-CE-LM (P<0.05). SD-CE-LM has a low recovery rate of diatoms especially for those with lengths shorter than 40 µm or densities less than 1/5. With a high recovery rate and accuracy in diatom test, MD-ME-SEM is suitable for diagnosis of suspected drowning cases. MD-MF-LM is highly efficient, sensitive and convenient for forensic diatom test.

[Residues of chloramphenicol in the calf organism following parenteral administration of the Czechoslovak preparation Chronicin inj].

PubMed

Malíková, M; Habrda, J

1976-03-01

Using two biological methods the chloramphenicol content in various tissues of 11 calves aged 3--18 days was determined after a single-dose therapeutical administration of the Czechoslovak preparation of Chronicin inj. in the quantity of 12 mg kg-1 body mass. Of four test strains, solely Micrococcus flavus (ATCC 10240) strain proved suitable. Chloramphenicol was quantitatively determined by reading from transformed standard curves. An evalua tion of the two approximately equally sensitive methods yielded the following results: three days after the injection all calves were positive, at 5 and 10 days, one of three calves in each group was negativ similarly to both calves slaughtered 15 days post injection. The residues appeared most frequently in the liver, at the site of injection, and in the fore and hind musculature. Maximum detectable concentrations were recorded in the liver. Culinary and technological treatment of positive meat and liver samples revealed that 15 minutes' boiling and 30 minutes' roasting destroyed the microbiologically active chloramphenicol residues in the samples. Neither deep freezing nor salting was sufficient for residue inactivation, although in some samples a decrease in biological chloramphenicol activity by circa 20--30% was recorded. a preslaughter withdrawal time of 15 days is recommended.

Determination of coumarin in seasonal bakery products using QuEChERS and GC-MS.

PubMed

Vetter, F; Müller, C; Stöckelhuber, M; Bracher, F

2017-06-01

Cinnamon is a traditional herbal drug, but more importantly, it is used as a flavor compound in the production of foodstuff. Due to the content of significant concentrations of coumarin in Cassia cinnamon, effective control of the coumarin content in seasonal bakery products like ginger bread and cinnamon biscuits is urgently needed. Here we present a novel, fast and fully validated protocol for the determination of coumarin in marketed bakery products using the QuEChERS sample preparation technique in combination with GC-MS analysis. Ten grams of homogenized sample was mixed with 20 mL acetonitrile/water (1:1) and 5 g magnesium sulfate/sodium chloride mixture (4:1). The organic phase was cleaned by dSPE with 25 mg magnesium sulfate/PSA (5:1). The LOD was 0.15 μg/mL and the LOQ 0.50 μg/mL. We detected a mean coumarin content of 19.5 μg/kg in 9 out of 14 seasonal food products (ranging from 1.45 to 39.4 mg/kg). No coumarin was detected in five cinnamon containing products. With this investigation we demonstrate that the QuEChERS sample preparation, previously applied mainly to the analysis of pesticides in vegetables, is also suitable for other complex matrices.

Suspensions as a Valuable Alternative to Extemporaneously Compounded Capsules.

PubMed

Dijkers, Eli; Nanhekhan, Valerie; Thorissen, Astrid; Polonini, Hudson

2017-01-01

The objective of this study was to determine the variation in content of 74 different active pharmaceutical ingredients (APIs) and compare it with what is known in the literature for the content uniformity of extemporaneous prepared capsules. Active pharmaceutical ingredients quantification was performed by high-performance liquid chromatography, via a stability-indicating method. Samples for all active pharmaceutical ingredients were taken throughout a 90-day period and the content was determined. In total, 5,190 different samples were analyzed for 74 different active pharmaceutical ingredients at room (15°C to 25°C) or controlled refrigerated temperature (2°C to 8°C). Each of these datasets was analyzed according to the United States Pharmacopeia Content Uniformity monograph, corrected for the sample number. The mean acceptance values were well within specifications. In addition, all suspensions complied with the criteria defined by the British Pharmacopoeia monograph for Content Uniformity of Liquid Dispersions for both room and controlled refrigerated temperature. In previous studies, it was found that a routine weight variation check is often not sufficient for quality assurance of extemporaneous prepared capsules. Compounded oral liquids show little variation in content for 74 different active pharmaceutical ingredients; therefore, compounded oral liquids are a suitable alternative when compounding individualized medications for patients. Copyright© by International Journal of Pharmaceutical Compounding, Inc.

Processing, Mechanical and Optical Properties of Additive-Free ZrC Ceramics Prepared by Spark Plasma Sintering

PubMed Central

Musa, Clara; Licheri, Roberta; Orrù, Roberto; Cao, Giacomo; Sciti, Diletta; Silvestroni, Laura; Zoli, Luca; Balbo, Andrea; Mercatelli, Luca; Meucci, Marco; Sani, Elisa

2016-01-01

In the present study, nearly fully dense monolithic ZrC samples are produced and broadly characterized from microstructural, mechanical and optical points of view. Specifically, 98% dense products are obtained by Spark Plasma Sintering (SPS) after 20 min dwell time at 1850 °C starting from powders preliminarily prepared by Self-propagating High-temperature Synthesis (SHS) followed by 20 min ball milling. A prolonged mechanical treatment up to 2 h of SHS powders does not lead to appreciable benefits. Vickers hardness of the resulting samples (17.5 ± 0.4 GPa) is reasonably good for monolithic ceramics, but the mechanical strength (about 250 MPa up to 1000 °C) could be further improved by suitable optimization of the starting powder characteristics. The very smoothly polished ZrC specimen subjected to optical measurements displays high absorption in the visible-near infrared region and low thermal emittance at longer wavelengths. Moreover, the sample exhibits goodspectral selectivity (2.1–2.4) in the 1000–1400 K temperature range. These preliminary results suggest that ZrC ceramics produced through the two-step SHS/SPS processing route can be considered as attractive reference materials for the development of innovative solar energy absorbers. PMID:28773611

Quality control of next-generation sequencing library through an integrative digital microfluidic platform.

PubMed

Thaitrong, Numrin; Kim, Hanyoup; Renzi, Ronald F; Bartsch, Michael S; Meagher, Robert J; Patel, Kamlesh D

2012-12-01

We have developed an automated quality control (QC) platform for next-generation sequencing (NGS) library characterization by integrating a droplet-based digital microfluidic (DMF) system with a capillary-based reagent delivery unit and a quantitative CE module. Using an in-plane capillary-DMF interface, a prepared sample droplet was actuated into position between the ground electrode and the inlet of the separation capillary to complete the circuit for an electrokinetic injection. Using a DNA ladder as an internal standard, the CE module with a compact LIF detector was capable of detecting dsDNA in the range of 5-100 pg/μL, suitable for the amount of DNA required by the Illumina Genome Analyzer sequencing platform. This DMF-CE platform consumes tenfold less sample volume than the current Agilent BioAnalyzer QC technique, preserving precious sample while providing necessary sensitivity and accuracy for optimal sequencing performance. The ability of this microfluidic system to validate NGS library preparation was demonstrated by examining the effects of limited-cycle PCR amplification on the size distribution and the yield of Illumina-compatible libraries, demonstrating that as few as ten cycles of PCR bias the size distribution of the library toward undesirable larger fragments. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Zn(2+) release behavior and surface characteristics of Zn/LDPE nanocomposites and ZnO/LDPE nanocomposites in simulated uterine solution.

PubMed

Yang, Zhihong; Xie, Changsheng; Xia, Xianping; Cai, Shuizhou

2008-11-01

To decrease the side effects of the existing copper-bearing intrauterine devices, the zinc/low-density polyethylene (Zn/LDPE) nanocomposite and zinc-oxide/low-density polyethylene (ZnO/LDPE) nanocomposite have been developed in our research for intrauterine devices (IUDs). In this study, the influences of preparation methods of nanocomposites and particle sizes of zinc and zinc oxide on Zn(2+) release from composites incubated in simulated uterine solution were investigated. All release profiles are biphasic: an initial rapid release phase is followed by a near zero-order release period. Zn(2+) release rates of nanocomposites prepared by compressing moulding are higher than those of the nanocomposites prepared by hot-melt extrusing. Compared with Zn(2+) release from the microcomposites, the release profiles of the nanocomposites exhibit a sharp decrease in Zn(2+) release rate in the first 18 days, an early onset of the zero-order release period and a high release rate of Zn(2+) at the later stage. The microstructure of the Zn/LDPE sample and the ZnO/LDPE sample after being incubated for 200 days was characterized by SEM, XRD and EDX techniques. The results show that the dissolution depth of ZnO/LDPE nanocomposite is about 60 mum. Lots of pores were formed on the surface of the Zn/LDPE sample and ZnO/LDPE sample, indicating that these pores can provide channels for the dissolution of nanoparticles in the matrix. The undesirable deposits that are composed of ZnO are only detected on the surface of Zn/LDPE nanocomposite, which may increase the risk of side effects associated with IUDs. It can be expected that ZnO/LDPE nanocomposite is more suitable for IUDs than Zn/LDPE nanocomposite.

Detection of nanoplastics in food by asymmetric flow field-flow fractionation coupled to multi-angle light scattering: possibilities, challenges and analytical limitations.

PubMed

Correia, Manuel; Loeschner, Katrin

2018-02-06

We tested the suitability of asymmetric flow field-flow fractionation (AF4) coupled to multi-angle light scattering (MALS) for detection of nanoplastics in fish. A homogenized fish sample was spiked with 100 nm polystyrene nanoparticles (PSNPs) (1.3 mg/g fish). Two sample preparation strategies were tested: acid digestion and enzymatic digestion with proteinase K. Both procedures were found suitable for degradation of the organic matrix. However, acid digestion resulted in large PSNPs aggregates/agglomerates (> 1 μm). The presence of large particulates was not observed after enzymatic digestion, and consequently it was chosen as a sample preparation method. The results demonstrated that it was possible to use AF4 for separating the PSNPs from the digested fish and to determine their size by MALS. The PSNPs could be easily detected by following their light scattering (LS) signal with a limit of detection of 52 μg/g fish. The AF4-MALS method could also be exploited for another type of nanoplastics in solution, namely polyethylene (PE). However, it was not possible to detect the PE particles in fish, due to the presence of an elevated LS background. Our results demonstrate that an analytical method developed for a certain type of nanoplastics may not be directly applicable to other types of nanoplastics and may require further adjustment. This work describes for the first time the detection of nanoplastics in a food matrix by AF4-MALS. Despite the current limitations, this is a promising methodology for detecting nanoplastics in food and in experimental studies (e.g., toxicity tests, uptake studies). Graphical abstract Basic concept for the detection of nanoplastics in fish by asymmetric flow field-flow fractionation coupled to multi-angle light scattering.

Performance and Storage Integrity of Dried Blood Spots for PCB, BFR and Pesticide Measurements

PubMed Central

Batterman, Stuart; Chernyak, Sergei

2014-01-01

Dried blood spots (DBS) can provide accurate and valuable estimates of exposure to environmental toxicants, and the use of information derived from archived newborn DBS information has enormous potential to open up new research on the impacts of early chemical exposure on disease. Broad application of DBS for the purpose of quantitative exposure estimation requires robust and validated methods. This study investigates the suitability of DBS analyses for population studies of exposure to three chemical groups: polychlorinated biphenyls (PCBs), brominated flame retardants (BFRs), and chlorinated pesticides. It examines background (matrix) contamination, recovery and extraction variability, sensitivity, and storage stability. DBS samples prepared using 50 μL of adult blood were analyzed by GC/MS, and method performance was confirmed by using certified materials and paired DBS-blood samples from six volunteers. Several of the target compounds and their degradation products have not been previously measured in DBS. All target compounds were detected in DBS samples collected from the volunteers. Sample DBS cards showed background contamination of several compounds. When stored at room temperature, target compounds, excluding PBDEs, were stable for up to one month. When refrigerated or frozen, stability was acceptable for all compounds up to one year, and multiyear storage appears acceptable at colder (e.g., −80 °C) temperatures. Multicompartment models may be used to estimate or correct for storage losses. Considering concentrations of contaminants for adults and children reported in the literature, and experimental values of detection limits and background contamination, DBS samples are suitable for quantifying exposures to many PCBs, BFRs and persistent pesticides. PMID:25058892

Effect of ZrO2 on the sintering behavior, strength and high-frequency dielectric properties of electrical ceramic porcelain insulator

NASA Astrophysics Data System (ADS)

Singh Mehta, Niraj; Sahu, Praveen Kumar; Ershad, Md; Saxena, Vipul; Pyare, Ram; Ranjan Majhi, Manas

2018-01-01

In the present study, the effect of ZrO2 on the sintering, strength and dielectric behavior of electrical ceramic porcelain insulator with substituting alumina content by zirconia (in weight percentage from 0% to 30%) is investigated. The different composition of samples containing different zirconia (ZrO2) contents of 0, 10, 20, and 30 wt% are prepared using the uniaxial pressure technique applying 160 MPa pressure. Further, the prepared samples are also analyzed for sintering temperatures (1350 °C), and effects are observed on mechanical and electric properties of porcelain insulator. Different characterizations such as Dilatometer, x-ray diffraction, scanning electron microscopy and differential thermal analysis/thermo gravimetric analysis were used to evaluate the thermal, phase detection, micro structural and weight loss changes by increasing concentration of ZrO2 on base porcelain composition. At 1350 °C, for the composition having 20 wt% ZrO2 with 10 wt% alumina, the maximum density was observed 2.81 g cm-3 with a porosity of 2.23%. The highest tensile strength of 41 ± 3 MPa is observed for the same sample composition. The minimum value of thermal expansion coefficient is found to be in the range of 10-6 for the sample with 30 wt% ZrO2 content sintered at 1350 °C compared to other prepared samples. Similarly, the highest dielectric value (5.1-4.4) having dielectric loss (0.08-0.12) is achieved for the sample with 30 wt% ZrO2 content sintered at 1350 °C in the frequency range of 4-20 GHz at room temperature. According to the mechanical properties, the composition having 20 wt% ZrO2 on base ceramic porcelain composition has enormous potential to serve as a high strength refractory material. For dielectric properties, the composition having 30 wt% ZrO2 is more suitable for the electrical application.

Evaluation of porogen factors for the preparation of ion imprinted polymer monoliths used in mercury removal

PubMed Central

Rahman, Siti Khadijah Ab.; Yusof, Nor Azah; Abdullah, Abdul Halim; Idris, Azni; Al-lohedan, Hamad A.

2018-01-01

In the present study, ion imprinted polymer monoliths (IIPMs) were developed to overcome the limitations of ion imprinted polymer particles (IIPPs) used for the removal of Hg(II) ions from waste water samples. The adsorbents preparation, characterization and Hg(II) removal were very well reported. The IIPMs on porogen optimization was prepared using the molding technique with Hg(II) as a template ion, [2-(methacryloyloxy)ethyl]trimethylammonium cysteine (MAETC) as ligand, methacrylic acid (MAA) as functional monomer, ethylene glycol dimethacrylamide (EGDMA) as cross-linker, benzoyl peroxide as an initiator and methanol and acetonitrile as porogen in the polypropylene tube (drinking straw) as mold. The IIPMs prepared with higher volumes of porogen were indicated to have a good adsorption rate for the Hg(II) removal along with good water permeability and larger porosity as compared to a lower volume of porogen. The IIPMs prepared using the binary porogen were able to improve the porosity and surface area of the monolithic polymers as compared to the single porogen added IIPMs. Finally, we indicate from our analysis that the IIPM having the efficient capacity for the Hg(II) ions is easy to prepare, and has higher water permeability along with high porosity and high adsorption capacity and all these factors making it one of the suitable adsorbent for the successful removal of Hg(II) ions. PMID:29649325

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

Influence of the Addition of Minced Fish on the Preparation of Fish Sausage: Effects on Sensory Properties.

PubMed

Lago, Amanda M T; Vidal, Ana C C; Schiassi, Maria C E V; Reis, Tatiana; Pimenta, Carlos; Pimenta, Maria E S G

2017-02-01

In this study, we evaluated the effect of minced fish (MF) inclusion on the acceptance of tilapia sausages. One hundred consumers participated in the sensory acceptance test in relation to the attributes appearance, color, aroma, flavor, texture, overall impression, and purchase intent. The tests were conducted using the same composition of ingredients, varying only the raw material (MF and fillet), resulting in 5 different formulations. To represent the results of the sensory attributes, we generated internal preference maps through principal component analysis and parallel factor analysis, as well as frequency histograms. The data showed greater acceptability for the sample produced with 50% MF, although all had shown satisfactory results. We conclude that inclusion of MF can be suitable in the preparation of fish sausage due to high consumer acceptance. © 2017 Institute of Food Technologists®.

Mesoporous cellular-structured carbons derived from glucose-fructose syrup and their adsorption properties towards acetaminophen

NASA Astrophysics Data System (ADS)

Tzvetkov, George; Spassov, Tony; Kaneva, Nina; Tsyntsarski, Boyko

Here, a series of cellular-structured and predominantly mesoporous carbons were prepared via carbonization of glucose-fructose syrup (GFS) with sulfuric acid and subsequent calcination between 400∘C and 700∘C. Comparative results on the microstructure, chemical and textural properties of the newly produced carbons are presented. Furthermore, their adsorption performance for removal of acetaminophen from water was tested and it was found that the carbon calcined at 700∘C has a maximum adsorption capacity (98.7mgṡg-1) among all samples due to its suitable textural properties (BET surface area of 418m2ṡg-1 and total pore volume of 0.2cm3ṡg-1). This study demonstrates the potential use of GFS as a precursor in the preparation of carbonaceous materials for removal of biologically-active micropollutants from water.

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

[Study on the analytical methods of catechins in tea and green tea polyphenol samples by high performance liquid chromatography].

PubMed

Dai, J; Wang, H X; Chen, S W; Tang, J

2001-09-01

Hypersil BDS C18 and Zorbax SB C18, suitable to separate simultaneously seven kinds of catechins and caffeine, were screened out from seven brands of reversed-phase columns. Mobile phase was a solution of methanol-water-acetic acid (or trifluoro acetic acid). Seven kinds of catechins in tea samples from six places in China and three green tea polyphenol(GTP) samples from different producers were separated and determined in 30 min by isocratic and gradient elutions. The effects of mobile phase components and temperature of column on retention parameters of catechins and caffeine are reviewed. Chromatographic conditions and pretreatment methods of samples were optimized. Gallocatechin gallate(GCG) and (-)-catechin gallate(CG) were identified by electrospray ionization mass spectrometry(ESI-MS) and prepared by high performance liquid chromatography for quantitative analysis. The other catechins, (-)-epigallocatechin (EGC), (+)-catechin (D-C), (-)-epicatechin(EC), (-)-epigallocatechin gallate(EGCG), (-)-epicatechin gallate(ECG) were identified with standards.

Microstructural Characterization of Semi-Interpenetrating Polymer Networks by Positron Lifetime Spectroscopy

NASA Technical Reports Server (NTRS)

Singh, Jag J.; Pater, Ruth H.; Eftekhari, Abe

1996-01-01

Thermoset and thermoplastic polyimides have complementary physical and mechanical properties. Whereas thermoset polyimides are brittle and generally easier to process, thermoplastic polyimides are tough but harder to process. A combination of these two types of polyimides may help produce polymers more suitable for aerospace applications. Semi-Interpenetrating Polymer Networks (S-IPN) of thermoset LaRC(TM)-RP46 and thermoplastic LaRC(TM)-IA polyimides were prepared in weight percent ratios ranging from 100:0 to 0:100. Positron lifetime measurements were made in these samples to correlate their free volume features with physical and mechanical properties. As expected, positronium atoms are not formed in these samples. The second lifetime component has been used to infer the positron trap dimensions. The 'free volume' goes through a minimum at a ratio of about 50:50, and this suggests that S-IPN samples are not merely solid solutions of the two polymers. These data and related structural properties of the S-IPN samples are discussed.

Quantitation of active pharmaceutical ingredients and excipients in powder blends using designed multivariate calibration models by near-infrared spectroscopy.

PubMed

Li, Weiyong; Worosila, Gregory D

2005-05-13

This research note demonstrates the simultaneous quantitation of a pharmaceutical active ingredient and three excipients in a simulated powder blend containing acetaminophen, Prosolv and Crospovidone. An experimental design approach was used in generating a 5-level (%, w/w) calibration sample set that included 125 samples. The samples were prepared by weighing suitable amount of powders into separate 20-mL scintillation vials and were mixed manually. Partial least squares (PLS) regression was used in calibration model development. The models generated accurate results for quantitation of Crospovidone (at 5%, w/w) and magnesium stearate (at 0.5%, w/w). Further testing of the models demonstrated that the 2-level models were as effective as the 5-level ones, which reduced the calibration sample number to 50. The models had a small bias for quantitation of acetaminophen (at 30%, w/w) and Prosolv (at 64.5%, w/w) in the blend. The implication of the bias is discussed.

Novel nanoliposomal encapsulated omega-3 fatty acids and their applications in food.

PubMed

Rasti, Babak; Erfanian, Arezoo; Selamat, Jinap

2017-09-01

The aim of the present research was to evaluate the application, stability and suitability of ω3 polyunsaturated fatty acids (PUFAs) incorporated nanoliposomes in food enrichment. Nanoliposomal ω3 PUFAs was prepared by Mozafari method, and their application in bread and milk was compared with unencapsulated (fish oil) and microencapsulated ω3 PUFAs. Sensory evaluation was conducted to determine the perceptible sensory difference/similarity between control, unencapsulated, microencapsulated, and nanoliposomal ω3 PUFAs enriched foods. Results showed no significant (p=0.11) detectable difference between control and nanoliposomal ω3 PUFAs enriched samples while, samples enriched with unencapsulated or microencapsulated ω3 PUFAs showed significant (p=0.02) fishy flavor. Moreover, significantly (p<0.01) higher ω3 PUFAs % recovery and lower peroxide and anisidine values were observed in nanoliposomal ω3 PUFAs enriched samples in comparison with other samples. In conclusion, an effective and reproducible method for application of ω3 PUFAs in the food system was developed. Copyright © 2017 Elsevier Ltd. All rights reserved.

Direct determination of Pb in raw milk by graphite furnace atomic absorption spectrometry (GF AAS) with electrothermal atomization sampling from slurries.

PubMed

de Oliveira, Tatiane Milão; Augusto Peres, Jayme; Lurdes Felsner, Maria; Cristiane Justi, Karin

2017-08-15

Milk is an important food in the human diet due to its physico-chemical composition; therefore, it is necessary to monitor contamination by toxic metals such as Pb. Milk sample slurries were prepared using Triton X-100 and nitric acid for direct analysis of Pb using graphite furnace atomic absorption spectrometry - GF AAS. After dilution of the slurries, 10.00µl were directly introduced into the pyrolytic graphite tube without use of a chemical modifier, which acts as an advantage considering this type of matrix. The limits of detection and quantification were 0.64 and 2.14µgl -1 , respectively. The figures of merit studied showed that the proposed methodology without pretreatment of the raw milk sample and using external standard calibration is suitable. The methodology was applied in milk samples from the Guarapuava region, in Paraná State (Brazil) and Pb concentrations ranged from 2.12 to 37.36µgl -1 . Copyright © 2017 Elsevier Ltd. All rights reserved.

Orodispersible films in individualized pharmacotherapy: The development of a formulation for pharmacy preparations.

PubMed

Visser, J Carolina; Woerdenbag, Herman J; Crediet, Stefan; Gerrits, Edwin; Lesschen, Marjan A; Hinrichs, Wouter L J; Breitkreutz, Jörg; Frijlink, Henderik W

2015-01-15

Orodispersible films (ODFs) are promising drug delivery systems for customized small scale pharmacy preparations. The aim of the present study was to develop a versatile casting solution suitable for the extemporaneous production of ODFs to which active pharmaceutical ingredients (APIs) can be added. Different combinations of film forming agents and other excipients and different casting heights were tested for their suitability for production of ODFs. The best suitable casting solution contained hypromellose, carbomer, glycerol, disodium EDTA and trometamol. This casting solution was used to prepare ODFs containing water-soluble APIs (enalapril maleate and prednisolone disodium phosphate) and a poorly water-soluble API (diazepam) for which ethanol 96% was used as co-solvent.The water-soluble APIs as well as ethanol influenced the viscosity of the casting solution, mechanical properties and disintegration time of the ODFs. All ODFs containing API met the requirements on uniformity of mass and uniformity of content set by the European Pharmacopoeia (2014) (Ph. Eur.) 8th edition. In conclusion, ODFs of good pharmaceutical quality can be prepared on small scale. Hereby opening the perspective of using ODFs for individualized pharmacotherapy. Copyright © 2014 Elsevier B.V. All rights reserved.

Suitability of spring wheat varieties for the production of best quality pizza.

PubMed

Tehseen, Saima; Anjum, Faqir Muhammad; Pasha, Imran; Khan, Muhammad Issa; Saeed, Farhan

2014-08-01

The selection of appropriate wheat cultivars is an imperative issue in product development and realization. The nutritional profiling of plants and their cultivars along with their suitability for development of specific products is of considerable interests for multi-national food chains. In this project, Pizza-Hut Pakistan provided funds for the selection of suitable newly developed Pakistani spring variety for pizza production. In this regard, the recent varieties were selected and evaluated for nutritional and functional properties for pizza production. Additionally, emphasis has been paid to assess all varieties for their physico-chemical attributes, rheological parameters and mineral content. Furthermore, pizza prepared from respective flour samples were further evaluated for sensory attributes Results showed that Anmool, Abadgar, Imdad, SKD-1, Shafaq and Moomal have higher values for protein, gluten content, pelshenke value and SDS sedimentation and these were relatively better in studied parameters as compared to other varieties although which were considered best for good quality pizza production. TD-1 got significantly highest score for flavor of pizza and lowest score was observed from wheat variety Kiran. Moreover, it is concluded from current study that all wheat varieties except TJ-83 and Kiran exhibited better results for flavor.

Charcoal as a capture material for silver nanoparticles in the aquatic environment

NASA Astrophysics Data System (ADS)

McGillicuddy, Eoin; Morrison, Liam; Cormican, Martin; Morris, Dearbháile

2017-04-01

Background: The reported antibacterial activity of silver nanoparticles (AgNPs) has led to their incorporation into numerous consumer products including; textiles, domestic appliances, food containers, cosmetics, paints, medical and medicinal products. The AgNPs incorporated into these products can be released into the environment and aquatic system during their production, use and end of life disposal. In the aquatic environment, uncertainties surround the concentration, fate and effects of AgNPs. The aim of this project is to examine charcoal as a potential material for capture of silver nanoparticles from the aquatic environment. Material/methods: Activated charcoal is a commonly used filter material and was selected for this project to determine its suitability as a capture material for AgNPs in water samples. Activated charcoal (Norit® CA1 (Sigma-Aldrich)) was exposed to 100 ppb, 25 nm PVP coated AgNPs (nanoComposix) prepared in Milli-Q water. These solutions were exposed to unaltered charcoal granules for 20 hours after which the decrease of silver in the solution was measured using ICP-MS. In order to improve the removal, the surface area of the charcoal was increased firstly by grinding with a pestle and mortar and secondly by milling the charcoal. The milled charcoal was prepared using an agate ball mill running at 500 rpm for 5 minutes. The activated charcoal was then exposed to samples containing 10 ppb AgNPs. Results: In the initial tests, approximately 10% of the silver was removed from the water samples using the unaltered activated charcoal granules. Further experiments were carried out to compare the unaltered granules with the ground and milled charcoal. These tests were carried out similarly to the previous test however lower concentration of 10 ppb was used. After 20 hours of exposure the granule samples, as previously, showed approximately a 10% reduction in silver content with the ground charcoal giving approximately 30% reduction in silver concentration and in the sample exposed to milled charcoal, approximately 60% reduction in silver concentration was observed. These tests found that increasing the surface area of the charcoal increased the silver reduction in the solution. Conclusions: Data suggest that charcoal may be a suitable material for use in the capture of AgNPs from water samples

Preparation of DNA from cytological material: effects of fixation, staining, and mounting medium on DNA yield and quality.

PubMed

Dejmek, Annika; Zendehrokh, Nooreldin; Tomaszewska, Malgorzata; Edsjö, Anders

2013-07-01

Personalized oncology requires molecular analysis of tumor cells. Several studies have demonstrated that cytological material is suitable for DNA analysis, but to the authors' knowledge there are no systematic studies comparing how the yield and quality of extracted DNA is affected by the various techniques used for the preparation of cytological material. DNA yield and quality were compared using cultured human lung cancer cells subjected to different preparation techniques used in routine cytology, including fixation, mounting medium, and staining. The results were compared with the outcome of epidermal growth factor receptor (EGFR) genotyping of 66 clinical cytological samples using the same DNA preparation protocol. All tested protocol combinations resulted in fragment lengths of at least 388 base pairs. The mounting agent EcoMount resulted in higher yields than traditional xylene-based medium. Spray and ethanol fixation resulted in both a higher yield and better DNA quality than air drying. In liquid-based cytology (LBC) methods, CytoLyt solution resulted in a 5-fold higher yield than CytoRich Red. Papanicolaou staining provided twice the yield of hematoxylin and eosin staining in both liquid-based preparations. Genotyping outcome and quality control values from the clinical EGFR genotyping demonstrated a sufficient amount and amplifiability of DNA in both spray-fixed and air-dried cytological samples. Reliable clinical genotyping can be performed using all tested methods. However, in the cell line experiments, spray- or ethanol-fixed, Papanicolaou-stained slides provided the best results in terms of yield and fragment length. In LBC, the DNA recovery efficiency of the preserving medium may differ considerably, which should be taken into consideration when introducing LBC. Cancer (Cancer Cytopathol) 2013;121:344-353. © 2013 American Cancer Society. © 2013 American Cancer Society.

9 CFR 108.4 - Preparation of blueprints.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 9 Animals and Animal Products 1 2010-01-01 2010-01-01 false Preparation of blueprints. 108.4 Section 108.4 Animals and Animal Products ANIMAL AND PLANT HEALTH INSPECTION SERVICE, DEPARTMENT OF... LICENSED ESTABLISHMENTS § 108.4 Preparation of blueprints. (a) Blueprints, drawn to any suitable scale, on...

Green and efficient sample preparation method for the determination of catalyst residues in margarine by ICP-MS.

PubMed

Hartwig, Carla Andrade; Pereira, Rodrigo Mendes; Novo, Diogo La Rosa; Oliveira, Dirce Taina Teixeira; Mesko, Marcia Foster

2017-11-01

Responding to the need for green and efficient methods to determine catalyst residues with suitable precision and accuracy in samples with high fat content, the present work evaluates a microwave-assisted ultraviolet digestion (MW-UV) system for margarines and subsequent determination of Ni, Pd and Pt using inductively coupled plasma mass spectrometry (ICP-MS). It was possible to digest up to 500mg of margarine using only 10mL of 4molL -1 HNO 3 with a digestion efficiency higher than 98%. This allowed the determination of catalyst residues using the ICP-MS and free of interferences. For this purpose, the following experimental parameters were evaluated: concentration of digestion solution, sample mass and microwave irradiation program. The residual carbon content was used as a parameter to evaluate the efficiency of digestion and to select the most suitable experimental conditions. The accuracy evaluation was performed by recovery tests using a standard solution and certified reference material, and recoveries ranging from 94% to 99% were obtained for all analytes. The limits of detection for Ni, Pd and Pt using the proposed method were 35.6, 0.264 and 0.302ngg -1 , respectively. When compared to microwave-assisted digestion (MW-AD) in closed vessels using concentrated HNO 3 (used as a reference method for sample digestion), the proposed MW-UV could be considered an excellent alternative for the digestion of margarine, as this method requires only a diluted nitric acid solution for efficient digestion. In addition, MW-UV provides appropriate solutions for further ICP-MS determination with suitable precision (relative standard deviation < 7%) and accuracy for all evaluated analytes. The proposed method was applied to margarines from different brands produced in Brazil, and the concentration of catalyst residues was in agreement with the current legislation or recommendations. Copyright © 2017 Elsevier B.V. All rights reserved.

Discreet passive explosive detection through 2-sided waveguided fluorescence

DOEpatents

Harper, Ross James [Stillwater, OK; la Grone, Marcus [Cushing, OK; Fisher, Mark [Stillwater, OK

2011-10-18

The current invention provides a passive sampling device suitable for collecting and detecting the presence of target analytes. In particular, the passive sampling device is suitable for detecting nitro-aromatic compounds. The current invention further provides a passive sampling device reader suitable for determining the collection of target analytes. Additionally, the current invention provides methods for detecting target analytes using the passive sampling device and the passive sampling device reader.

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.

Highly sensitive serological methods for detecting tomato yellow leaf curl virus in tomato plants and whiteflies.

PubMed

Xie, Yan; Jiao, Xiaoyang; Zhou, Xueping; Liu, Huan; Ni, Yuequn; Wu, Jianxiang

2013-05-06

Tomato yellow leaf curl virus (TYLCV) is a member of the genus Begomovirus in the family Geminiviridae, which causes severe losses in tomato production in tropic and subtropic regions. The purified TYLCV virions were used as the immunogen to produce monoclonal antibodies (MAbs) using the hybridoma technology. MAb-based dot enzyme-linked immunosorbent assay (dot-ELISA) and direct tissue blot immunoassay (DTBIA) were developed for sensitive, simple, and rapid detection of TYLCV in field tomato and whitefly (Bemisia tabaci) samples collected from TYLCV prevalent provinces in China. Using the hybridoma technology, six murine MAbs (1C4, 8D10, 6E3, 2F2, 3F4 and 4G3) against TYLCV were prepared. Using the MAb 1C4, dot-ELISA and DTBIA were then established for detecting TYLCV in field tomato and whitefly samples collected from TYLCV prevalent provinces in China. The dot-ELISA could detect TYLCV in infected tissue crude extract diluted at 1:5,120 (w/v, g mL-1), and in viruliferous whitefly homogenate diluted at 1:128 (individual whitefly/μL), respectively. Field tomato samples (n=487) and whitefly samples (n=110) from TYLCV prevalent districts in China were screened for the presence of TYLCV using the two developed methods, and the results were further confirmed by PCR and nucleotide sequencing. The survey revealed that TYLCV is widespread on tomato plants in Zhejiang, Shandong and Henan provinces in China. The developed dot-ELISA is very suitable for the routine detection of TYLCV in field tomato and whitefly samples, and the DTBIA is more suitable for the routine detection of TYLCV in large-scale tomato plant samples collected from TYLCV prevalent areas.

New approach of a transient ICP-MS measurement method for samples with high salinity.

PubMed

Hein, Christina; Sander, Jonas Michael; Kautenburger, Ralf

2017-03-01

In the near future it is necessary to establish a disposal for high level nuclear waste (HLW) in deep and stable geological formations. In Germany typical host rocks are salt or claystone. Suitable clay formations exist in the south and in the north of Germany. The geochemical conditions of these clay formations show a strong difference. In the northern ionic strengths of the pore water up to 5M are observed. The determination of parameters like K d values during sorption experiments of metal ions like uranium or europium as homologues for trivalent actinides onto clay stones are very important for long term safety analysis. The measurement of the low concentrated, not sorbed analytes commonly takes place by inductively coupled plasma mass spectrometry (ICP-MS). A direct measurement of high saline samples like seawater with more than 1% total dissolved salt content is not possible. Alternatives like sample clean up, preconcentration or strong dilution have more disadvantages than advantages for example more preparation steps or additional and expensive components. With a small modification of the ICP-MS sample introduction system and a home-made reprogramming of the autosampler a transient analysing method was developed which is suitable for measuring metal ions like europium and uranium in high saline sample matrices up to 5M (NaCl). Comparisons at low ionic strength between the default and the transient measurement show the latter performs similarly well to the default measurement. Additionally no time consuming sample clean-up or expensive online dilution or matrix removal systems are necessary and the analysation shows a high sensitivity due to the data processing based on the peak area. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparative Evaluation of Three Homogenization Methods for Isolating Middle East Respiratory Syndrome Coronavirus Nucleic Acids From Sputum Samples for Real-Time Reverse Transcription PCR.

PubMed

Sung, Heungsup; Yong, Dongeun; Ki, Chang Seok; Kim, Jae Seok; Seong, Moon Woo; Lee, Hyukmin; Kim, Mi Na

2016-09-01

Real-time reverse transcription PCR (rRT-PCR) of sputum samples is commonly used to diagnose Middle East respiratory syndrome coronavirus (MERS-CoV) infection. Owing to the difficulty of extracting RNA from sputum containing mucus, sputum homogenization is desirable prior to nucleic acid isolation. We determined optimal homogenization methods for isolating viral nucleic acids from sputum. We evaluated the following three sputum-homogenization methods: proteinase K and DNase I (PK-DNase) treatment, phosphate-buffered saline (PBS) treatment, and N-acetyl-L-cysteine and sodium citrate (NALC) treatment. Sputum samples were spiked with inactivated MERS-CoV culture isolates. RNA was extracted from pretreated, spiked samples using the easyMAG system (bioMérieux, France). Extracted RNAs were then subjected to rRT-PCR for MERS-CoV diagnosis (DiaPlex Q MERS-coronavirus, SolGent, Korea). While analyzing 15 spiked sputum samples prepared in technical duplicate, false-negative results were obtained with five (16.7%) and four samples (13.3%), respectively, by using the PBS and NALC methods. The range of threshold cycle (Ct) values observed when detecting upE in sputum samples was 31.1-35.4 with the PK-DNase method, 34.7-39.0 with the PBS method, and 33.9-38.6 with the NALC method. Compared with the control, which were prepared by adding a one-tenth volume of 1:1,000 diluted viral culture to PBS solution, the ranges of Ct values obtained by the PBS and NALC methods differed significantly from the mean control Ct of 33.2 (both P<0.0001). The PK-DNase method is suitable for homogenizing sputum samples prior to RNA extraction.

Comparative Evaluation of Three Homogenization Methods for Isolating Middle East Respiratory Syndrome Coronavirus Nucleic Acids From Sputum Samples for Real-Time Reverse Transcription PCR

PubMed Central

Yong, Dongeun; Ki, Chang-Seok; Kim, Jae-Seok; Seong, Moon-Woo; Lee, Hyukmin

2016-01-01

Background Real-time reverse transcription PCR (rRT-PCR) of sputum samples is commonly used to diagnose Middle East respiratory syndrome coronavirus (MERS-CoV) infection. Owing to the difficulty of extracting RNA from sputum containing mucus, sputum homogenization is desirable prior to nucleic acid isolation. We determined optimal homogenization methods for isolating viral nucleic acids from sputum. Methods We evaluated the following three sputum-homogenization methods: proteinase K and DNase I (PK-DNase) treatment, phosphate-buffered saline (PBS) treatment, and N-acetyl-L-cysteine and sodium citrate (NALC) treatment. Sputum samples were spiked with inactivated MERS-CoV culture isolates. RNA was extracted from pretreated, spiked samples using the easyMAG system (bioMérieux, France). Extracted RNAs were then subjected to rRT-PCR for MERS-CoV diagnosis (DiaPlex Q MERS-coronavirus, SolGent, Korea). Results While analyzing 15 spiked sputum samples prepared in technical duplicate, false-negative results were obtained with five (16.7%) and four samples (13.3%), respectively, by using the PBS and NALC methods. The range of threshold cycle (Ct) values observed when detecting upE in sputum samples was 31.1–35.4 with the PK-DNase method, 34.7–39.0 with the PBS method, and 33.9–38.6 with the NALC method. Compared with the control, which were prepared by adding a one-tenth volume of 1:1,000 diluted viral culture to PBS solution, the ranges of Ct values obtained by the PBS and NALC methods differed significantly from the mean control Ct of 33.2 (both P<0.0001). Conclusions The PK-DNase method is suitable for homogenizing sputum samples prior to RNA extraction. PMID:27374711

Hematocrit-Independent Quantitation of Stimulants in Dried Blood Spots: Pipet versus Microfluidic-Based Volumetric Sampling Coupled with Automated Flow-Through Desorption and Online Solid Phase Extraction-LC-MS/MS Bioanalysis.

PubMed

Verplaetse, Ruth; Henion, Jack

2016-07-05

A workflow overcoming microsample collection issues and hematocrit (HCT)-related bias would facilitate more widespread use of dried blood spots (DBS). This report describes comparative results between the use of a pipet and a microfluidic-based sampling device for the creation of volumetric DBS. Both approaches were successfully coupled to HCT-independent, fully automated sample preparation and online liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) analysis allowing detection of five stimulants in finger prick blood. Reproducible, selective, accurate, and precise responses meeting generally accepted regulated bioanalysis guidelines were observed over the range of 5-1000 ng/mL whole blood. The applied heated flow-through solvent desorption of the entire spot and online solid phase extraction (SPE) procedure were unaffected by the blood's HCT value within the tested range of 28.0-61.5% HCT. Enhanced stability for mephedrone on DBS compared to liquid whole blood was observed. Finger prick blood samples were collected using both volumetric sampling approaches over a time course of 25 h after intake of a single oral dose of phentermine. A pharmacokinetic curve for the incurred phentermine was successfully produced using the described validated method. These results suggest that either volumetric sample collection method may be amenable to field-use followed by fully automated, HCT-independent DBS-SPE-LC-MS/MS bioanalysis for the quantitation of these representative controlled substances. Analytical data from DBS prepared with a pipet and microfluidic-based sampling devices were comparable, but the latter is easier to operate, making this approach more suitable for sample collection by unskilled persons.

Fast determination of diphenhydramine hydrochloride in reconstitutable syrups by CWT, PLS AND PCR methods.

PubMed

Devrim, Burcu; Dinç, Erdal; Bozkir, Asuman

2014-01-01

Diphenhydramine hydrochloride (DPH), a histamine H1-receptor antagonist, is widely used as antiallergic, antiemetic and antitussive drug found in many pharmaceutical preparations. In this study, a new reconstitutable syrup formulation of DPH was prepared because it is more stable in solid form than that in liquid form. The quantitative estimation of the DPH content of a reconstitutable syrup formulation in the presence of pharmaceutical excipients, D-sorbitol, sodium citrate, sodium benzoate and sodium EDTA is not possible by the direct absorbance measurement. Therefore, a signal processing approach based on continuous wavelet transform was used to determine the DPH in the reconstitutable syrup formulations and to eliminate the effect of excipients on the analysis. The absorption spectra of DPH in the range of 5.0-40.0 μg/mL were recorded between 200-300 nm. Various wavelet families were tested and Biorthogonal1.1 continuous wavelet transform (BIOR1.1-CWT) was found to be optimal signal processing family to get fast and desirable determination results and to overcome excipient interference effects. For a comparison of the experimental results obtained by partial least squares (PLS) and principal component regression (PCR) methods were applied to the quantitative prediction of DPH in the mentioned samples. The validity of the proposed BIOR1.1-CWT, PLS and PCR methods were achieved analyzing the prepared samples containing the mentioned excipients and using standard addition technique. It was observed that the proposed graphical and numerical approaches are suitable for the quantitative analysis of DPH in samples including excipients.

Determination of As concentration in earthworm coelomic fluid extracts by total-reflection X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Allegretta, Ignazio; Porfido, Carlo; Panzarino, Onofrio; Fontanella, Maria Chiara; Beone, Gian Maria; Spagnuolo, Matteo; Terzano, Roberto

2017-04-01

Earthworms are often used as sentinel organisms to study As bioavailability in polluted soils. Arsenic in earthworms is mainly sequestrated in the coelomic fluids whose As content can therefore be used to asses As bioavalability. In this work, a method for determining As concentration in coelomic fluid extracts using total-reflection X-ray fluorescence spectrometry (TXRF) is presented. For this purpose coelomic fluid extracts from earthworms living in three polluted soils and one non-polluted (control) soil have been collected and analysed. A very simple sample preparation was implemented, consisting of a dilution of the extracts with polyvinyl alcohol (PVA) using a 1:8 ratio and dropwise deposition of the sample on the reflector. A detection limit of 0.2 μg/l and quantification limit of 0.6 μg/l was obtained in the diluted samples, corresponding to 2 μg/l and 6 μg/l in the coelomic fluid extracts, respectively. This allowed to quantify As concentration in coelomic fluids extracted from earthworms living in soils polluted with As at concentrations higher than 20 mg/kg (considered as a pollution threshold for agricultural soils). The TXRF method has been validated by comparison with As concentrations in standards and by analysing the same samples by ICP-MS, after acid digestion of the sample. The low limit of detection, the proven reliability of the method and the little sample preparation make TXRF a suitable, cost-efficient and "green" technique for the analysis of As in earthworm coelomic fluid extracts for bioavailability studies.

Investigation of the influence of vanadium, iron and nickel dopants on the morphology, and crystal structure and photocatalytic properties of titanium dioxide based nanopowders.

PubMed

Shao, Godlisten N; Jeon, Sun-Jeong; Haider, M Salman; Abbass, Nadir; Kim, Hee Taik

2016-07-15

Photoactive V, Fe and Ni doped TiO2 (M-TiO2) nanopowders were synthesized by a modified two-step sol-gel process in the absence of additives. Titanium oxychloride, which is a rarely-used TiO2 precursor was used to yield M-TiO2 photocatalysts with preferential photochemical performance in the presence of natural solar irradiation. The obtained samples were calcined at different calcination temperatures ranging from 450 to 800°C to evaluate the influence of the sintering on the physicochemical properties. The properties of the obtained samples were examined by XRF, XRD, Raman spectroscopy, UV-visible DRS, XPS, nitrogen gas physisorption studies, SEM-EDAX and HRTEM analyses. Structural characterization of the samples revealed the incorporation of these transition metal element into TiO2. It was also depicted that the morphology, crystal structure, optical and photochemical properties of the obtained samples were largely dependent on the calcination temperature and the type of dopant used during the preparation process. The photochemical performance of the samples was investigated in the photodegradation of methylene blue in the presence of natural sunlight. The experimental results indicated that the VT600 sample possessed the highest activity due to its superior properties. This study provides a systematic preparation and selection of the precursor, dopant and calcination temperature that are suitable for the formation of TiO2-based heterogeneous photocatalysts with appealing morphology, crystal structure, optical and photochemical properties for myriad of applications. Copyright © 2016 Elsevier Inc. All rights reserved.

High refractive index gold nanoparticle doped Bi2O3-B2O3 glasses for THz frequencies

NASA Astrophysics Data System (ADS)

Singla, Shivani; Achanta, Venu Gopal; Mahendru, Nancy; Prabhu, Shriganesh S.; Falconieri, Mauro; Sharma, Gopi

2017-10-01

Direct incorporation of gold nanoparticles from suspensions in 30%Bi2O3:70%B2O3 glass was achieved. This method has advantage over traditional methods where a gold salt is added to the precursor mixture and gold nanoparticles are obtained with subsequent heat treatment, eventually inducing crystallization with associated scattering of light and hence resulting in reduced optical quality of material. X-ray diffraction and differential thermal analysis were carried out in order to confirm the amorphous nature of the material and thermal properties of the prepared glasses, respectively. The size of the gold nanoparticles in the prepared glass matrix was measured using scanning electron microscopy. Optical characterization of prepared glass samples in ultraviolet-visible and terahertz regions was performed using ellipsometry, UV-VIS spectrophotometry and THz-time-domain spectroscopy. Comparison was made between glasses with and without gold nanoparticles and the effect of gold nanoparticle concentration on their optical behaviour is studied. These glasses are found to have high refractive index in the THz region making them suitable for photonic applications.

Discreet passive explosive detection through 2-sided wave guided fluorescence

DOEpatents

Harper, Ross James; la Grone, Marcus; Fisher, Mark

2012-10-16

The current invention provides a passive sampling device suitable for collecting and detecting the presence of target analytes. In particular, the passive sampling device is suitable for detecting nitro-aromatic compounds. The current invention further provides a passive sampling device reader suitable for determining the collection of target analytes. Additionally, the current invention provides methods for detecting target analytes using the passive sampling device and the passive sampling device reader.

Freezing of homogenized sputum samples for intermittent storage.

PubMed

Holz, O; Mücke, M; Zarza, P; Loppow, D; Jörres, R A; Magnussen, H

2001-08-01

Among the reasons that restrict the application of sputum induction in outpatient settings is the need for processing of samples within 2 h after induction. The aim of our study was to assess whether freezing is suitable for intermediate storage of sputum samples before processing. We compared differential cell counts between two sputum aliquots derived from the same sample. One aliquot was processed within 2 h after production and one, after it had been frozen under addition of dimethyl-sulfoxid (DMSO) and stored up to 10 days at -20 degrees C. Thirty-five samples were frozen immediately prior to preparation of cytospins, and 10 samples were frozen at an even earlier stage, directly after homogenization. In both sets of experiments we observed a significant relationship between frozen and native samples regarding macrophages, neutrophils and eosinophils, as indicated by respective intraclass correlation coefficients of 0.96, 0.96, and 0.93 in the first, and of 0.92, 0.96 and 0.77 in the second experiments. Our results indicate that the freezing of sputum samples at different stages of processing does not alter sputum morphology to an extent that affects the results of differential cell counts.

An automated multidimensional preparative gas chromatographic system for isolation and enrichment of trace amounts of xenon from ambient air.

PubMed

Larson, Tuula; Östman, Conny; Colmsjö, Anders

2011-04-01

The monitoring of radioactive xenon isotopes is one of the principal methods for the detection of nuclear explosions in order to identify clandestine nuclear testing. In this work, a miniaturized, multiple-oven, six-column, preparative gas chromatograph was constructed in order to isolate trace quantities of radioactive xenon isotopes from ambient air, utilizing nitrogen as the carrier gas. The multidimensional chromatograph comprised preparative stainless steel columns packed with molecular sieves, activated carbon, and synthetic carbon adsorbents (e.g., Anasorb®-747 and Carbosphere®). A combination of purification techniques--ambient adsorption, thermal desorption, back-flushing, thermal focusing, and heart cutting--was selectively optimized to produce a well-defined xenon peak that facilitated reproducible heart cutting and accurate quantification. The chromatographic purification of a sample requires approximately 4 h and provides complete separation of xenon from potentially interfering components (such as water vapor, methane, carbon dioxide, and radon) with recovery and accuracy close to 100%. The preparative enrichment process isolates and concentrates a highly purified xenon gas fraction that is suitable for subsequent ultra-low-level γ-, ß/γ-spectroscopic or high-resolution mass spectrometric measurement (e.g., to monitor the gaseous fission products of nuclear explosions at remote locations). The Xenon Processing Unit is a free-standing, relatively lightweight, and transportable system that can be interfaced to a variety of sampling and detection systems. It has a relatively inexpensive, rugged, and compact modular (19-inch rack) design that provides easy access to all parts for maintenance and has a low power requirement.

Liquid composition having ammonia borane and decomposing to form hydrogen and liquid reaction product

DOEpatents

Davis, Benjamin L; Rekken, Brian D

2014-04-01

Liquid compositions of ammonia borane and a suitably chosen amine borane material were prepared and subjected to conditions suitable for their thermal decomposition in a closed system that resulted in hydrogen and a liquid reaction product.

Arc-melting preparation of single crystal LaB.sub.6 cathodes

DOEpatents

Gibson, Edwin D.; Verhoeven, John D.

1977-06-21

A method for preparing single crystals of lanthanum hexaboride (LaB.sub.6) by arc melting a rod of compacted LaB.sub.6 powder. The method is especially suitable for preparing single crystal LaB.sub.6 cathodes for use in scanning electron microscopes (SEM) and scanning transmission electron microscopes (STEM).

Application of miniaturized near-infrared spectroscopy for quality control of extemporaneous orodispersible films.

PubMed

Foo, Wen Chin; Widjaja, Effendi; Khong, Yuet Mei; Gokhale, Rajeev; Chan, Sui Yung

2018-02-20

Extemporaneous oral preparations are routinely compounded in the pharmacy due to a lack of suitable formulations for special populations. Such small-scale pharmacy preparations also present an avenue for individualized pharmacotherapy. Orodispersible films (ODF) have increasingly been evaluated as a suitable dosage form for extemporaneous oral preparations. Nevertheless, as with all other extemporaneous preparations, safety and quality remain a concern. Although the United States Pharmacopeia (USP) recommends analytical testing of compounded preparations for quality assurance, pharmaceutical assays are typically not routinely performed for such non-sterile pharmacy preparations, due to the complexity and high cost of conventional assay methods such as high performance liquid chromatography (HPLC). Spectroscopic methods including Raman, infrared and near-infrared spectroscopy have been successfully applied as quality control tools in the industry. The state-of-art benchtop spectrometers used in those studies have the advantage of superior resolution and performance, but are not suitable for use in a small-scale pharmacy setting. In this study, we investigated the application of a miniaturized near infrared (NIR) spectrometer as a quality control tool for identification and quantification of drug content in extemporaneous ODFs. Miniaturized near infrared (NIR) spectroscopy is suitable for small-scale pharmacy applications in view of its small size, portability, simple user interface, rapid measurement and real-time prediction results. Nevertheless, the challenge with miniaturized NIR spectroscopy is its lower resolution compared to state-of-art benchtop equipment. We have successfully developed NIR spectroscopy calibration models for identification of ODFs containing five different drugs, and quantification of drug content in ODFs containing 2-10mg ondansetron (OND). The qualitative model for drug identification produced 100% prediction accuracy. The quantitative model to predict OND drug content in ODFs was divided into two calibrations for improved accuracy: Calibration I and II covered the 2-4mg and 4-10mg ranges respectively. Validation was performed for method accuracy, linearity and precision. In conclusion, this study demonstrates the feasibility of miniaturized NIR spectroscopy as a quality control tool for small-scale, pharmacy preparations. Due to its non-destructive nature, every dosage unit can be tested thus affording positive impact on patient safety. Copyright © 2017 Elsevier B.V. All rights reserved.

Capillary electrophoresis of inorganic anions.

PubMed

Kaniansky, D; Masár, M; Marák, J; Bodor, R

1999-02-26

This review deals with the separation mechanisms applied to the separation of inorganic anions by capillary electrophoresis (CE) techniques. It covers various CE techniques that are suitable for the separation and/or determination of inorganic anions in various matrices, including capillary zone electrophoresis, micellar electrokinetic chromatography, electrochromatography and capillary isotachophoresis. Detection and sample preparation techniques used in CE separations are also reviewed. An extensive part of this review deals with applications of CE techniques in various fields (environmental, food and plant materials, biological and biomedical, technical materials and industrial processes). Attention is paid to speciations of anions of arsenic, selenium, chromium, phosphorus, sulfur and halogen elements by CE.

ELECTRON MICROSCOPIC EXAMINATION OF SUBCELLULAR FRACTIONS

PubMed Central

Baudhuin, Pierre; Evrard, Philippe; Berthet, Jacques

1967-01-01

A method is described for preparing, by filtration on Millipore filters, very thin (about 10 µ) pellicles of packed particles. These pellicles can be embedded in Epon for electron microscopic examination. They are also suitable for cytochemical assays. The method was used with various particulate fractions from rat liver. Its main advantages over the usual centrifugal packing techniques are that it produces heterogeneity solely in the direction perpendicular to the surface of the pellicle and that sections covering the whole depth of the pellicle can be photographed in a single field. It thus answers the essential criterion of random sampling and can be used for accurate quantitative evaluations. PMID:10976209

Quantitation of Bone Growth Rate Variability in Rats Exposed to Micro-(near zero G) and Macrogravity (2G)

NASA Technical Reports Server (NTRS)

Bromage, Timothy G.; Doty, Stephen B.; Smolyar, Igor; Holton, Emily

1997-01-01

Our stated primary objective is to quantify the growth rate variability of rat lamellar bone exposed to micro- (near zero G: e.g., Cosmos 1887 & 2044; SLS-1 & SLS-2) and macrogravity (2G). The primary significance of the proposed work is that an elegant method will be established that unequivocally characterizes the morphological consequences of gravitational factors on developing bone. The integrity of this objective depends upon our successful preparation of thin sections suitable for imaging individual bone lamellae, and our imaging and quantitation of growth rate variability in populations of lamellae from individual bone samples.

Measurement of residual solvents in a drug substance by a purge-and-trap method.

PubMed

Lakatos, Miklós

2008-08-05

The purge-and-trap (P&T) gas extraction method combined with gas chromatography was studied for its suitability for quantitative residual solvents determination in a water-soluble active pharmaceutical ingredient (API). Some analytical method performance characteristics were investigated, namely, the repeatability, the accuracy and the detection limit of determination. The results show that the P&T technique is--as expected--more sensitive than the static headspace, thus it can be used for the determination of residual solvents pertaining to the ICH Class 1 group. It was found that it could be an alternative sample preparation method besides the static headspace (HS) method.

Preparation of dilute magnetic semiconductor films by metalorganic chemical vapor deposition

NASA Technical Reports Server (NTRS)

Nouhi, Akbar (Inventor); Stirn, Richard J. (Inventor)

1988-01-01

A method for preparation of a dilute magnetic semiconductor (DMS) film is provided, in which a Group II metal source, a Group VI metal source and a transition metal magnetic ion source are pyrolyzed in the reactor of a metalorganic chemical vapor deposition (MOCVD) system by contact with a heated substrate. As an example, the preparation of films of Cd(sub 1-x)Mn(sub x)Te, in which 0 is less than or equal to x less than or equal to 0.7, on suitable substrates (e.g., GaAs) is described. As a source of manganese, tricarbonyl (methylcyclopentadienyl) manganese (TCPMn) is employed. To prevent TCPMn condensation during its introduction into the reactor, the gas lines, valves and reactor tubes are heated. A thin-film solar cell of n-i-p structure, in which the i-type layer comprises a DMS, is also described; the i-type layer is suitably prepared by MOCVD.

Preparation of dilute magnetic semiconductor films by metalorganic chemical vapor deposition

NASA Technical Reports Server (NTRS)

Nouhi, Akbar (Inventor); Stirn, Richard J. (Inventor)

1990-01-01

A method for preparation of a dilute magnetic semiconductor (DMS) film is provided, wherein a Group II metal source, a Group VI metal source and a transition metal magnetic ion source are pyrolyzed in the reactor of a metalorganic chemical vapor deposition (MOCVD) system by contact with a heated substrate. As an example, the preparation of films of Cd.sub.1-x Mn.sub.x Te, wherein 0.ltoreq..times..ltoreq.0.7, on suitable substrates (e.g., GaAs) is described. As a source of manganese, tricarbonyl (methylcyclopentadienyl) maganese (TCPMn) is employed. To prevent TCPMn condensation during the introduction thereof int the reactor, the gas lines, valves and reactor tubes are heated. A thin-film solar cell of n-i-p structure, wherein the i-type layer comprises a DMS, is also described; the i-type layer is suitably prepared by MOCVD.

The Development of Lyophilized Loop-mediated Isothermal Amplification Reagents for the Detection of Coxiella burnetii.

PubMed

Chen, Hua-Wei; Ching, Wei-Mei

2016-04-18

Coxiella burnetii, the agent causing Q fever, is an obligate intracellular bacterium. PCR based diagnostic assays have been developed for detecting C. burnetii DNA in cell cultures and clinical samples. PCR requires specialized equipment and extensive end user training, and therefore, it is not suitable for routine work especially in a resource-constrained area. We have developed a loop-mediated isothermal amplification (LAMP) assay to detect the presence of C. burnetii in patient samples. This method is performed at a single temperature around 60 °C in a water bath or heating block. The sensitivity of this LAMP assay is very similar to PCR with a detection limit of about 25 copies per reaction. This report describes the preparation of the reaction using lyophilized reagents and visualization of results using hydroxynaphthol blue (HNB) or a UV lamp with fluorescent intercalating dye in the reaction. The LAMP reagents were lyophilized and stored at room temperature (RT) for one month without loss of detection sensitivity. This LAMP assay is particularly robust because the reaction mixture preparation does not involve complex steps. This method is ideal for use in resource-limited settings where Q fever is endemic.

Assessment and mapping of water pollution indices in zone-III of municipal corporation of hyderabad using remote sensing and geographic information system.

PubMed

Asadi, S S; Vuppala, Padmaja; Reddy, M Anji

2005-01-01

A preliminary survey of area under Zone-III of MCH was undertaken to assess the ground water quality, demonstrate its spatial distribution and correlate with the land use patterns using advance techniques of remote sensing and geographical information system (GIS). Twenty-seven ground water samples were collected and their chemical analysis was done to form the attribute database. Water quality index was calculated from the measured parameters, based on which the study area was classified into five groups with respect to suitability of water for drinking purpose. Thematic maps viz., base map, road network, drainage and land use/land cover were prepared from IRS ID PAN + LISS III merged satellite imagery forming the spatial database. Attribute database was integrated with spatial sampling locations map in Arc/Info and maps showing spatial distribution of water quality parameters were prepared in Arc View. Results indicated that high concentrations of total dissolved solids (TDS), nitrates, fluorides and total hardness were observed in few industrial and densely populated areas indicating deteriorated water quality while the other areas exhibited moderate to good water quality.

Size-exclusion chromatography of perfluorosulfonated ionomers.

PubMed

Mourey, T H; Slater, L A; Galipo, R C; Koestner, R J

2011-08-26

A size-exclusion chromatography (SEC) method in N,N-dimethylformamide containing 0.1 M LiNO(3) is shown to be suitable for the determination of molar mass distributions of three classes of perfluorosulfonated ionomers, including Nafion(®). Autoclaving sample preparation is optimized to prepare molecular solutions free of aggregates, and a solvent exchange method concentrates the autoclaved samples to enable the use of molar-mass-sensitive detection. Calibration curves obtained from light scattering and viscometry detection suggest minor variation in the specific refractive index increment across the molecular size distributions, which introduces inaccuracies in the calculation of local absolute molar masses and intrinsic viscosities. Conformation plots that combine apparent molar masses from light scattering detection with apparent intrinsic viscosities from viscometry detection partially compensate for the variations in refractive index increment. The conformation plots are consistent with compact polymer conformations, and they provide Mark-Houwink-Sakurada constants that can be used to calculate molar mass distributions without molar-mass-sensitive detection. Unperturbed dimensions and characteristic ratios calculated from viscosity-molar mass relationships indicate unusually free rotation of the perfluoroalkane backbones and may suggest limitations to applying two-parameter excluded volume theories for these ionomers. Copyright © 2011 Elsevier B.V. All rights reserved.

Synthesis and analysis of acou-physical properties of banana biocomposite

NASA Astrophysics Data System (ADS)

Mishra, S. P.; Bhanupriya; Nath, G.

2018-02-01

The sound absorbing materials have been developed using various natural fibres which are renewable, biodegradable, recyclable and economic in nature. After the cultivation of banana fruit as its stem which is fibrous in nature has no use, it may use in various scientific applications as like as the preparation of sound absorbing materials. The suitable and proper mixture of the epoxy resin with the banana fibre gives rise to formation of the biocomposite material which is mechanically firm and tough. The EDS and SEM analysis of the sample gives an idea about the formation of closed chain in between banana fibre and epoxy in the molecular level and porous quality. The thermal conductivity gradually decreases with the increase of particle concentration and the electrical conductivity increases in the order of 10-5 which demonstrates the insulating behaviour of the prepared sample. At the higher frequencies there is a reduction of dielectric constant due to the interfacial and orientation polarisation. The intensity of sound decreases in presence of the material and the absorption coefficient rise with increase of frequency. Thus the banana fibre biocomposite material can be used as a sound absorber which behaves as thermally and electrically insulator.

Size-dependent photocatalytic activity of La0.8Sr0.2MnO3 nanoparticles prepared by hydrothermal synthesis

NASA Astrophysics Data System (ADS)

Rahmani Afje, F.; Ehsani, M. H.

2018-04-01

Synthesize of La0.8Sr0.2MnO3 (LSMO) manganite were carried out in different particle sizes by hydrothermal method. Structural and optical properties of the prepared specimens were studied by x-ray diffraction (XRD), Fourier transform infra-red (FT-IR) spectroscopy, field emission scanning electron microscopy (FESEM), and UV–vis spectroscopy. The XRD study, coupled with the Rietveld refinement, exhibited rhombohedral structure with R-3C space group. Using the FT-IR and FESEM analyses, the perovskite structure of the samples with Nano-rod-like morphologies were inferred. Furthermore, the average sizes of 48.11, 70.99 and 111.45 nm were obtained for the ones sintered at 800, 900, and 1000 °C temperatures, respectively. The optical research showed that band gap energy is about 2.13 eV, being suitable in visible-light photocatalytic activity for water purification from dyes and toxic organic materials. The photo-degradation efficiency for decolorizing methyl orange solution (10 ppm) for various samples (100 ppm) were systematically probed and a strong relation is concluded between particle size and photocatalytic activity.

Optimisation and validation of a rapid and efficient microemulsion liquid chromatographic (MELC) method for the determination of paracetamol (acetaminophen) content in a suppository formulation.

PubMed

McEvoy, Eamon; Donegan, Sheila; Power, Joe; Altria, Kevin

2007-05-09

A rapid and efficient oil-in-water microemulsion liquid chromatographic method has been optimised and validated for the analysis of paracetamol in a suppository formulation. Excellent linearity, accuracy, precision and assay results were obtained. Lengthy sample pre-treatment/extraction procedures were eliminated due to the solubilising power of the microemulsion and rapid analysis times were achieved. The method was optimised to achieve rapid analysis time and relatively high peak efficiencies. A standard microemulsion composition of 33 g SDS, 66 g butan-1-ol, 8 g n-octane in 1l of 0.05% TFA modified with acetonitrile has been shown to be suitable for the rapid analysis of paracetamol in highly hydrophobic preparations under isocratic conditions. Validated assay results and overall analysis time of the optimised method was compared to British Pharmacopoeia reference methods. Sample preparation and analysis times for the MELC analysis of paracetamol in a suppository were extremely rapid compared to the reference method and similar assay results were achieved. A gradient MELC method using the same microemulsion has been optimised for the resolution of paracetamol and five of its related substances in approximately 7 min.

Influence of composition of diluent on populations of yeasts and moulds recovered from raw fruits.

PubMed

Beuchat, L R; Scouten, A J; Jablonska, J

2002-01-01

The aims of this study were (i) to determine the retention of viability of mycoflora removed from raw fruits, and how this affected diluents used to prepare samples for enumeration of propagules, and (ii) to evaluate the performance of recovery media for supporting colony development. Yeasts and moulds removed from seven types of raw fruit were held in seven diluents for 1 h before plating on dichloran rose bengal chloramphenicol (DRBC) agar and plate count agar supplemented with chloramphenicol (100 micro g ml-1) (PCAC). Significant reductions (P=0.05) in populations of yeasts, moulds, and yeasts plus moulds occurred within the 1 h holding period, regardless of diluent composition. Overall, retention of viability was not influenced by diluent composition, and neither DRBC agar nor PCAC were superior in supporting colony development. The composition of diluents used to prepare food samples for mycological analysis has little affect on the number of yeasts and moulds recovered from seven types of naturally contaminated raw fruit. Both DRBC agar and PCAC are suitable as enumeration media. Diluents and media most often recommended for enumerating yeasts and moulds in foods are appropriate for raw fruits.

Preparation of Chloramphenicol/Amino Acid Combinations Exhibiting Enhanced Dissolution Rates and Reduced Drug-Induced Oxidative Stress.

PubMed

Sterren, Vanesa B; Aiassa, Virginia; Garnero, Claudia; Linck, Yamila Garro; Chattah, Ana K; Monti, Gustavo A; Longhi, Marcela R; Zoppi, Ariana

2017-11-01

Chloramphenicol is an old antibiotic agent that is re-emerging as a valuable alternative for the treatment of multidrug-resistant pathogens. However, it exhibits suboptimal biopharmaceutical properties and toxicity profiles. In this work, chloramphenicol was combined with essential amino acids (arginine, cysteine, glycine, and leucine) with the aim of improving its dissolution rate and reduce its toxicity towards leukocytes. The chloramphenicol/amino acid solid samples were prepared by freeze-drying method and characterized in the solid state by using Fourier transform infrared spectroscopy, powder X-ray diffraction, differential scanning calorimetry, scanning electron microscopy, and solid-state nuclear magnetic resonance. The dissolution properties, antimicrobial activity, reactive oxygen species production, and stability of the different samples were studied. The dissolution rate of all combinations was significantly increased in comparison to that of the pure active pharmaceutical ingredient. Additionally, oxidative stress production in human leukocytes caused by chloramphenicol was decreased in the chloramphenicol/amino acid combinations, while the antimicrobial activity of the antibiotic was maintained. The CAP:Leu binary combination resulted in the most outstanding solid system makes it suitable candidate for the development of pharmaceutical formulations of this antimicrobial agent with an improved safety profile.

Novel micro-extraction by packed sorbent procedure for the liquid chromatographic analysis of antiepileptic drugs in human plasma and urine.

PubMed

Rani, Susheela; Malik, Ashok K; Singh, Baldev

2012-02-01

A method for the simultaneous determination of the antiepileptic drugs, phenobarbital (PHB), phenytoin (PTN), carbamazepine (CBZ), primidone (PRM) and oxcarbazepine (OXC) in human plasma and urine samples by using micro-extraction in a packed syringe as the sample preparation method connected with LC/UV (MEPS/LC/UV) is described. Micro-extraction in a packed syringe (MEPS) is a new miniaturized, solid-phase extraction technique that can be connected online to gas or liquid chromatography without any modifications. In MEPS approximately 1 mg of the solid packing material is inserted into a syringe (100-250 μL) as a plug. Sample preparation takes place on the packed bed. The bed can be coated to provide selective and suitable sampling conditions. The new method is very promising, easy to use, fully automated, inexpensive and quick. The standard curves were obtained within the concentration range 1-500 ng/mL in both plasma and urine samples. The results showed high correlation coefficients (R(2) >0.988) for all of the analytes within the calibration range. The extraction recovery was found to be between 88.56 and 99.38%. The limit of quantification was found to be between 0.132 and 1.956 ng/mL. The precision (RSD) values of quality control samples (QC) had a maximum deviation of 4.9%. A comparison of the detection limits with similar methods indicates high sensitivity of the present method. The method is applied for the analysis of these drugs in real urine and plasma samples of epileptic patients. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Simultaneous determination of three anticonvulsants using hydrophilic interaction LC-MS.

PubMed

Oertel, Reinhard; Arenz, Norman; Pietsch, Jörg; Kirch, Wilhelm

2009-01-01

A specific and automated method was developed to quantify the anticonvulsants gabapentin, pregabalin and vigabatrin simultaneously in human serum. Samples were prepared with a protein precipitation. The hydrophilic interaction chromatography (HILIC) with a mobile phase gradient was used to divide off ions of the matrix and for separation of the analytes. Four different HILIC-columns and two different column temperatures were tested. The Tosoh-Amid column gave the best results: single small peaks. The anticonvulsants were detected in the multiple reaction monitoring mode (MRM) with ESI-MS-MS. Using a volume of 100 microL biological sample the lowest point of the standard curve, i.e. the lower LOQs were 312 ng/mL. The described HILIC-MS-MS method is suitable for therapeutic drug monitoring and for clinical and pharmcokinetical investigations of the anticonvulsives.

Soft ferromagnetic properties of Ni44Fe6Mn32Al18 doped Co partially

NASA Astrophysics Data System (ADS)

Notonegoro, Hamdan Akbar; Kurniawan, Budhy; Kurniawan, Candra; Manaf, Azwar

2017-01-01

Research in finding suitable magnetocaloric material around room temperature made ferromagnetic (FM) (Ni-Mn)-based Heusler alloys receive considerable attention as a potential candidate for the magnetic refrigerator. This compound are associated with the shape-memory effect, magnetic superelasticity, and more others magneto-functional properties. The compounds were prepared by vacuum arc melter (VAM) under argon atmosphere which sintering and annealing process were running with quartz cube in vacuum condition. A small amount of coercivity value at σ = 0 in the hysteresis curve occurred whereas magnetization of the sample in various temperature does not reach saturation. The Currie temperature Tc of the sample was obtained at 358 K. Nevertheless, this is dubious value because at T = 300 K the curves had swooped down. Additional measurements necessary to taken as a comparison to verify this value.

Simultaneous quantification of acetaminophen and five acetaminophen metabolites in human plasma and urine by high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry: Method validation and application to a neonatal pharmacokinetic study.

PubMed

Cook, Sarah F; King, Amber D; van den Anker, John N; Wilkins, Diana G

2015-12-15

Drug metabolism plays a key role in acetaminophen (paracetamol)-induced hepatotoxicity, and quantification of acetaminophen metabolites provides critical information about factors influencing susceptibility to acetaminophen-induced hepatotoxicity in clinical and experimental settings. The aims of this study were to develop, validate, and apply high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) methods for simultaneous quantification of acetaminophen, acetaminophen-glucuronide, acetaminophen-sulfate, acetaminophen-glutathione, acetaminophen-cysteine, and acetaminophen-N-acetylcysteine in small volumes of human plasma and urine. In the reported procedures, acetaminophen-d4 and acetaminophen-d3-sulfate were utilized as internal standards (IS). Analytes and IS were recovered from human plasma (10μL) by protein precipitation with acetonitrile. Human urine (10μL) was prepared by fortification with IS followed only by sample dilution. Calibration concentration ranges were tailored to literature values for each analyte in each biological matrix. Prepared samples from plasma and urine were analyzed under the same HPLC-ESI-MS/MS conditions, and chromatographic separation was achieved through use of an Agilent Poroshell 120 EC-C18 column with a 20-min run time per injected sample. The analytes could be accurately and precisely quantified over 2.0-3.5 orders of magnitude. Across both matrices, mean intra- and inter-assay accuracies ranged from 85% to 112%, and intra- and inter-assay imprecision did not exceed 15%. Validation experiments included tests for specificity, recovery and ionization efficiency, inter-individual variability in matrix effects, stock solution stability, and sample stability under a variety of storage and handling conditions (room temperature, freezer, freeze-thaw, and post-preparative). The utility and suitability of the reported procedures were illustrated by analysis of pharmacokinetic samples collected from neonates receiving intravenous acetaminophen. Copyright © 2015 Elsevier B.V. All rights reserved.

Method of preparation of uranium nitride

DOEpatents

Kiplinger, Jaqueline Loetsch; Thomson, Robert Kenneth James

2013-07-09

Method for producing terminal uranium nitride complexes comprising providing a suitable starting material comprising uranium; oxidizing the starting material with a suitable oxidant to produce one or more uranium(IV)-azide complexes; and, sufficiently irradiating the uranium(IV)-azide complexes to produce the terminal uranium nitride complexes.

Mucoadhesive in situ gel formulation for vaginal delivery of clotrimazole: formulation, preparation, and in vitro/in vivo evaluation.

PubMed

Rençber, Seda; Karavana, Sinem Yaprak; Şenyiğit, Zeynep Ay; Eraç, Bayri; Limoncu, Mine Hoşgör; Baloğlu, Esra

2017-06-01

The purpose of this study was to develop a suitable mucoadhesive in situ gel formulation of clotrimazole (CLO) for the treatment of vaginal candidiasis. For this aim, the mixture of poloxamer (PLX) 407 and 188 were used to prepare in situ gels. Hydroxypropyl methylcellulose (HPMC) K100M or E50 was added to in situ gels in 0.5% ratio to improve the mucoadhesive and mechanical properties of formulations and to prolong the residence time in vaginal cavity. After the preparation of mucoadhesive in situ gels; gelation temperature/time, viscosity, mechanical, mucoadhesive, syringeability, spreadibility and rheological properties, in vitro release behavior, and anticandidal activities were determined. Moreover vaginal retention of mucoadhesive in situ gels was investigated with in vivo distribution studies in rats. Based on the obtained results, it was found that gels prepared with 20% PLX 407, 10% PLX 188 and 0.5% HPMC K100M/E50 might be suitable for vaginal administration of CLO. In addition, the results of in vivo distribution studies showed that gel formulations remained on the vaginal mucosa even 24 h after application. In conclusion, the mucoadhesive in situ gels of CLO would be alternative candidate for treatment of vaginal candidiasis since it has suitable gel properties with good vaginal retention.

Foamed oligo(poly(ethylene glycol)fumarate) hydrogels as versatile prefabricated scaffolds for tissue engineering.

PubMed

Henke, Matthias; Baumer, Julia; Blunk, Torsten; Tessmar, Joerg

2014-03-01

Radically cross-linked hydrogels are frequently used as cell carriers due to their excellent biocompatibility and their tissue-like mechanical properties. Through frequent investigation, PEG-based polymers such as oligo(poly(ethylene glycol)fumarate [OPF] have proven to be especially suitable as cell carriers by encapsulating cells during hydrogel formation. In some cases, NaCl or biodegradable gelatin microparticles were added prior to cross-linking in order to provide space for the proliferating cells, which would otherwise stay embedded in the hydrogel matrix. However, all of these immediate cross-linking procedures involve time consuming sample preparation and sterilization directly before cell culture and often show notable swelling after their preparation. In this study, ready to use OPF-hydrogel scaffolds were prepared by gas foaming, freeze drying, individual packing into bags and subsequent γ-sterilization. The scaffolds could be stored and used "off-the-shelf" without any need for further processing prior to cell culture. Thus the handling was simplified and the sterility of the cell carrier was assured. Further improvement of the gel system was achieved using a two component injectable system, which may be used for homogenous injection molding in order to create individually shaped three dimensional scaffolds. In order to evaluate the suitability of the scaffolds for tissue engineering, constructs were seeded with juvenile bovine chondrocytes and cultured for 28 days. Cross-sections of the respective constructs showed an intense and homogenous red staining of GAG with safranin O, indicating a homogenous cell distribution within the scaffolds and the production of substantial amounts of GAG-rich matrix. Copyright © 2012 John Wiley & Sons, Ltd.

Vortex-assisted emulsification semimicroextraction for the analytical control of restricted ingredients in cosmetic products: determination of bronopol by liquid chromatography.

PubMed

Miralles, Pablo; Bellver, Raquel; Chisvert, Alberto; Salvador, Amparo

2016-03-01

Vortex-assisted emulsification semimicroextraction is proposed as a one-step solution-extraction procedure for sample preparation in cosmetic products. The procedure allows rapid preparation based on dispersion of the sample in a mixture of 1 mL of n-hexane and 0.5 mL of ethanol, followed by the addition of 0.5 mL of water and centrifugation to obtain two separated phases. This procedure provides good sample clean-up with minimum dilution and is very useful for the determination of ingredients with restricted concentrations, such as bronopol. The procedure was applied to the determination of bronopol by liquid chromatography with UV detection. The best chromatographic separation was obtained by using a C18 column set at 40 °C and performing a stepwise elution with a mixture of ethanol/aqueous 1 % acetic acid solution as mobile phase pumped at 0.5 mL min(-1). The detection wavelength was set at 250 nm and the total run time required was 12 min. The method was successfully applied to 18 commercial cosmetic samples including creams, shampoos, and bath gels. Good recoveries and repeatability were obtained, with a limit of detection of 0.9 μg mL(-1), which makes the method suitable for the analytical control of cosmetic products. Moreover, it could be considered environmentally friendly, because water, ethanol, and only a low volume of n-hexane are used as solvents.

Quantitative determination of n-propane, iso-butane, and n-butane by headspace GC-MS in intoxications by inhalation of lighter fluid.

PubMed

Bouche, Marie-Paule L A; Lambert, Willy E; Van Bocxlaer, Jan F P; Piette, Michel H; De Leenheer, André P

2002-01-01

This report describes a fully elaborated and validated method for quantitation of the hydrocarbons n-propane, iso-butane, and n-butane in blood samples. The newly developed analytical procedure is suitable for both emergency cases and forensic medicine investigations. Its practical applicability is illustrated with a forensic blood sample after acute inhalative intoxication with lighter fluid; case history and toxicological findings are included. Identification and quantitation of the analytes were performed using static headspace extraction combined with gas chromatography-mass spectrometry. In order to reconcile the large gas volumes injected (0.5 mL) with the narrowbore capillary column and thus achieve preconcentration, cold trapping on a Tenax sorbent followed by flash desorption was applied. Adequate retention and separation were achieved isothermally at 35 degrees C on a thick-film capillary column. Sample preparation was kept to a strict minimum and involved simply adding 2.5 microL of a liquid solution of 1,1,2-trichlorotrifluoroethane in t-butyl-methylether as an internal standard to aliquots of blood in a capped vial. Standards were created by volumetric dilution departing from a gravimetrically prepared calibration gas mixture composed of 0.3% of n-propane, 0.7% of iso-butane, and 0.8% of n-butane in nitrogen. In the forensic blood sample, the following concentrations were measured: 90.0 microg/L for n-propane, 246 microg/L for iso-butane, and 846 microg/L for n-butane.

Using tobacco plants as biomonitors of contaminated norm areas.

PubMed

Máté, B; Horváth, M; Somlai, J; Kovács, T

2013-03-01

One of the largest biomonitoring tasks is the assessing and environment monitoring of radiological wastes produced by mining. Po-210 and Pb-210 are easy to mobilise even in a weak acidic medium and as we know the biological behaviour and accumulation capacity of tobacco, this could be a suitable option for biomonitoring. During our work the Pb-210 and Po-210 concentration values of tobacco parts and soil samples originating from a Hungarian remediated uranium mine site were determined. The source preparation was spontaneous deposition following combined acidic leaching with a Po-209 tracer; the detection was carried out with a semiconductor ('PIPS') detector alpha-spectrometer. According to the results for the tobacco plant parts and soil samples, secular equilibrium could be found between the Pb-210 and Po-210 isotopes, and the isotope content of the lower leaves of the tobacco plants was in correlation with the isotope concentration of the soil; therefore, the measurement of the activity concentration is suitable for tracing smaller levels of washing out. The Po-210 activity concentration values of tobacco (average: 15.5 ± 3.6 Bq kg(-1)) and soil (average: 60.1 ± 15.2 Bq kg(-1)) samples originating from the area investigated compared with samples from another part of Hungary, Balatonalmádi (tobacco: 12.5 ± 1.0 Bq kg(-1), soil: 57.0 ± 4.7 Bq kg(-1)), do not show significant radionuclide migration.

Spectro-photometric determinations of Mn, Fe and Cu in aluminum master alloys

NASA Astrophysics Data System (ADS)

Rehan; Naveed, A.; Shan, A.; Afzal, M.; Saleem, J.; Noshad, M. A.

2016-08-01

Highly reliable, fast and cost effective Spectro-photometric methods have been developed for the determination of Mn, Fe & Cu in aluminum master alloys, based on the development of calibration curves being prepared via laboratory standards. The calibration curves are designed so as to induce maximum sensitivity and minimum instrumental error (Mn 1mg/100ml-2mg/100ml, Fe 0.01mg/100ml-0.2mg/100ml and Cu 2mg/100ml-10mg/ 100ml). The developed Spectro-photometric methods produce accurate results while analyzing Mn, Fe and Cu in certified reference materials. Particularly, these methods are suitable for all types of Al-Mn, Al-Fe and Al-Cu master alloys (5%, 10%, 50% etc. master alloys).Moreover, the sampling practices suggested herein include a reasonable amount of analytical sample, which truly represent the whole lot of a particular master alloy. Successive dilution technique was utilized to meet the calibration curve range. Furthermore, the workout methods were also found suitable for the analysis of said elements in ordinary aluminum alloys. However, it was observed that Cush owed a considerable interference with Fe, the later one may not be accurately measured in the presence of Cu greater than 0.01 %.

Analysis of anabolic androgenic steroids as sulfate conjugates using high performance liquid chromatography coupled to tandem mass spectrometry.

PubMed

Rzeppa, S; Heinrich, G; Hemmersbach, P

2015-01-01

Improvements in doping analysis can be effected by speeding up analysis time and extending the detection time. Therefore, direct detection of phase II conjugates of doping agents, especially anabolic androgenic steroids (AAS), is proposed. Besides direct detection of conjugates with glucuronic acid, the analysis of sulfate conjugates, which are usually not part of the routine doping control analysis, can be of high interest. Sulfate conjugates of methandienone and methyltestosterone metabolites have already been identified as long-term metabolites. This study presents the synthesis of sulfate conjugates of six commonly used AAS and their metabolites: trenbolone, nandrolone, boldenone, methenolone, mesterolone, and drostanolone. In the following these sulfate conjugates were used for development of a fast and easy analysis method based on sample preparation using solid phase extraction with a mixed-mode sorbent and detection by high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). Validation demonstrated the suitability of the method with regard to the criteria given by the technical documents of the World Anti-Doping Agency (WADA). In addition, suitability has been proven by successful detection of the synthesized sulfate conjugates in excretion urines and routine doping control samples. Copyright © 2015 John Wiley & Sons, Ltd.

Outsourcing cytological samples to a referral laboratory for EGFR testing in non-small cell lung cancer: does theory meet practice?

PubMed

Vigliar, E; Malapelle, U; Bellevicine, C; de Luca, C; Troncone, G

2015-10-01

Guidelines from the College of American Pathologists (CAP), the International Association for the Study of Lung Cancer (IASLC) and the Association for Molecular Pathology (AMP) consider cytology suitable for testing epidermal growth factor receptor (EGFR) mutations in lung adenocarcinoma. The guidelines recommend that cytopathologists first discuss the possibility of testing squamous cell carcinomas (SqCC) in multidisciplinary meetings. Second, cell blocks should be analysed rather than smear preparations and, third, specimens should be sent to external molecular laboratories within three working days of receiving requests. This study monitored how these recommendations are met in practice. Our laboratory received 596 requests from cytologists from 13 different institutions. For each case, the cytological diagnosis, cytopreparation type, and time between the request and sample mailing were compared with the recommendations. Of the 596 samples, 32 (5.4%) had been reported as SqCC. Three of these (9.4%) showed EGFR mutation. Cytological slides, either ThinPrep(™) (51.2%) or direct smears (43.2%), were more frequently received than cell blocks (5.7%). The mean time between the oncologist's request and specimen dispatching was 5.8 working days. The occurrence of mutations in samples reported as SqCC was higher than expected. This questions the reliability of the original diagnosis, which reinforced the recommendation to evaluate the opportunity for testing non-adenocarcinoma cytology on a case-by-case basis. In spite of CAP/IASLC/AMP recommendations, cell blocks were underutilized for EGFR testing, but cytological slides were suitable for DNA analyses. Significant efforts are needed to avoid delays in outsourcing cytological samples for EGFR testing. © 2014 John Wiley & Sons Ltd.

Process for the synthesis of iron powder

DOEpatents

Not Available

1982-03-06

A process for preparing iron powder suitable for use in preparing the iron-potassium perchlorate heat-powder fuel mixture used in thermal batteries, comprises preparing a homogeneous, dense iron oxide hydroxide precipitate by homogeneous precipitation from an aqueous mixture of a ferric salt, formic or sulfuric acid, ammonium hydroxide and urea as precipitating agent; and then reducing the dense iron oxide hydroxide by treatment with hydrogen to prepare the iron powder.

Process for the synthesis of iron powder

DOEpatents

Welbon, William W.

1983-01-01

A process for preparing iron powder suitable for use in preparing the iron-potassium perchlorate heat-powder fuel mixture used in thermal batteries, comprises preparing a homogeneous, dense iron oxide hydroxide precipitate by homogeneous precipitation from an aqueous mixture of a ferric salt, formic or sulfuric acid, ammonium hydroxide and urea as precipitating agent; and then reducing the dense iron oxide hydroxide by treatment with hydrogen to prepare the iron powder.

Preparation of four 1,4-dihydropyridine derivatives (DHPs) labeled with carbon-14.

PubMed

Ahmadi Faghih, Mohammad Amin; Moslemin, Mohammad Hossein; Shirvani, Gholamhossein; Javaheri, Mohsen

2018-05-23

The importance of DHPs compounds and the need for examining the mechanism of their effect, mandated us to synthesize a number of carbon-14 labeled 1,4-dihydropyridine derivatives for pharmacological studies. Simple preparation and suitable radiochemical yield were advantages of this preparation. This article is protected by copyright. All rights reserved.

Comparative evaluation of the Cobas Amplicor HIV-1 Monitor Ultrasensitive Test, the new Cobas AmpliPrep/Cobas Amplicor HIV-1 Monitor Ultrasensitive Test and the Versant HIV RNA 3.0 assays for quantitation of HIV-1 RNA in plasma samples.

PubMed

Berger, Annemarie; Scherzed, Lina; Stürmer, Martin; Preiser, Wolfgang; Doerr, Hans Wilhelm; Rabenau, Holger Felix

2005-05-01

There are several commercially available assays for the quantitation of HIV RNA. A new automated specimen preparation system, the Cobas AmpliPrep, was developed to automate this last part of the PCR. We compared the results obtained by the Roche Cobas Amplicor HIV-1 Monitor Ultrasensitive Test (MCA, manual sample preparation) with those by the Versant HIV-1 RNA 3.0 assay (bDNA). Secondly we compared the MCA with the new Cobas AmpliPrep/Cobas Amplicor HIV Monitor Ultrasensitive Test (CAP/CA, automated specimen preparation) by investigating clinical patient samples and a panel of HIV-1 non-B subtypes. Furthermore, we assessed the assay throughput and workflow (especially hands-on time) for all three assays. Seventy-two percent of the 140 investigated patient samples gave concordant results in the bDNA and MCA assays. The MCA values were regularly higher than the bDNA values. One sample was detected only by the MCA within the linear range of quantification. In contrast, 38 samples with results <50 copies/ml in the MCA showed in the bDNA results between 51 and 1644 copies/ml (mean value 74 copies/ml); 21 of these specimens were shown to have detectable HIV RNA < 50 copies/ml in the MCA assay. The overall agreement between the MCA and the CAP/CA was 94.3% (551/584). The quantification results showed significant correlation, although the CAP/CA generated values slightly lower than those generated by the manual procedure. We found that the CAP/CA produced comparable results with the MCA test in a panel of HIV-1 non-B subtypes. All three assays showed comparable results. The bDNA provides a high sample throughput without the need of full automation. The new CAP/CA provides reliable test results with no HIV-subtype specific influence and releases time for other works in the laboratory; thus it is suitable for routine diagnostic PCR.

Preparation of l-phenylalanine-imprinted solid-phase extraction sorbent by Pickering emulsion polymerization and the selective enrichment of l-phenylalanine from human urine.

PubMed

Li, Ji; Hu, Xiaoling; Guan, Ping; Zhang, Xiaoyan; Qian, Liwei; Zhang, Nan; Du, Chunbao; Song, Renyuan

2016-05-01

A novel l-phenylalanine molecularly imprinted solid-phase extraction sorbent was synthesized by the combination of Pickering emulsion polymerization and ion-pair dummy template imprinting. Compared to other polymerization methods, the molecularly imprinted polymers thus prepared exhibit a high specific surface, large pore diameter, and appropriate particle size. The key parameters for solid-phase extraction were optimized, and the result indicated that the molecularly imprinted polymer thus prepared exhibits a good recovery of 98.9% for l-phenylalanine. Under the optimized conditions of the procedure, an analytical method for l-phenylalanine was well established. By comparing the performance of the molecularly imprinted polymer and a commercial reverse-phase silica gel, the obtained molecularly imprinted polymer as an solid-phase extraction sorbent is more suitable, exhibiting high precision (relative standard deviation 3.2%, n = 4) and a low limit of detection (60.0 ± 1.9 nmol·L(-1) ) for the isolation of l-phenylalanine. Based on these results, the combination of the Pickering emulsion polymerization and ion-pair dummy template imprinting is effective for preparing selective solid-phase extraction sorbents for the separation of amino acids and organic acids from complex biological samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Isoelectric focusing of small non-covalent metal species from plants.

PubMed

Köster, Jessica; Hayen, Heiko; von Wirén, Nicolaus; Weber, Günther

2011-03-01

IEF is known as a powerful electrophoretic separation technique for amphoteric molecules, in particular for proteins. The objective of the present work is to prove the suitability of IEF also for the separation of small, non-covalent metal species. Investigations are performed with copper-glutathione complexes, with the synthetic ligand ethylenediamine-N,N'-bis(o-hydroxyphenyl)acetic acid (EDDHA) and respective metal complexes (Fe, Ga, Al, Ni, Zn), and with the phytosiderophore 2'-deoxymugineic acid (DMA) and its ferric complex. It is shown that ethylenediamine-N,N'-bis(o-hydroxyphenyl)acetic acid and DMA species are stable during preparative scale IEF, whereas copper-glutathione dissociates considerably. It is also shown that preparative scale IEF can be applied successfully to isolate ferric DMA from real plant samples, and that multidimensional separations are possible by combining preparative scale IEF with subsequent HPLC-MS analysis. Focusing of free ligands and respective metal complexes with di- and trivalent metals results in different pIs, but CIEF is usually needed for a reliable estimation of pI values. Limitations of the proposed methods (preparative IEF and CIEF) and consequences of the results with respect to metal speciation in plants are discussed. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Detection of Cytomegalovirus (CMV) DNA in EDTA Whole-Blood Samples: Evaluation of the Quantitative artus CMV LightCycler PCR Kit in Conjunction with Automated Sample Preparation▿

PubMed Central

Michelin, Birgit D. A.; Hadžisejdić, Ita; Bozic, Michael; Grahovac, Maja; Hess, Markus; Grahovac, Blaženka; Marth, Egon; Kessler, Harald H.

2008-01-01

Whole blood has been found to be a reliable matrix for the detection and quantitation of cytomegalovirus (CMV) DNA. In this study, the performance of the artus CMV LightCycler (LC) PCR kit in conjunction with automated sample preparation on a BioRobot EZ1 workstation was evaluated. The accuracy, linearity, analytical sensitivity, and inter- and intra-assay variations were determined. A total of 102 clinical EDTA whole-blood samples were investigated, and results were compared with those obtained with the in vitro diagnostics (IVD)/Conformité Européene (CE)-labeled CMV HHV6,7,8 R-gene quantification kit. When the accuracy of the new kit was tested, seven of eight results were found to be within ±0.5 log10 unit of the expected panel results. Determination of linearity resulted in a quasilinear curve over more than 5 log units. The lower limit of detection of the assay was determined to be 139 copies/ml in EDTA whole blood. The interassay variation ranged from 15 to 58%, and the intra-assay variation ranged from 7 to 35%. When clinical samples were tested and the results were compared with those of the routinely used IVD/CE-labeled assay, 53 samples tested positive and 13 samples tested negative by both of the assays. One sample was found to be positive with the artus CMV LC PCR kit only, and 35 samples tested positive with the routinely used assay only. The majority of discrepant results were found with low-titer samples. In conclusion, use of the artus CMV LC PCR kit in conjunction with automated sample preparation on the BioRobot EZ1 workstation may be suitable for the detection and quantitation of CMV DNA in EDTA whole blood in the routine low-throughput laboratory; however, low-positive results may be missed by this assay. PMID:18272703

Automated saliva processing for LC-MS/MS: Improving laboratory efficiency in cortisol and cortisone testing.

PubMed

Antonelli, Giorgia; Padoan, Andrea; Artusi, Carlo; Marinova, Mariela; Zaninotto, Martina; Plebani, Mario

2016-04-01

The aim of this study was to implement in our routine practice an automated saliva preparation protocol for quantification of cortisol (F) and cortisone (E) by LC-MS/MS using a liquid handling platform, maintaining the previously defined reference intervals with the manual preparation. Addition of internal standard solution to saliva samples and calibrators and SPE on μ-elution 96-well plate were performed by liquid handling platform. After extraction, the eluates were submitted to LC-MS/MS analysis. The manual steps within the entire process were to transfer saliva samples in suitable tubes, to put the cap mat and transfer of the collection plate to the LC auto sampler. Transference of the reference intervals from the manual to the automated procedure was established by Passing Bablok regression on 120 saliva samples analyzed simultaneously with the two procedures. Calibration curves were linear throughout the selected ranges. The imprecision ranged from 2 to 10%, with recoveries from 95 to 116%. Passing Bablok regression demonstrated no significant bias. The liquid handling platform translates the manual steps into automated operations allowing for saving hands-on time, while maintaining assay reproducibility and ensuring reliability of results, making it implementable in our routine with the previous established reference intervals. Copyright © 2015 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Structural morphology of zinc oxide structures with antibacterial application of calamine lotion

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

Ann, Ling Chuo; Mahmud, Shahrom; Bakhori, Siti Khadijah Mohd

In this study, we report the structural morphology of a zinc oxide (ZnO) sample and antibacterial application of the ZnO structures in calamine lotion. Antibacterial activities of the calamine lotion towards Staphylococcus aureus and Pseudomonas aeruginosa were investigated. The structural morphology of ZnO sample was studied using a transmission electron microscope (TEM) and a field-emission scanning electron microscope (FESEM). The morphologies of the ZnO structure consisted of many rod and spherical structures. The particle sizes of the sample ranged from 40 nm to 150 nm. A calamine lotion was prepared through mixing the ZnO structures with other constituents in suitable proportion. Themore » energy-dispersive x-ray spectroscopy (EDS) revealed the presence of large amount of ZnO structures whiles the X-ray diffraction (XRD) results showed a good crystalline property of ZnO in the calamine lotion mixture. The morphological structures of ZnO were found to remain unchanged in the calamine lotion mixture through FESEM imaging. In the antibacterial test, prepared calamine lotion exhibited a remarkable bacterial inhibition on Staphylococcus aureus and Pseudomonas aeruginosa after 24 h of treatment. The bactericidal capability of calamine lotion was largely due to the presence of ZnO structures which induce high toxicity and killing effect on the bacteria.« less

Fluorescence Spectrometric Determination of Drugs Containing α-Methylene Sulfone/Sulfonamide Functional Groups Using N-Methylnicotinamide Chloride as a Fluorogenic Agent.

PubMed

Elokely, Khaled M; Eldawy, Mohamed A; Elkersh, Mohamed A; El-Moselhy, Tarek F

2011-01-01

A simple spectrofluorometric method has been developed, adapted, and validated for the quantitative estimation of drugs containing α-methylene sulfone/sulfonamide functional groups using N(1)-methylnicotinamide chloride (NMNCl) as fluorogenic agent. The proposed method has been applied successfully to the determination of methyl sulfonyl methane (MSM) (1), tinidazole (2), rofecoxib (3), and nimesulide (4) in pure forms, laboratory-prepared mixtures, pharmaceutical dosage forms, spiked human plasma samples, and in volunteer's blood. The method showed linearity over concentration ranging from 1 to 150 μg/mL, 10 to 1000 ng/mL, 1 to 1800 ng/mL, and 30 to 2100 ng/mL for standard solutions of 1, 2, 3, and 4, respectively, and over concentration ranging from 5 to 150 μg/mL, 10 to 1000 ng/mL, 10 to 1700 ng/mL, and 30 to 2350 ng/mL in spiked human plasma samples of 1, 2, 3, and 4, respectively. The method showed good accuracy, specificity, and precision in both laboratory-prepared mixtures and in spiked human plasma samples. The proposed method is simple, does not need sophisticated instruments, and is suitable for quality control application, bioavailability, and bioequivalency studies. Besides, its detection limits are comparable to other sophisticated chromatographic methods.

Measurement of Neuropeptides in Crustacean Hemolymph via MALDI Mass Spectrometry

PubMed Central

Chen, Ruibing; Ma, Mingming; Hui, Limei; Zhang, Jiang; Li, Lingjun

2009-01-01

Neuropeptides are often released into circulatory fluid (hemolymph) to act as circulating hormones and regulate many physiological processes. However, the detection of these low-level peptide hormones in circulation is often complicated by high salt interference and rapid degradation of proteins and peptides in crude hemolymph extracts. In this study, we systematically evaluated three different neuropeptide extraction protocols and developed a simple and effective hemolymph preparation method suitable for MALDI MS profiling of neuropeptides by combining acid-induced abundant protein precipitation/depletion, ultrafiltration, and C18 micro-column desalting. In hemolymph samples collected from crab Cancer borealis several secreted neuropeptides have been detected, including members from at least five neuropeptide families, such as RFamide, allatostatin, orcokinin, tachykinin-related peptide (TRP), and crustacean cardioactive peptide (CCAP). Furthermore, two TRPs were detected in the hemolymph collected from food-deprived animals, suggesting the potential role of these neuropeptides in feeding regulation. In addition, a novel peptide with a Lys-Phe-amide C-terminus was identified and de novo sequenced directly from the Cancer borealis hemolymph sample. To better characterize the hemolymph peptidome, we also identified several abundant peptide signals in C. borealis hemolymph that were assigned to protein degradation products. Collectively, our study describes a simple and effective sample preparation method for neuropeptide analysis directly from crude crustacean hemolymph. Numerous endogenous neuropeptides were detected including both known ones and new peptides whose functions remain to be characterized. PMID:19185513

Matrix-assisted laser desorption-ionization time-of-flight mass spectrometry in the subunit stoichiometry study of high-mass non-covalent complexes

NASA Astrophysics Data System (ADS)

Moniatte, M.; Lesieur, C.; Vecsey-Semjen, B.; Buckley, J. T.; Pattus, F.; van der Goot, F. G.; van Dorsselaer, A.

1997-12-01

This study explores the potential of MALDI-TOF MS for the mass measurement of large non-covalent protein complexes. The following non-covalent complexes have been investigated: aerolysin from Aeromonas hydrophila (335 kDa) and [alpha]-haemolysin from Staphylococcus aureus (233 kDa) which are both cytolytic toxins, three enzymes known to be homotetramers in solution: bovine liver catalase (235 kDa), rabbit muscle pyruvate kinase (232 kDa), yeast alcohol dehydrogenase (147 kDa) and finally a lectin, concanavalin A (102 kDa). Three different matrix preparations were systematically tested under various conditions: ferulic acid dissolved in THF, 2,6-dihydroxyacetophenone in 20 mM aqueous ammonium citrate and a two-step sample preparation with sinapinic acid. It was possible to find a suitable combination of matrix and preparation type which allowed the molecularity of all complexes tested to be deduced from the MALDI mass spectrum. Trimeric and tetrameric intermediates accumulating during the formation of the active heptameric aerolysin complex were also identified, this allowing a formation mechanism to be proposed. The observation of large specific non-covalent complexes has been found to be dependent on the choice of matrix, the type of sample preparation used, the solvent evaporation speed, the pH of the resulting matrix-sample mixture and the number of shots acquired on a given area. From this set of experiments, some useful guidelines for the observation of large complexes by MALDI could therefore be deduced. Fast evaporation of the solvent is particularly necessary in the case of pH sensitive complexes. An ESMS study on the same non-covalent complexes indicated that, rather surprisingly, reliable results could be obtained by MALDI-TOF MS on several very large complexes (above 200 kDa) for which ESMS yielded no clear spectra.

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.

Astronaut training manual

NASA Technical Reports Server (NTRS)

Coleman, E. A.

1980-01-01

Scientific information from previous space flights, space medicine, exercise physiology, and sports medicine was used to prepare a physical fitness manual suitable for use by members of the NASA astronaut population. A variety of scientifically valid exercise programs and activities suitable for the development of physical fitness are provided. Programs, activities, and supportive scientific data are presented in a concise, easy to read format so as to permit the user to select his or her mode of training with confidence and devote time previously spent experimenting with training routines to preparation for space flight. The programs and activities included were tested and shown to be effective and enjoyable.

Development of a screen-printed carbon electrode based disposable enzyme sensor strip for the measurement of glycated albumin.

PubMed

Hatada, Mika; Tsugawa, Wakako; Kamio, Eri; Loew, Noya; Klonoff, David C; Sode, Koji

2017-02-15

Glycated proteins, such as glycated hemoglobin (HbA1c) or glycated albumin (GA) in the blood, are essential indicators of glycemic control for diabetes mellitus. Since GA, compared to HbA1c, is more sensitive to short term changes in glycemic levels, GA is expected to be used as an alternative or together with HbA1c as a surrogate marker indicator for glycemic control. In this paper we report the development of a sensing system for measuring GA by combining an enzyme analysis method, which is already used in clinical practice, with electrochemical principles. We used fructosyl amino acid oxidase, hexaammineruthenium(III) chloride as the electron mediator, and an inexpensive and economically attractive screen-printed carbon electrode. We used chronoamperometry to measure protease-digested GA samples. The developed sensor strips were able to measure protease-digested samples containing GA in very small sample volumes (1.3μL) within about 1min. We also prepared enzyme sensor strips suitable for clinical use in which the enzyme and the mediator were deposited and dried on. This sensor system showed a clear correlation between the GA concentration and the resulting current. The strips were stable following 3 months of storage at 37°C. We conclude that this disposable enzyme sensor strip system for measuring GA is suitable for point-of-care test (POCT) applications. Copyright © 2016 Elsevier B.V. All rights reserved.

In vitro biosynthesis, isolation, and identification of predominant metabolites of 2-(4-(2-hydroxyethoxy)-3,5-dimethylphenyl)-5,7-dimethoxyquinazolin-4(3H)-one (RVX-208).

PubMed

Khmelnitsky, Yuri L; Mozhaev, Vadim V; Cotterill, Ian C; Michels, Peter C; Boudjabi, Sihem; Khlebnikov, Vladimir; Madhava Reddy, M; Wagner, Gregory S; Hansen, Henrik C

2013-06-01

The structures of the two predominant metabolites (M4 and M5) of RVX-208, observed both in in vitro human and animal liver microsomal incubations, as well as in plasma from animal in vivo studies, were determined. A panel of biocatalytic systems was tested to identify biocatalysts suitable for milligram scale production of metabolite M4 from RVX-208. Rabbit liver S9 fraction was selected as the most suitable system, primarily based on pragmatic metrics such as catalyst cost and estimated yield of M4 (∼55%). Glucuronidation of RVX-208 catalyzed by rabbit liver S9 fraction was optimized to produce M4 in amounts sufficient for structural characterization. Structural studies using LC/MS/MS analysis and (1)H NMR spectroscopy showed the formation of a glycosidic bond between the primary hydroxyl group of RVX-208 and glucuronic acid. NMR results suggested that the glycosidic bond has the β-anomeric configuration. A synthetic sample of M4 confirmed the proposed structure. Metabolite M5, hypothesized to be the carboxylate of RVX-208, was prepared using human liver microsomes, purified by HPLC, and characterized by LC/MS/MS and (1)H NMR. The structure was confirmed by comparison to a synthetic sample. Both samples confirmed M5 as a product of oxidation of primary hydroxyl group of RVX-208 to carboxylic acid. Copyright © 2013 Elsevier Masson SAS. All rights reserved.

Evaluation of Training Samples Manually Welded With the Universal Handtool in a Space Simulation Chamber

NASA Technical Reports Server (NTRS)

Russell, C. K.; Malone, T. W.; Cato, S. N.

2004-01-01

The international space welding experiment was designed to evaluate the universal handtool (UHT) functions as a welding, brazing, coating, and cutting tool for in-space operations. The UHT is an electron beam welding system developed by the Paton Welding Institute (PWI), Kiev, Ukraine, and operated a 8 kV with up to 1 kW of power. In preparation for conducting the space welding experiment, cosmonauts were trained to properly operate the UHT and correctly process samples. This Technical Memorandum presents the results of the destructive and nondestructive evaluation of the training samples made in Russia in 1998. It was concluded that acceptable welds can be made with the UHT despite the constraints imposed by a space suit. The lap joint fillet weld configuration was more suitable than the butt joint configuration for operators with limited welding experience. The tube braze joint configuration designed by the PWI was easily brazed in a repeatable manner.

Geochemistry of CI chondrites: Major and trace elements, and Cu and Zn Isotopes

NASA Astrophysics Data System (ADS)

Barrat, J. A.; Zanda, B.; Moynier, F.; Bollinger, C.; Liorzou, C.; Bayon, G.

2012-04-01

In order to check the heterogeneity of the CI chondrites and determine the average composition of this group of meteorites, we analyzed a series of six large chips (weighing between 0.6 and 1.2 g) of Orgueil prepared from five different stones. In addition, one sample from each of Ivuna and Alais was analyzed. Although the sizes of the chips used in this study were “large”, our results show evidence for minor chemical heterogeneity in Orgueil, particularly for alkali elements and U. After removal of one outlier sample, the spread of the results is considerably reduced. For most of the 46 elements analyzed in this study, the average composition calculated for Orgueil is in very good agreement with previous CI estimates. This average, obtained with a “large” mass of samples, is analytically homogeneous and is suitable for normalization purposes. Finally, the Cu and Zn isotopic ratios are homogeneously distributed within the CI parent body with a spread of less than 100 ppm per atomic mass unit (amu).

A simple aloe vera plant-extracted microwave and conventional combustion synthesis: Morphological, optical, magnetic and catalytic properties of CoFe2O4 nanostructures

NASA Astrophysics Data System (ADS)

Manikandan, A.; Sridhar, R.; Arul Antony, S.; Ramakrishna, Seeram

2014-11-01

Nanocrystalline magnetic spinel CoFe2O4 was synthesized by a simple microwave combustion method (MCM) using ferric nitrate, cobalt nitrate and Aloe vera plant extracted solution. For the comparative study, it was also prepared by a conventional combustion method (CCM). Powder X-ray diffraction, energy dispersive X-ray and selected-area electron diffraction results indicate that the as-synthesized samples have only single-phase spinel structure with high crystallinity and without the presence of other phase impurities. The crystal structure and morphology of the powders were revealed by high resolution scanning electron microscopy and transmission electron microscopy, show that the MCM products of CoFe2O4 samples contain sphere-like nanoparticles (SNPs), whereas the CCM method of samples consist of flake-like nanoplatelets (FNPs). The band gap of the samples was determined by UV-Visible diffuse reflectance and photoluminescence spectroscopy. The magnetization (Ms) results showed a ferromagnetic behavior of the CoFe2O4 nanostructures. The Ms value of CoFe2O4-SNPs is higher i.e. 77.62 emu/g than CoFe2O4-FNPs (25.46 emu/g). The higher Ms value of the sample suggest that the MCM technique is suitable for preparing high quality nanostructures for magnetic applications. Both the samples were successfully tested as catalysts for the conversion of benzyl alcohol. The resulting spinel ferrites were highly selective for the oxidation of benzyl alcohol and exhibit important difference among their activities. It was found that CoFe2O4-SNPs catalyst show the best performance, whereby 99.5% selectivity of benzaldehyde was achieved at close to 93.2% conversion.

A simple and automated sample preparation system for subsequent halogens determination: Combustion followed by pyrohydrolysis.

PubMed

Pereira, L S F; Pedrotti, M F; Vecchia, P Dalla; Pereira, J S F; Flores, E M M

2018-06-20

A simple and automated system based on combustion followed by a pyrohydrolysis reaction was proposed for further halogens determination. This system was applied for digestion of soils containing high (90%) and also low (10%) organic matter content for further halogens determination. The following parameters were evaluated: sample mass, use of microcrystalline cellulose and heating time. For analytes absorption, a diluted alkaline solution (6 mL of 25 mmol L -1  NH 4 OH) was used in all experiments. Up to 400 mg of soil with high organic matter content and 100 mg of soil with low organic matter content (mixed with 400 mg of cellulose) could be completely digested using the proposed system. Quantitative results for all halogens were obtained using less than 12 min of sample preparation step (about 1.8 min for sample combustion and 10 min for pyrohydrolysis). The accuracy was evaluated using a certified reference material of coal and spiked samples. No statistical difference was observed between the certified values and results obtained by the proposed method. Additionally, the recoveries obtained using spiked samples were in the range of 98-103% with relative standard deviation values lower than 5%. The limits of quantification obtained for F, Cl, Br and I for soil with high (400 mg of soil) and low (100 mg of soil) organic matter were in the range of 0.01-2 μg g -1 and 0.07-59 μg g -1 , respectively. The proposed system was considered as a simple and suitable alternative for soils digestion for further halogens determination by ion chromatography and inductively coupled plasma mass spectrometry techniques. Copyright © 2018 Elsevier B.V. All rights reserved.

Process for the synthesis of iron powder

DOEpatents

Welbon, W.W.

1983-11-08

A process for preparing iron powder suitable for use in preparing the iron-potassium perchlorate heat-powder fuel mixture used in thermal batteries, comprises preparing a homogeneous, dense iron oxide hydroxide precipitate by homogeneous precipitation from an aqueous mixture of a ferric salt, formic or sulfuric acid, ammonium hydroxide and urea as precipitating agent; and then reducing the dense iron oxide hydroxide by treatment with hydrogen to prepare the iron powder. 2 figs.

Effect of charge compensator ions (R+ = Li+, Na+ and K+) on Sr2MgSi2O7:Dy3+ phosphors by solid-state reaction method

NASA Astrophysics Data System (ADS)

Sahu, Ishwar Prasad

2016-09-01

The Sr2MgSi2O7:Dy3+ and Sr2MgSi2O7:Dy3+, R+ (R+ = Li+, Na+ and K+) phosphors were prepared by solid-state reaction method. The crystal structures of sintered phosphors were an akermanite-type structure which belongs to the tetragonal crystallography. The prepared phosphors were excited at 350 nm, and their corresponding emission spectrum were recorded at blue (482 nm) and yellow (575 nm) region due to the 4F9/2 → 6H15/2 and 4F9/2 → 6H13/2 transitions, respectively, of Dy3+ ions. Commission Internationale de L'Eclairage coordinates have been calculated for each sample and its value exhibited that overall emission is near white light. The possible mechanisms of discussed white light emitting phosphors were also investigated. In order to investigate the suitability of the samples as white color light sources for industrial uses, color purity, correlated color temperature (CCT) and color rendering index (CRI) were calculated. Values of color purity, CCT and CRI were found well within the defined acceptable range. With incorporating (R+ = Li+, Na+ and K+) as charge compensator ions, the emission intensity of Sr2MgSi2O7:Dy3+ can be obviously enhanced. The results indicate that prepared phosphors may be a potential application in display devices.

Survival of Escherichia coli O157:H7 in ground beef jerky assessed on two plating media.

PubMed

Harrison, J A; Harrison, M A; Rose, R A

1998-01-01

Recent outbreaks of food-borne illness due to Salmonella spp. in beef jerky and Escherichia coli O157:H7 in venison jerky, coupled with the fact that a variety of preparation methods and dying procedures abound, raise concern over the safety of processed meat products made in the home. The potential of injured bacterial cells to regain the ability to cause illness is a particular threat with pathogens such as E. coli O157:H7, which is believed to have a low infectious dose. This study examined the efficacy of various methods of jerky preparation in reducing populations of E, coli O157:H7 in ground beef jerky and compared the recovery rate of E. coli O157:H7 on two selective plating media, modified sorbitol MacConkey agar (MSMA) and modified eosin methylene blue agar (MEMB). Populations of E. coli O157:H7 in both heated and unheated samples exhibited a greater decline during drying when a nitrite and salt cure mix was added during jerky preparation. When recovery of E. coli O157:H7 on MSMA and MEMB was compared, a trend toward slightly higher recovery rates with MEMB was observed. On the basis of these results, MEMB is a suitable alternative to MSMA for the recovery of E. coli O157:H7 from heated and dried meat samples similar to beef jerky.

Study of formation of deep trapping mechanism by UV, beta and gamma irradiated Eu(3+) activated SrY2O4 and Y4Al2O9 phosphors.

PubMed

Dubey, Vikas; Kaur, Jagjeet; Parganiha, Yogita; Suryanarayana, N S; Murthy, K V R

2016-04-01

This paper reports the thermoluminescence properties of Eu(3+) doped different host matrix phosphors (SrY2O4 and Y4Al2O9). The phosphor is prepared by high temperature solid state reaction method. The method is suitable for large scale production and fixed concentration of boric acid using as a flux. The prepared samples were characterized by X-ray diffraction technique and the crystallite size calculated by Scherer's formula. The prepared phosphor characterized by Scanning Electron Microscopic (SEM), Fourier Transform Infrared (FTIR), Energy Dispersive X-ray analysis (EDX), thermoluminescence (TL) and Transmission Electron Microscopic (TEM) techniques. The prepared phosphors for different concentration of Eu(3+) ions were examined by TL glow curve for UV, beta and gamma irradiation. The UV 254nm source used for UV irradiation, Sr(90) source was used for beta irradiation and Co(60) source used for gamma irradiation. SrY2O4:Eu(3+)and Y4Al2O9:Eu(3+) phosphors which shows both higher temperature peaks and lower temperature peaks for UV, beta and gamma irradiation. Here UV irradiated sample shows the formation of shallow trap (surface trapping) and the gamma irradiated sample shows the formation of deep trapping. The estimation of trap formation was evaluated by knowledge of trapping parameters. The trapping parameters such as activation energy, order of kinetics and frequency factor were calculated by peak shape method. Here most of the peak shows second order of kinetics. The effect of gamma, beta and UV exposure on TL studies was also examined and it shows linear response with dose which indicate that the samples may be useful for TL dosimetry. Formation of deep trapping mechanism by UV, beta and gamma irradiated Eu(3+) activated SrY2O4 and Y4Al2O9 phosphors is discussed in this paper. Copyright © 2015 Elsevier Ltd. All rights reserved.

21 CFR 113.81 - Product preparation.

Code of Federal Regulations, 2011 CFR

2011-04-01

... Production and Process Controls § 113.81 Product preparation. (a) Before using raw materials and ingredients susceptible to microbiological contamination, the processor shall ensure that those materials and ingredients... by receiving the raw materials and ingredients under a supplier's guarantee that they are suitable...

Nuclear Instruments and Methods in Physics Research. Section B; Microstructural Characterization of Semi-Interpenetrating Polymer Networks by Positron Lifetime Spectroscopy

NASA Technical Reports Server (NTRS)

Singh, Jag J.; Pater, Ruth H.; Eftekhari, Abe

1998-01-01

Thermoset and thermoplastic polyimides have complementary physical/mechanical properties. Whereas thermoset polyimides are brittle and generally easier to process, thermoplastic polyimides are tough but harder to process. It is expected that a combination of these two types of polyimides may help produce polymers more suitable for aerospace applications. Semi-Interpenetrating Polymer Networks (S-IPNs) of thermoset LaRC(Trademark)-RP46 and thermoplastic LARC(Trademark)-IA polyimides were prepared in weight percent ratios ranging from 100:0 to 0: 100. Positron lifetime measurements were made in these samples to correlate their free volume features with physical/mechanical properties. As expected, positronium atoms are not formed in these samples. The second life time component has been used to infer the positron trap dimensions. The "free volume" goes through a minimum at about 50:50 ratio, suggesting that S-IPN samples are not merely solid solutions of the two polymers. These data and related structural properties of the S-IPN samples have been discussed in this paper.

Accelerator mass spectrometry of strontium-90 for homeland security, environmental monitoring and human health

NASA Astrophysics Data System (ADS)

Tumey, Scott J.; Brown, Thomas A.; Hamilton, Terry E.; Hillegonds, Darren J.

2008-05-01

Strontium-90 is one of the most hazardous materials managed by agencies charged with protecting the public from radiation. Traditional radiometric methods have been limited by low sample throughput and slow turnaround times. Mass spectrometry offers the advantage of shorter analysis times and the ability to measure samples immediately after processing, however conventional mass spectrometric techniques are susceptible to molecular isobaric interferences that limit their overall sensitivity. In contrast, accelerator mass spectrometry is insensitive to molecular interferences and we have therefore begun developing a method for determination of 90Sr by accelerator mass spectrometry. Despite a pervasive interference from 90Zr, our initial development has yielded an instrumental background of ∼108 atoms (75 mBq) per sample. Further refinement of our system (e.g. redesign of our detector, use of alternative target materials) is expected to push the background below 106 atoms, close to the theoretical limit for AMS. Once we have refined our system and developed suitable sample preparation protocols, we will utilize our capability in applications to homeland security, environmental monitoring and human health.

An iterative and targeted sampling design informed by habitat suitability models for detecting focal plant species over extensive areas.

PubMed

Wang, Ophelia; Zachmann, Luke J; Sesnie, Steven E; Olsson, Aaryn D; Dickson, Brett G

2014-01-01

Prioritizing areas for management of non-native invasive plants is critical, as invasive plants can negatively impact plant community structure. Extensive and multi-jurisdictional inventories are essential to prioritize actions aimed at mitigating the impact of invasions and changes in disturbance regimes. However, previous work devoted little effort to devising sampling methods sufficient to assess the scope of multi-jurisdictional invasion over extensive areas. Here we describe a large-scale sampling design that used species occurrence data, habitat suitability models, and iterative and targeted sampling efforts to sample five species and satisfy two key management objectives: 1) detecting non-native invasive plants across previously unsampled gradients, and 2) characterizing the distribution of non-native invasive plants at landscape to regional scales. Habitat suitability models of five species were based on occurrence records and predictor variables derived from topography, precipitation, and remotely sensed data. We stratified and established field sampling locations according to predicted habitat suitability and phenological, substrate, and logistical constraints. Across previously unvisited areas, we detected at least one of our focal species on 77% of plots. In turn, we used detections from 2011 to improve habitat suitability models and sampling efforts in 2012, as well as additional spatial constraints to increase detections. These modifications resulted in a 96% detection rate at plots. The range of habitat suitability values that identified highly and less suitable habitats and their environmental conditions corresponded to field detections with mixed levels of agreement. Our study demonstrated that an iterative and targeted sampling framework can address sampling bias, reduce time costs, and increase detections. Other studies can extend the sampling framework to develop methods in other ecosystems to provide detection data. The sampling methods implemented here provide a meaningful tool when understanding the potential distribution and habitat of species over multi-jurisdictional and extensive areas is needed for achieving management objectives.

An Iterative and Targeted Sampling Design Informed by Habitat Suitability Models for Detecting Focal Plant Species over Extensive Areas

PubMed Central

Wang, Ophelia; Zachmann, Luke J.; Sesnie, Steven E.; Olsson, Aaryn D.; Dickson, Brett G.

2014-01-01

Prioritizing areas for management of non-native invasive plants is critical, as invasive plants can negatively impact plant community structure. Extensive and multi-jurisdictional inventories are essential to prioritize actions aimed at mitigating the impact of invasions and changes in disturbance regimes. However, previous work devoted little effort to devising sampling methods sufficient to assess the scope of multi-jurisdictional invasion over extensive areas. Here we describe a large-scale sampling design that used species occurrence data, habitat suitability models, and iterative and targeted sampling efforts to sample five species and satisfy two key management objectives: 1) detecting non-native invasive plants across previously unsampled gradients, and 2) characterizing the distribution of non-native invasive plants at landscape to regional scales. Habitat suitability models of five species were based on occurrence records and predictor variables derived from topography, precipitation, and remotely sensed data. We stratified and established field sampling locations according to predicted habitat suitability and phenological, substrate, and logistical constraints. Across previously unvisited areas, we detected at least one of our focal species on 77% of plots. In turn, we used detections from 2011 to improve habitat suitability models and sampling efforts in 2012, as well as additional spatial constraints to increase detections. These modifications resulted in a 96% detection rate at plots. The range of habitat suitability values that identified highly and less suitable habitats and their environmental conditions corresponded to field detections with mixed levels of agreement. Our study demonstrated that an iterative and targeted sampling framework can address sampling bias, reduce time costs, and increase detections. Other studies can extend the sampling framework to develop methods in other ecosystems to provide detection data. The sampling methods implemented here provide a meaningful tool when understanding the potential distribution and habitat of species over multi-jurisdictional and extensive areas is needed for achieving management objectives. PMID:25019621

A simple and rapid method for preparing the whole section of starchy seed to investigate the morphology and distribution of starch in different regions of seed.

PubMed

Zhao, Lingxiao; Pan, Ting; Guo, Dongwei; Wei, Cunxu

2018-01-01

Storage starch in starchy seed influences the seed weight and texture, and determines its applications in food and nonfood industries. Starch granules from different plant sources have significantly different shapes and sizes, and even more the difference exists in the different regions of the same tissue. Therefore, it is very important to in situ investigate the morphology and distribution of starch in the whole seed. However, a simple and rapid method is deficient to prepare the whole section of starchy seed for investigating the morphology and distribution of starch in the whole seeds for a large number of samples. A simple and rapid method was established to prepare the whole section of starchy seed, especially for floury seed, in this study. The whole seeds of translucent and chalky rice, vitreous and floury maize, and normal barley and wheat were sectioned successfully using the newly established method. The iodine-stained section clearly exhibited the shapes and size of starch granules in different regions of seed. The starch granules with different morphologies and iodine-staining colors existed regionally in the seeds of high-amylose rice and maize. The sections of lotus and kidney bean seeds also showed the feasibility of this method for starchy non-cereal seeds. The simple and rapid method was proven effective for preparing the whole sections of starchy seeds. The whole section of seed could be used to investigate the morphology and distribution of starch granules in different regions of the whole seed. The method was especially suitable for large sample numbers to investigate the starch morphology in short time.

Maskless Lithography Using Negative Photoresist Material: Impact of UV Laser Intensity on the Cured Line Width

NASA Astrophysics Data System (ADS)

Mohammed, Mohammed Ziauddin; Mourad, Abdel-Hamid I.; Khashan, Saud A.

2018-06-01

The application of maskless lithography technique on negative photoresist material is investigated in this study. The equipment used in this work is designed and built especially for maskless lithography applications. The UV laser of 405 nm wavelength with 0.85 Numerical Aperture is selected for direct laser writing. All the samples are prepared on a glass substrate. Samples are tested at different UV laser intensities and different stage velocities in order to study the impact on patterned line width. Three cases of spin coated layers of thickness 90 μm, 40 μm, and 28 μm on the substrate are studied. The experimental results show that line width has a generally increasing trend with intensity. However, a decreasing trend was observed for increasing velocity. The overall performance shows that the mr-DWL material is suitable for direct laser writing systems.

Synthesis of nanocomposites based on carbon nanotube/smart copolymer with nonlinear optical properties

NASA Astrophysics Data System (ADS)

Sousani, Abbas; Motiei, Hamideh; Najafimoghadam, Peyman; Hasanzade, Reza

2017-05-01

In this study new nanocompoites based on polyglycidylmethacrylate grafted 4-[(4-methoxyphenyl) diazenyl] phenol (Azo-PGMA) and Carboxylicacid functionalized multi-walled carbon nanotubes (MWCNT-COOH) were prepared. The nanocomposites structure was characterized by FT-IR, TGA and SEM. The Z-scan technique was applied for measuring the nonlinear parameters of nanocomposites. The samples after solving in AWM solution (equal ratio of acetone, deionized water and methanol) were investigated by using closed aperture Z-scan technique and a diode-pumped laser at the line 532 nm. All the nonlinear refractive index of the samples at three concentrations of carbon nanotubes in three different intensities of the laser beam were investigated and the nonlinear optical response of them are compared under the same condition. Because of high order of nonlinear refractive coefficient and good nonlinearity, these compounds are suitable candidate for optical switching, optical limiting and electro-optical devices.

Maskless Lithography Using Negative Photoresist Material: Impact of UV Laser Intensity on the Cured Line Width

NASA Astrophysics Data System (ADS)

Mohammed, Mohammed Ziauddin; Mourad, Abdel-Hamid I.; Khashan, Saud A.

2018-04-01

The application of maskless lithography technique on negative photoresist material is investigated in this study. The equipment used in this work is designed and built especially for maskless lithography applications. The UV laser of 405 nm wavelength with 0.85 Numerical Aperture is selected for direct laser writing. All the samples are prepared on a glass substrate. Samples are tested at different UV laser intensities and different stage velocities in order to study the impact on patterned line width. Three cases of spin coated layers of thickness 90 μm, 40 μm, and 28 μm on the substrate are studied. The experimental results show that line width has a generally increasing trend with intensity. However, a decreasing trend was observed for increasing velocity. The overall performance shows that the mr-DWL material is suitable for direct laser writing systems.

Instant, Visual, and Instrument-Free Method for On-Site Screening of GTS 40-3-2 Soybean Based on Body-Heat Triggered Recombinase Polymerase Amplification.

PubMed

Wang, Rui; Zhang, Fang; Wang, Liu; Qian, Wenjuan; Qian, Cheng; Wu, Jian; Ying, Yibin

2017-04-18

On-site monitoring the plantation of genetically modified (GM) crops is of critical importance in agriculture industry throughout the world. In this paper, a simple, visual and instrument-free method for instant on-site detection of GTS 40-3-2 soybean has been developed. It is based on body-heat recombinase polymerase amplification (RPA) and followed with naked-eye detection via fluorescent DNA dye. Combining with extremely simplified sample preparation, the whole detection process can be accomplished within 10 min and the fluorescent results can be photographed by an accompanied smart phone. Results demonstrated a 100% detection rate for screening of practical GTS 40-3-2 soybean samples by 20 volunteers under different ambient temperatures. This method is not only suitable for on-site detection of GM crops but also demonstrates great potential to be applied in other fields.

Carbohydrate composition of compost during composting and mycelium growth of Agaricus bisporus.

PubMed

Jurak, Edita; Kabel, Mirjam A; Gruppen, Harry

2014-01-30

Changes of plant cell wall carbohydrate structures occurring during the process to make suitable compost for growth of Agaricus bisporus are unknown. In this paper, composition and carbohydrate structures in compost samples collected during composting and mycelium growth were analyzed. Furthermore, different extracts of compost samples were prepared with water, 1M and 4M alkali and analyzed. At the beginning of composting, 34% and after 16 days of mycelium growth 27% of dry matter was carbohydrates. Carbohydrate composition analysis showed that mainly cellulose and poorly substituted xylan chains with similar amounts and ratios of xylan building blocks were present in all phases studied. Nevertheless, xylan solubility increased 20% over the period of mycelium growth indicating partial degradation of xylan backbone. Apparently, degradation of carbohydrates occurred over the process studied by both bacteria and fungi, mainly having an effect on xylan-chain length and solubility. Copyright © 2013 Elsevier Ltd. All rights reserved.

Synthesis and characterization of MOF-aminated graphite oxide composites for CO2 capture

NASA Astrophysics Data System (ADS)

Zhao, Yunxia; Ding, Huiling; Zhong, Qin

2013-11-01

A kind of metal-organic frameworks (MOF-5) and aminated graphite oxide (AGO) composites were prepared for CO2 capture to mitigate global warming. MOF-5, MOF-5/GO (composite of MOF-5 and graphite oxide) and MOF-5/AGO samples were characterized by X-ray powder diffraction (XRD), infrared spectroscopy (IR), scanning electron microscope (SEM), nitrogen adsorption as well as thermogravimetric analysis to figure out their chemistry and structure information. Three types of samples with suitable specific surface area and pore diameter were chosen to test CO2 adsorption performance and stability under humidity conditions. The results indicate that high surface area and pore volume, pore similar in size to the size of gas adsorbate, and extra reactive sites modified in the composites contributes to the high CO2 capacity. Besides, the composites involved by GO or AGO show better anti-moisture performance than the parent MOF.

Tools for phospho- and glycoproteomics of plasma membranes.

PubMed

Wiśniewski, Jacek R

2011-07-01

Analysis of plasma membrane proteins and their posttranslational modifications is considered as important for identification of disease markers and targets for drug treatment. Due to their insolubility in water, studying of plasma membrane proteins using mass spectrometry has been difficult for a long time. Recent technological developments in sample preparation together with important improvements in mass spectrometric analysis have facilitated analysis of these proteins and their posttranslational modifications. Now, large scale proteomic analyses allow identification of thousands of membrane proteins from minute amounts of sample. Optimized protocols for affinity enrichment of phosphorylated and glycosylated peptides have set new dimensions in the depth of characterization of these posttranslational modifications of plasma membrane proteins. Here, I summarize recent advances in proteomic technology for the characterization of the cell surface proteins and their modifications. In the focus are approaches allowing large scale mapping rather than analytical methods suitable for studying individual proteins or non-complex mixtures.

Untargeted NMR Spectroscopic Analysis of the Metabolic Variety of New Apple Cultivars

PubMed Central

Eisenmann, Philipp; Ehlers, Mona; Weinert, Christoph H.; Tzvetkova, Pavleta; Silber, Mara; Rist, Manuela J.; Luy, Burkhard; Muhle-Goll, Claudia

2016-01-01

Metabolome analyses by NMR spectroscopy can be used in quality control by generating unique fingerprints of different species. Hundreds of components and their variation between different samples can be analyzed in a few minutes/hours with high accuracy and low cost of sample preparation. Here, apple peel and pulp extracts of a variety of apple cultivars were studied to assess their suitability to discriminate between the different varieties. The cultivars comprised mainly newly bred varieties or ones that were brought onto the market in recent years. Multivariate analyses of peel and pulp extracts were able to unambiguously identify all cultivars, with peel extracts showing a higher discriminative power. The latter was increased if the highly concentrated sugar metabolites were omitted from the analysis. Whereas sugar concentrations lay within a narrow range, polyphenols, discussed as potential health promoting substances, and acids varied remarkably between the cultivars. PMID:27657148

Untargeted NMR Spectroscopic Analysis of the Metabolic Variety of New Apple Cultivars.

PubMed

Eisenmann, Philipp; Ehlers, Mona; Weinert, Christoph H; Tzvetkova, Pavleta; Silber, Mara; Rist, Manuela J; Luy, Burkhard; Muhle-Goll, Claudia

2016-09-19

Metabolome analyses by NMR spectroscopy can be used in quality control by generating unique fingerprints of different species. Hundreds of components and their variation between different samples can be analyzed in a few minutes/hours with high accuracy and low cost of sample preparation. Here, apple peel and pulp extracts of a variety of apple cultivars were studied to assess their suitability to discriminate between the different varieties. The cultivars comprised mainly newly bred varieties or ones that were brought onto the market in recent years. Multivariate analyses of peel and pulp extracts were able to unambiguously identify all cultivars, with peel extracts showing a higher discriminative power. The latter was increased if the highly concentrated sugar metabolites were omitted from the analysis. Whereas sugar concentrations lay within a narrow range, polyphenols, discussed as potential health promoting substances, and acids varied remarkably between the cultivars.

A Single Molecular Diels-Alder Crosslinker for Achieving Recyclable Cross-Linked Polymers.

PubMed

Chen, Shengli; Wang, Fenfen; Peng, Yongjin; Chen, Tiehong; Wu, Qiang; Sun, Pingchuan

2015-09-01

A triol-functional crosslinker combining the thermoreversible properties of Diels-Alder (DA) adducts in one molecule is designed, synthesized, and used as an ideal substitute of a traditional crosslinker to prepare thermal recyclable cross-linked polyurethanes with excellent mechanical properties and recyclability in a very simple and efficient way. The recycle property of these materials achieved by the DA/retro-DA reaction at a suitable temperature is verified by differential scanning calorimetry and in situ variable temperature solid-state NMR experiments during the cyclic heating and cooling processes. The thermal recyclability and remending ability of the bulk polyurethanes is demonstrated by three polymer processing methods, including hot-press molding, injection molding, and solution casting. It is notable that all the recycled cross-linked polymers display nearly invariable elongation/stress at break compared to the as-synthesized samples. Further end-group functionalization of this single molecular DA crosslinker provides the potential in preparing a wide range of recyclable cross-linked polymers. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation of stir bars for sorptive extraction using sol-gel technology.

PubMed

Liu, Wenmin; Wang, Hanwen; Guan, Yafeng

2004-08-06

A sol-gel coating method for the preparation of extractive phase on bars used in sorptive microextraction is described. The extraction phase of poly(dimethylsiloxane) is partially crosslinked with the sol-gel network, and the most part is physically incorporated in the network. Three aging steps at different temperatures are applied to complete the crosslinking process. Thirty-micrometer-thick coating layer is obtained by one coating process. The improved coating shows good thermal stability up to 300 degrees C. Spiked aqueous samples containing n-alkanes, polycyclic aromatic hydrocarbons and organophosphorus pesticides were analyzed by using the sorptive bars and GC. The results demonstrate that it is suitable for both aploar and polar analytes. The detection limit for chrysene is 7.44 ng/L, 0.74 ng/L for C19 and 0.9 ng/L for phorate. The extraction equilibration can be reached in less than 15 min by supersonic extraction with the bars of 30 microm coating layer.

Evaluation of inorganic elements in cat's claw teas using ICP OES and GF AAS.

PubMed

Pereira, João B; Dantas, Kelly G F

2016-04-01

The determination of Ba, Ca, Cu, Fe, Mg, Mn, P, Pb, and Zn by inductively coupled plasma optical emission spectrometry (ICP OES), and Se by graphite furnace atomic absorption spectrometry (GF AAS), has been carried out in dry matter and teas from 11 samples of the cat's claw plant. The accuracy and precision values were verified against GBW 07604 (Poplar leaves) certified reference material and by the recovery test. Results showed a high content of Ca in the medicinal plant studied, followed by Mg and P. The values obtained showed that the elements studied have different concentrations depending on the method of tea preparation. The highest levels were observed in Ca and Mg, and the lowest for Se and Pb, by both infusion and decoction. Teas prepared from this plant were found to be at safe levels for human consumption, and may be suitable as sources of these elements in the human diet. Copyright © 2015 Elsevier Ltd. All rights reserved.

miRNA detection at single-cell resolution using microfluidic LNA flow-FISH

DOE PAGES

Wu, Meiye; Piccini, Matthew Ernest; Koh, Chung -Yan; ...

2014-08-20

Flow cytometry in combination with fluorescent in situ hybridization (flow-FISH) is a powerful technique that can be utilized to rapidly detect nucleic acids at single-cell resolution without the need for homogenization or nucleic acid extraction. Here, we describe a microfluidic-based method which enables the detection of microRNAs or miRNAs in single intact cells by flow-FISH using locked nucleic acid (LNA)-containing probes. Our method can be applied to all RNA species including mRNA and small noncoding RNA and is suitable for multiplexing with protein immunostaining in the same cell. For demonstration of our method, this chapter details the detection of miR155more » and CD69 protein in PMA and ionomycin-stimulated Jurkat cells. Here, we also include instructions on how to set up a microfluidic chip sample preparation station to prepare cells for imaging and analysis on a commercial flow cytometer or a custom-built micro-flow cytometer.« less

Ultrasonic analysis to discriminate bread dough of different types of flour

NASA Astrophysics Data System (ADS)

García-Álvarez, J.; Rosell, C. M.; García-Hernández, M. J.; Chávez, J. A.; Turó, A.; Salazar, J.

2012-12-01

Many varieties of bread are prepared using flour coming from wheat. However, there are other types of flours milled from rice, legumes and some fruits and vegetables that are also suitable for baking purposes, used alone or in combination with wheat flour. The type of flour employed strongly influences the dough consistency, which is a relevant property for determining the dough potential for breadmaking purposes. Traditional methods for dough testing are relatively expensive, time-consuming, off-line and often require skilled operators. In this work, ultrasonic analysis are performed in order to obtain acoustic properties of bread dough samples prepared using two different types of flour, wheat flour and rice flour. The dough acoustic properties can be related to its viscoelastic characteristics, which in turn determine the dough feasibility for baking. The main advantages of the ultrasonic dough testing can be, among others, its low cost, fast, hygienic and on-line performance. The obtained results point out the potential of the ultrasonic analysis to discriminate doughs of different types of flour.

Effect of sterilization on the physical stability of brimonidine-loaded solid lipid nanoparticles and nanostructured lipid carriers.

PubMed

El-Salamouni, Noha S; Farid, Ragwa M; El-Kamel, Amal H; El-Gamal, Safaa S

2015-12-30

Nanoparticulate delivery systems have recently been under consideration for topical ophthalmic drug delivery. Brimonidine base-loaded solid lipid nanoparticles and nanostructured lipid carrier formulations were prepared using glyceryl monostearate as solid lipid and were evaluated for their physical stability following sterilization by autoclaving at 121°C for 15min. The objective of this work was to evaluate the effect of autoclaving on the physical appearance, particle size, polydispersity index, zeta potential, entrapment efficiency and particle morphology of the prepared formulations, compared to non-autoclaved ones. Results showed that, autoclaving at 121°C for 15min allowed the production of physically stable formulations in nanometric range, below 500nm suitable for ophthalmic application. Moreover, the autoclaved samples appeared to be superior to non-autoclaved ones, due to their increased zeta potential values, indicating a better physical stability. As well as, increased amount of brimonidine base entrapped in the tested formulations. Copyright © 2015 Elsevier B.V. All rights reserved.

Apricot DNA as an indicator for persipan: detection and quantitation in marzipan using ligation-dependent probe amplification.

PubMed

Luber, Florian; Demmel, Anja; Hosken, Anne; Busch, Ulrich; Engel, Karl-Heinz

2012-06-13

The confectionery ingredient marzipan is exclusively prepared from almond kernels and sugar. The potential use of apricot kernels, so-called persipan, is an important issue for the quality assessment of marzipan. Therefore, a ligation-dependent probe amplification (LPA) assay was developed that enables a specific and sensitive detection of apricot DNA, as an indicator for the presence of persipan. The limit of detection was determined to be 0.1% persipan in marzipan. The suitability of the method was confirmed by the analysis of 20 commercially available food samples. The integration of a Prunus -specific probe in the LPA assay as a reference allowed for the relative quantitation of persipan in marzipan. The limit of quantitation was determined to be 0.5% persipan in marzipan. The analysis of two self-prepared mixtures of marzipan and persipan demonstrated the applicability of the quantitation method at concentration levels of practical relevance for quality control.

Quantitative 3D Analysis of Nuclear Morphology and Heterochromatin Organization from Whole-Mount Plant Tissue Using NucleusJ.

PubMed

Desset, Sophie; Poulet, Axel; Tatout, Christophe

2018-01-01

Image analysis is a classical way to study nuclear organization. While nuclear organization used to be investigated by colorimetric or fluorescent labeling of DNA or specific nuclear compartments, new methods in microscopy imaging now enable qualitative and quantitative analyses of chromatin pattern, and nuclear size and shape. Several procedures have been developed to prepare samples in order to collect 3D images for the analysis of spatial chromatin organization, but only few preserve the positional information of the cell within its tissue context. Here, we describe a whole mount tissue preparation procedure coupled to DNA staining using the PicoGreen ® intercalating agent suitable for image analysis of the nucleus in living and fixed tissues. 3D Image analysis is then performed using NucleusJ, an open source ImageJ plugin, which allows for quantifying variations in nuclear morphology such as nuclear volume, sphericity, elongation, and flatness as well as in heterochromatin content and position in respect to the nuclear periphery.

Quality control of plant food supplements.

PubMed

Sanzini, Elisabetta; Badea, Mihaela; Santos, Ariana Dos; Restani, Patrizia; Sievers, Hartwig

2011-12-01

It is essential to guarantee the safety of unprocessed plants and food supplements if consumers' health is to be protected. Although botanicals and their preparations are regulated at EU level, at least in part, there is still considerable discretion at national level, and Member States may choose to classify a product either as a food supplement or as a drug. Accurate data concerning the finished products and the plant used as the starting point are of major importance if risks and safety are to be properly assessed, but in addition standardized criteria for herbal preparation must be laid down and respected by researchers and manufacturers. Physiologically active as well as potentially toxic constituents need to be identified, and suitable analytical methods for their measurement specified, particularly in view of the increasing incidence of economically motivated adulteration of herbal raw materials and extracts. It remains the duty of food operators to keep up with the scientific literature and to provide sufficient information to enable the adaptation of specifications, sampling schemes and analytical methods to a fast-changing environment.

Dithizone modified magnetic nanoparticles for fast and selective solid phase extraction of trace elements in environmental and biological samples prior to their determination by ICP-OES.

PubMed

Cheng, Guihong; He, Man; Peng, Hanyong; Hu, Bin

2012-01-15

A fast and simple method for analysis of trace amounts of Cr(III), Cu(II), Pb(II) and Zn(II) in environmental and biological samples was developed by combining magnetic solid phase extraction (MSPE) with inductively coupled plasma-optical emission spectrometry (ICP-OES) detection. Dithizone modified silica-coated magnetic Fe(3)O(4) nanoparticles (H(2)Dz-SCMNPs) were prepared and used for MSPE of trace amounts of Cr(III), Cu(II), Pb(II) and Zn(II). The prepared magnetic nanoparticles were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray powder diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). The factors affecting the extraction of the target metal ions such as pH, sample volume, eluent, and interfering ions had been investigated and the adsorption mechanism of the target metals on the self-prepared H(2)Dz-SCMNPs was investigated by FT-IR and X-ray photo electron spectroscopy (XPS). Under the optimized conditions, the detection limits of the developed method for Cr(III), Cu(II), Pb(II) and Zn(II) were 35, 11, 62, and 8ngL(-1), respectively, with the enrichment factor of 100. The relative standard deviations (RSDs, c=10μgL(-1), n=7) were in the range of 1.7-3.1% and the linear range was 0.1-100μgL(-1). The proposed method had been validated by two certified reference materials (GSBZ50009-88 environmental water and GBW07601 human hair), and the determined values were in good agreement with the certified values. The method was also applied for the determination of trace metals in real water and human hair samples with recoveries in the range of 85-110% for the spiked samples. The developed MSPE-ICP-OES method has the advantages of simplicity, rapidity, selectivity, high extraction efficiency and is suitable for the analysis of samples with large volume and complex matrix. Copyright © 2011 Elsevier B.V. All rights reserved.

Changes in the quality of surimi made from thornback ray (Raja clavata, L. 1758) during frozen storage.

PubMed

Turan, Hülya; Sönmez, Gülşah

2007-11-01

Surimi was prepared from the thornback ray (Raja clavata L. 1758) and divided into two groups. The first group was prepared with 4% sorbitol, 4% sucrose and 0.3% sodium tripolyphosphate as a cryoprotectant, while surimi in second group was prepared with 8% sorbitol and 0.3% sodium tripolyphosphate. The frozen surimi samples were stored at 23.8 +/- 2 degrees C for 6 months. The total volatile basic nitrogen (8.40 mg/100 g for group A, 6.30 mg/100 g for group B), trimethylamine nitrogen (2.55 mg/100 g for group A, 2.38 mg/100 g for group B), thiobarbituric acid (1.29 mg malondialdehyde/100 g for group A, 1.17 mg malondialdehyde/ 100 g for group B), and pH values (7.34 for group A, 6.98 for group B) of surimi increased during frozen storage but remained within the acceptable limits. Total psychrophilic aerobic bacteria counts and sensory evaluation points in both groups decreased during frozen storage. The results of this study showed that thornback ray was found to be suitable for surimi production and the surimis were still acceptable at the end of the 6-month storage period.

Scalable purification of the lantibiotic nisin and isolation of chemical/enzymatic cleavage fragments suitable for semi-synthesis.

PubMed

Slootweg, Jack C; Liskamp, Rob M J; Rijkers, Dirk T S

2013-11-01

Herein, we describe a scalable purification of the lantibiotic nisin via an extraction/precipitation approach using a biphasic system, which can be carried out up to 40-80 gram scale. This approach results in an at least tenfold enrichment of commercially available preparations of nisin, which usually contain only 2.5% of the desired peptide, to allow further purification by preparative HPLC. As a follow-up study, the enriched nisin sample was digested either by trypsin or chymotrypsin, or treated by CNBr, and these reactions were monitored by LC-MS to identify and characterize the obtained fragments. Two previously unknown cleavage sites have been identified: Asn20-Met21 and Met21-Lys22 for trypsin and chymotrypsin, respectively. Furthermore, a novel and convenient enzymatic approach to isolate the native nisin C-ring [nisin fragment (13-20)] was uncovered. Finally, by means of preparative HPLC, nisin fragments (1-12), (1-20), (22-34), and (22-31) could be isolated and will be used in a semi-synthesis approach to elucidate the role of each fragment in the mode of action of nisin as an antimicrobial peptide. Copyright © 2013 European Peptide Society and John Wiley & Sons, Ltd.

The suitability of the simplified method of the analysis of coffee infusions on the content of Ca, Cu, Fe, Mg, Mn and Zn and the study of the effect of preparation conditions on the leachability of elements into the coffee brew.

PubMed

Stelmach, Ewelina; Pohl, Pawel; Szymczycha-Madeja, Anna

2013-12-01

A fast and straightforward method of the analysis of coffee infusions was developed for measurements of total concentrations of Ca, Cu, Fe, Mg, Mn and Zn by flame atomic absorption spectrometry. Its validity was proved by the analysis of spiked samples; recoveries of added metals were found to be within 98-104% while the precision was better than 4%. The method devised was used for the analysis of re-distilled water infusions of six popular ground coffees available in the Polish market. Using the mud coffee preparation it was established that percentages of metals leached in these conditions varied a lot among analysed coffees, especially for Ca (14-42%), Mg (6-25%) and Zn (1-24%). For remaining metals, the highest extractabilities were assessed for Mn (30-52%) while the lowest for Fe (4-16%) and Cu (2-12%). In addition, it was found that the water type and the coffee brewing preparation method influence the concentration of studied metals in coffee infusions the most. Copyright © 2013 Elsevier Ltd. All rights reserved.

Simultaneous determination of ezetimibe and simvastatin in pharmaceutical preparations by MEKC.

PubMed

Yardimci, Ceren; Ozaltin, Nuran

2010-02-01

A micellar electrokinetic capillary chromatography method was developed and validated for the simultaneous determination of ezetimibe and simvastatin in pharmaceutical preparations. The influence of buffer concentration, buffer pH, sodium dodecyl sulphate (SDS) concentration, organic modifier, capillary temperature, applied voltage, and injection time was investigated, and the method validation studies were performed. The optimum separation for these analytes was achieved in less than 10 min at 30 degrees C with a fused-silica capillary column (56 cm x 50 microm i.d.) and a 25mM borate buffer at pH 9.0 containing 25mM SDS and 10% (v/v) acetonitrile. The samples were injected hydrodynamically for 3 s at 50 mbar, and the applied voltage was +30.0 kV. Detection wavelength was set at 238 nm. Diflunisal was used as internal standard. The method was suitably validated with respect to stability, specificity, linearity, limits of detection and quantification, accuracy, precision, and robustness. The limits of detection and quantification were 1.0 and 2.0 microg/mL for both ezetimibe and simvastatin, respectively. The method developed was successfully applied to the simultaneous determination of ezetimibe and simvastatin in pharmaceutical preparations.

Preparation of candidate reference materials for the determination of phosphorus containing flame retardants in styrene-based polymers.

PubMed

Roth, Thomas; Urpi Bertran, Raquel; Latza, Andreas; Andörfer-Lang, Katrin; Hügelschäffer, Claudia; Pöhlein, Manfred; Puchta, Ralph; Placht, Christian; Maid, Harald; Bauer, Walter; van Eldik, Rudi

2015-04-01

Candidate reference materials (RM) for the analysis of phosphorus-based flame retardants in styrene-based polymers were prepared using a self-made mini-extruder. Due to legal requirements of the current restriction for the use of certain hazardous substances in electrical and electronic equipment, focus now is placed on phosphorus-based flame retardants instead of the brominated kind. Newly developed analytical methods for the first-mentioned substances also require RMs similar to industrial samples for validation and verification purposes. Hence, the prepared candidate RMs contained resorcinol-bis-(diphenyl phosphate), bisphenol A bis(diphenyl phosphate), triphenyl phosphate and triphenyl phosphine oxide as phosphorus-based flame retardants. Blends of polycarbonate and acrylonitrile-co-butadiene-co-styrene as well as blends of high-impact polystyrene and polyphenylene oxide were chosen as carrier polymers. Homogeneity and thermal stability of the candidate RMs were investigated. Results showed that the candidate RMs were comparable to the available industrial materials. Measurements by ICP/OES, FTIR and NMR confirmed the expected concentrations of the flame retardants and proved that analyte loss and degradation, respectively, was below the uncertainty of measurement during the extrusion process. Thus, the candidate RMs were found to be suitable for laboratory use.

[Various methods for the determination of preservatives in food. II. Gaschromatography, high performance liquid chromatography, TAS-method (author's transl)].

PubMed

Hild, J; Gertz, C

1980-02-01

For the quantitative determination of preservatives in food, analyses were carried out by means of GLC, HPLC, and TLC according to the TAS-method. Using the alkaline extract (sample preparation see part I) the preservatives can be analysed as free acid or appropriate ester out the same GLC-column without any interference from coextractives. A fast and accurate HPLC determination can be achieved by direct injection of the alkaline extract. All preservatives were well separated and detected at a wavelength of 225 resp. 232 nm. As a quick test for the qualitative estimation the TLC (TAS) method is suggested and a suitable solvent system is proposed.

Process for the separation and purification of yttrium-90 for medical applications

DOEpatents

Horwitz, P.E.; Dietz, M.L.

1994-11-29

An extraction chromatographic method for the preparation of [sup 90]Y of high chemical and radiochemical purity is disclosed. After an initial purification of a [sup 90]Sr stock solution and a suitable period of [sup 90]Y ingrowth, the solution is passed through a series of strontium-selective chromatographic columns, each of which lowers the [sup 90]Sr content of the mixture by a factor of about 10[sup 3]. The [sup 90]Y remaining is freed from any residual [sup 90]Sr, from its [sup 90]Zr daughter, and from any remaining impurities by passing the sample through a final column designed to selectively retain yttrium. 5 figures.

Characterization and Application of Passive Samplers for Monitoring of Pesticides in Water.

PubMed

Ahrens, Lutz; Daneshvar, Atlasi; Lau, Anna E; Kreuger, Jenny

2016-08-03

Five different water passive samplers were calibrated under laboratory conditions for measurement of 124 legacy and current used pesticides. This study provides a protocol for the passive sampler preparation, calibration, extraction method and instrumental analysis. Sampling rates (RS) and passive sampler-water partition coefficients (KPW) were calculated for silicone rubber, polar organic chemical integrative sampler POCIS-A, POCIS-B, SDB-RPS and C18 disk. The uptake of the selected compounds depended on their physicochemical properties, i.e., silicone rubber showed a better uptake for more hydrophobic compounds (log octanol-water partition coefficient (KOW) > 5.3), whereas POCIS-A, POCIS-B and SDB-RPS disk were more suitable for hydrophilic compounds (log KOW < 0.70).

A process for the separation and purification of yttrium-90 for medical applications

DOEpatents

Horwitz, P.E.; Dietz, M.L.

1993-01-01

An extraction chromatographic method for the preparation of {sup 90}Y of high chemical and radiochemical purity is disclosed. After an initial purification of a {sup 90}Sr stock solution and a suitable period of {sup 90}Y ingrowth, the solution is passed through a series of strontium-selective chromatographic columns, each of which lowers the {sup 90}Sr content of the mixture by a factor of about 10{sup 3}. The {sup 90}Y remaining is freed from any residual {sup 90}Sr, from its {sup 90}Zr daughter, and from any remaining impurities by passing the sample through a final column designed to selectively retain yttrium.

ChIP-seq and RNA-seq methods to study circadian control of transcription in mammals

PubMed Central

Takahashi, Joseph S.; Kumar, Vivek; Nakashe, Prachi; Koike, Nobuya; Huang, Hung-Chung; Green, Carla B.; Kim, Tae-Kyung

2015-01-01

Genome-wide analyses have revolutionized our ability to study the transcriptional regulation of circadian rhythms. The advent of next-generation sequencing methods has facilitated the use of two such technologies, ChIP-seq and RNA-seq. In this chapter, we describe detailed methods and protocols for these two techniques, with emphasis on their usage in circadian rhythm experiments in the mouse liver, a major target organ of the circadian clock system. Critical factors for these methods are highlighted and issues arising with time series samples for ChIP-seq and RNA-seq are discussed. Finally detailed protocols for library preparation suitable for Illumina sequencing platforms are presented. PMID:25662462

Process for the separation and purification of yttrium-90 for medical applications

DOEpatents

Horwitz, Philip E.; Dietz, Mark L.

1994-01-01

An extraction chromatographic method for the preparation of .sup.90 Y of high chemical and radiochemical purity is disclosed. After an initial purification of a .sup.90 Sr stock solution and a suitable period of .sup.90 Y ingrowth, the solution is passed through a series of strontium-selective chromatographic columns, each of which lowers the .sup.90 Sr content of the mixture by a factor of about 10.sup.3. The .sup.90 Y remaining is freed from any residual .sup.90 Sr, from its .sup.90 Zr daughter, and from any remaining impurities by passing the sample through a final column designed to selectively retain yttrium.

Preparation of Emulsifying Wax/GMO Nanoparticles and Evaluation as a Delivery System for Repurposing Simvastatin in Bone Regeneration.

PubMed

Eskinazi-Budge, Aaron; Manickavasagam, Dharani; Czech, Tori; Novak, Kimberly; Kunzler, James; Oyewumi, Moses O

2018-05-30

Simvastatin (Sim) is a widely known drug in the treatment of hyperlipidemia that has attracted so much attention in bone regeneration based on its potential osteoanabolic effect. However, repurposing of Sim in bone regeneration will require suitable delivery systems that can negate undesirable off-target/side effects. In this study, we have investigated a new lipid nanoparticle (NP) platform that was fabricated using a binary blend of emulsifying wax (Ewax) and glyceryl monooleate (GMO). Using the binary matrix materials, NPs loaded with Sim (0-500 µg/mL) were prepared and showed an average particle size of about 150 nm. NP size stability was dependent on Sim concentration loaded in NPs. The suitability of NPs prepared with the binary matrix materials in Sim delivery for potential application in bone regeneration was supported by biocompatibility in pre-osteoclastic and pre-osteoblastic cells. Additional data demonstrated that biofunctional Sim was released from NPs that facilitated differentiation of osteoblasts (cells that form bones) while inhibiting differentiation of osteoclasts (cells that resorb bones). The overall work demonstrated the preparation of NPs from Ewax/GMO blends and characterization to ascertain potential suitability in Sim delivery for bone regeneration. Additional studies on osteoblast and osteoclast functions are warranted to fully evaluate the efficacy simvastatin-loaded Ewax/GMO NPs using in-vitro and in-vivo approaches.

Pelletizing/reslurrying as a means of distributing and firing clean coal

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

Conkle, H.N.; Raghavan, J.K.; Smit, F.J.

1991-11-21

The objective of this study is to develop technology that permits the practical and economic preparation, storage, handling, and transportation of coal pellets, which can be reslurried into Coal water fuels (CWF) suitable for firing in small- and medium-size commercial and industrial boilers, furnaces, and engines. The project includes preparing coal pellets and capsules from wet filter cake that can be economically stored, handled, transported, and reslurried into a CWF that can be suitably atomized and fired at the user site. The wet cakes studied were prepared from ultra-fine (95% -325 mesh) coal beneficiated by advanced froth-flotation techniques. The coalsmore » studied included two eastern bituminous coals, one from Virginia (Elkhorn) and one from Illinois (Illinois No. 6) and one western bituminous coal from Utah (Sky Line coal).« less

Choosing suitable times for prescribed burning in southern New Jersey

Treesearch

S. Little; H. A. Somes; J. P. Allen

1952-01-01

Prescribed burning is useful in managing pine-oak forests in the Pine Region of southern New Jersey. It favors reproduction of pine by preparing suitable seed beds; it checks the development of hardwood reproduction; and it protects against wild fires by reducing the amount of fuel on the forest floor.

An approach for land suitability evaluation using geostatistics, remote sensing, and geographic information system in arid and semiarid ecosystems.

PubMed

Emadi, Mostafa; Baghernejad, Majid; Pakparvar, Mojtaba; Kowsar, Sayyed Ahang

2010-05-01

This study was undertaken to incorporate geostatistics, remote sensing, and geographic information system (GIS) technologies to improve the qualitative land suitability assessment in arid and semiarid ecosystems of Arsanjan plain, southern Iran. The primary data were obtained from 85 soil samples collected from tree depths (0-30, 30-60, and 60-90 cm); the secondary information was acquired from the remotely sensed data from the linear imaging self-scanner (LISS-III) receiver of the IRS-P6 satellite. Ordinary kriging and simple kriging with varying local means (SKVLM) methods were used to identify the spatial dependency of soil important parameters. It was observed that using the data collected from the spectral values of band 1 of the LISS-III receiver as the secondary variable applying the SKVLM method resulted in the lowest mean square error for mapping the pH and electrical conductivity (ECe) in the 0-30-cm depth. On the other hand, the ordinary kriging method resulted in a reliable accuracy for the other soil properties with moderate to strong spatial dependency in the study area for interpolation in the unstamped points. The parametric land suitability evaluation method was applied on the density points (150 x 150 m(2)) instead of applying on the limited representative profiles conventionally, which were obtained by the kriging or SKVLM methods. Overlaying the information layers of the data was used with the GIS for preparing the final land suitability evaluation. Therefore, changes in land characteristics could be identified in the same soil uniform mapping units over a very short distance. In general, this new method can easily present the squares and limitation factors of the different land suitability classes with considerable accuracy in arbitrary land indices.

21 CFR 606.122 - Circular of information.

Code of Federal Regulations, 2014 CFR

2014-04-01

... collecting the Whole Blood from each product is prepared. (e) A statement that the product was prepared from... and administration recommendations. (j) [Reserved] (k) For Red Blood Cells, the circular of information must contain: (1) Instructions to administer a suitable plasma volume expander if Red Blood Cells...

Isotope Inversion Experiment evaluating the suitability of calibration in surrogate matrix for quantification via LC-MS/MS-Exemplary application for a steroid multi-method.

PubMed

Suhr, Anna Catharina; Vogeser, Michael; Grimm, Stefanie H

2016-05-30

For quotable quantitative analysis of endogenous analytes in complex biological samples by isotope dilution LC-MS/MS, the creation of appropriate calibrators is a challenge, since analyte-free authentic material is in general not available. Thus, surrogate matrices are often used to prepare calibrators and controls. However, currently employed validation protocols do not include specific experiments to verify the suitability of a surrogate matrix calibration for quantification of authentic matrix samples. The aim of the study was the development of a novel validation experiment to test whether surrogate matrix based calibrators enable correct quantification of authentic matrix samples. The key element of the novel validation experiment is the inversion of nonlabelled analytes and their stable isotope labelled (SIL) counterparts in respect to their functions, i.e. SIL compound is the analyte and nonlabelled substance is employed as internal standard. As a consequence, both surrogate and authentic matrix are analyte-free regarding SIL analytes, which allows a comparison of both matrices. We called this approach Isotope Inversion Experiment. As figure of merit we defined the accuracy of inverse quality controls in authentic matrix quantified by means of a surrogate matrix calibration curve. As a proof-of-concept application a LC-MS/MS assay addressing six corticosteroids (cortisol, cortisone, corticosterone, 11-deoxycortisol, 11-deoxycorticosterone, and 17-OH-progesterone) was chosen. The integration of the Isotope Inversion Experiment in the validation protocol for the steroid assay was successfully realized. The accuracy results of the inverse quality controls were all in all very satisfying. As a consequence the suitability of a surrogate matrix calibration for quantification of the targeted steroids in human serum as authentic matrix could be successfully demonstrated. The Isotope Inversion Experiment fills a gap in the validation process for LC-MS/MS assays quantifying endogenous analytes. We consider it a valuable and convenient tool to evaluate the correct quantification of authentic matrix samples based on a calibration curve in surrogate matrix. Copyright © 2016 Elsevier B.V. All rights reserved.

CRISPR/Cas9 Technology-Based Xenograft Tumors as Candidate Reference Materials for Multiple EML4-ALK Rearrangements Testing.

PubMed

Peng, Rongxue; Zhang, Rui; Lin, Guigao; Yang, Xin; Li, Ziyang; Zhang, Kuo; Zhang, Jiawei; Li, Jinming

2017-09-01

The echinoderm microtubule-associated protein-like 4 and anaplastic lymphoma kinase (ALK) receptor tyrosine kinase (EML4-ALK) rearrangement is an important biomarker that plays a pivotal role in therapeutic decision making for non-small-cell lung cancer (NSCLC) patients. Ensuring accuracy and reproducibility of EML4-ALK testing by fluorescence in situ hybridization, immunohistochemistry, RT-PCR, and next-generation sequencing requires reliable reference materials for monitoring assay sensitivity and specificity. Herein, we developed novel reference materials for various kinds of EML4-ALK testing. CRISPR/Cas9 was used to edit various NSCLC cell lines containing EML4-ALK rearrangement variants 1, 2, and 3a/b. After s.c. inoculation, the formalin-fixed, paraffin-embedded (FFPE) samples from xenografts were prepared and tested for suitability as candidate reference materials by fluorescence in situ hybridization, immunohistochemistry, RT-PCR, and next-generation sequencing. Sample validation and commutability assessments showed that all types of FFPE samples derived from xenograft tumors have typical histological structures, and EML4-ALK testing results were similar to the clinical ALK-positive NSCLC specimens. Among the four methods for EML4-ALK detection, the validation test showed 100% concordance. Furthermore, these novel FFPE reference materials showed good stability and homogeneity. Without limitations on variant types and production, our novel FFPE samples based on CRISPR/Cas9 editing and xenografts are suitable as candidate reference materials for the validation, verification, internal quality control, and proficiency testing of EML4-ALK detection. Copyright © 2017 American Society for Investigative Pathology and the Association for Molecular Pathology. Published by Elsevier Inc. All rights reserved.

Development and optimization of SPE-HPLC-UV/ELSD for simultaneous determination of nine bioactive components in Shenqi Fuzheng Injection based on Quality by Design principles.

PubMed

Wang, Lu; Qu, Haibin

2016-03-01

A method combining solid phase extraction, high performance liquid chromatography, and ultraviolet/evaporative light scattering detection (SPE-HPLC-UV/ELSD) was developed according to Quality by Design (QbD) principles and used to assay nine bioactive compounds within a botanical drug, Shenqi Fuzheng Injection. Risk assessment and a Plackett-Burman design were utilized to evaluate the impact of 11 factors on the resolutions and signal-to-noise of chromatographic peaks. Multiple regression and Pareto ranking analysis indicated that the sorbent mass, sample volume, flow rate, column temperature, evaporator temperature, and gas flow rate were statistically significant (p < 0.05) in this procedure. Furthermore, a Box-Behnken design combined with response surface analysis was employed to study the relationships between the quality of SPE-HPLC-UV/ELSD analysis and four significant factors, i.e., flow rate, column temperature, evaporator temperature, and gas flow rate. An analytical design space of SPE-HPLC-UV/ELSD was then constructed by calculated Monte Carlo probability. In the presented approach, the operating parameters of sample preparation, chromatographic separation, and compound detection were investigated simultaneously. Eight terms of method validation, i.e., system-suitability tests, method robustness/ruggedness, sensitivity, precision, repeatability, linearity, accuracy, and stability, were accomplished at a selected working point. These results revealed that the QbD principles were suitable in the development of analytical procedures for samples in complex matrices. Meanwhile, the analytical quality and method robustness were validated by the analytical design space. The presented strategy provides a tutorial on the development of a robust QbD-compliant quantitative method for samples in complex matrices.

A novel ion-exclusion chromatography-mass spectrometry method to measure concentrations and cycling rates of carbohydrates and amino sugars in freshwaters.

PubMed

Horňák, Karel; Pernthaler, Jakob

2014-10-24

The concentrations of free neutral carbohydrates and amino sugars were determined in freshwater samples of distinct matrix complexity, including meso-, eu- and dystrophic lakes and ponds, using high-performance ion-exclusion chromatography (HPIEC) coupled to mass spectrometry (MS). In contrast to other methods, our approach allowed the quantification of free neutral carbohydrates and amino sugars at low nM concentrations without derivatization, de-salting or pre-concentration. New sample preparation procedures were applied prior to injection employing syringe and hollow fiber filtration. Analytes were separated on a strong cation exchange resin under 100% aqueous conditions using 0.1% formic acid as a mobile phase. To minimize background noise in MS, analytes were detected in a multiple reaction monitoring scan mode with double ion filtering. Detection limits of carbohydrates and amino sugars ranged between 0.2 and 2nM at a signal-to-noise ratio >5. Error ranged between 1 and 12% at 0.5-500nM levels. Using a stable isotope dilution approach, both the utilization and recycling of glucose in Lake Zurich was observed. In contrast, N-acetyl-glucosamine was equally rapidly consumed but there was no visible de novo production. The simple and rapid sample preparation makes our protocol suitable for routine analyses of organic compounds in freshwater samples. Application of stable isotope tracers along with accurate measures of carbohydrate and amino sugar concentrations enables novel insights into the compound in situ dynamics. Copyright © 2014 Elsevier B.V. All rights reserved.

Multiresidue Method for Quantification of Sulfonamides and Trimethoprim in Tilapia Fillet by Liquid Chromatography Coupled to Quadrupole Time-of-Flight Mass Spectrometry Using QuEChERS for Sample Preparation.

PubMed

Nunes, Kátia S D; Assalin, Márcia R; Vallim, José H; Jonsson, Claudio M; Queiroz, Sonia C N; Reyes, Felix G R

2018-01-01

A multiresidue method for detecting and quantifying sulfonamides (sulfapyridine, sulfamerazine, sulfathiazole, sulfamethazine, sulfadimethoxine, sulfamethoxazole, and sulfamethoxypyridazine) and trimethoprim in tilapia fillet ( Oreochromis niloticus ) using liquid chromatography coupled to mass spectrometry was developed and validated. The sample preparation was optimized using the QuEChERS approach. The chromatographic separation was performed using a C18 column and 0.1% formic acid in water and acetonitrile as the mobile phase in the isocratic elution mode. Method validation was performed based on the Commission Decision 2002/657/EC and Brazilian guideline. The validation parameters evaluated were linearity ( r  ≥ 0.99); limits of detection (LOD) and quantification (LOQ), 1 ng·g -1 and 5 ng·g -1 , respectively; intraday and interdays precision (CV lower than 19.4%). The decision limit (CC α 102.6-120.0 ng·g -1 and 70 ng·g -1 for sulfonamides and trimethoprim, respectively) and detection capability (CC β 111.7-140.1 ng·g -1 and 89.9 ng·g -1 for sulfonamides and trimethoprim, respectively) were determined. Analyses of tilapia fillet samples from fish exposed to sulfamethazine through feed (incurred samples) were conducted in order to evaluate the method. This new method was demonstrated to be fast, sensitive, and suitable for monitoring sulfonamides and trimethoprim in tilapia fillet in health surveillance programs, as well as to be used in pharmacokinetics and residue depletion studies.

A novel combined thermometric and amperometric biosensor for lactose determination based on immobilised cellobiose dehydrogenase.

PubMed

Yakovleva, Maria; Buzas, Orsolya; Matsumura, Hirotoshi; Samejima, Masahiro; Igarashi, Kiyohiko; Larsson, Per-Olof; Gorton, Lo; Danielsson, Bengt

2012-01-15

A novel method for lactose determination in milk is proposed. It is based on oxidation of lactose by cellobiose dehydrogenase (CDH) from the basidiomycete Phanerochaete chrysosporium, immobilised in an enzyme reactor. The reactor was prepared by cross-linking CDH onto aminopropyl-silanised controlled pore glass (CPG) beads using glutaraldehyde. The combined biosensor worked in flow injection analysis (FIA) mode and was developed for simultaneous monitoring of the thermometric signal associated with the enzymatic oxidation of lactose using p-benzoquinone as electron acceptor and the electrochemically generated current associated with the oxidation of the hydroquinone formed. A highly reproducible linear response for lactose was obtained between 0.05 mM and 30 mM. For a set of more than 500 samples an R.S.D. of less than 10% was achieved. The assay time was ca. 2 min per sample. The sensor was applied for the determination of lactose in dairy milk samples (milk with a fat content of 1.5% or 3% and also "lactose free" milk). No sample preparation except dilution with buffer was needed. The proposed method is rapid, suitable for repeated use and allows the possibility to compare results from two different detection methods, thus providing a built-in quality assurance. Some differences in the response observed between the methods indicate that the dual approach can be useful in mechanistic studies of redox enzymes. In addition, a dual system opens up interesting possibilities for studies of enzyme properties and mechanisms. Copyright © 2011 Elsevier B.V. All rights reserved.

Multiresidue Method for Quantification of Sulfonamides and Trimethoprim in Tilapia Fillet by Liquid Chromatography Coupled to Quadrupole Time-of-Flight Mass Spectrometry Using QuEChERS for Sample Preparation

PubMed Central

Nunes, Kátia S. D.; Assalin, Márcia R.; Vallim, José H.; Jonsson, Claudio M.; Queiroz, Sonia C. N.

2018-01-01

A multiresidue method for detecting and quantifying sulfonamides (sulfapyridine, sulfamerazine, sulfathiazole, sulfamethazine, sulfadimethoxine, sulfamethoxazole, and sulfamethoxypyridazine) and trimethoprim in tilapia fillet (Oreochromis niloticus) using liquid chromatography coupled to mass spectrometry was developed and validated. The sample preparation was optimized using the QuEChERS approach. The chromatographic separation was performed using a C18 column and 0.1% formic acid in water and acetonitrile as the mobile phase in the isocratic elution mode. Method validation was performed based on the Commission Decision 2002/657/EC and Brazilian guideline. The validation parameters evaluated were linearity (r ≥ 0.99); limits of detection (LOD) and quantification (LOQ), 1 ng·g−1 and 5 ng·g−1, respectively; intraday and interdays precision (CV lower than 19.4%). The decision limit (CCα 102.6–120.0 ng·g−1 and 70 ng·g−1 for sulfonamides and trimethoprim, respectively) and detection capability (CCβ 111.7–140.1 ng·g−1 and 89.9 ng·g−1 for sulfonamides and trimethoprim, respectively) were determined. Analyses of tilapia fillet samples from fish exposed to sulfamethazine through feed (incurred samples) were conducted in order to evaluate the method. This new method was demonstrated to be fast, sensitive, and suitable for monitoring sulfonamides and trimethoprim in tilapia fillet in health surveillance programs, as well as to be used in pharmacokinetics and residue depletion studies. PMID:29686929

Fluorimetric detection of Sn(2+) ion in aqueous medium using Salicylaldehyde based nanoparticles and application to natural samples analysis.

PubMed

Patil, Kishor S; Mahajan, Prasad G; Patil, Shivajirao R

2017-01-05

The fluorescent 2-[(E)-(2-phenylhydrazinylidene)methyl]phenol nanoparticles (PHPNPs) were prepared by a simple reprecipitation method. The prepared PHPNPs examined by Dynamic Light Scattering show narrower particle size distribution having an average particle size of 93.3nm. The Scanning Electron Microphotograph shows distinct spherical shaped morphology of nanoparticles. The blue shift in UV-absorption and fluorescence spectra of PHPNPs with respect to corresponding spectra of PHP in acetone solution indicates H- aggregates and Aggregation Induced Enhanced Emission (AIEE) for nanoparticles. The nanoparticles show selective tendency towards the recognition of Sn(2+) ions by enhancing the fluorescence intensity preference to Cu(2+), Fe(3+), Fe(2+), Ni(2+), NH4(+), Ca(2+), Pb(2+), Hg(2+) and Zn(2+) ions, which actually seem to quench the fluorescence of nanoparticles. The studies on Langmuir adsorption plot, fluorescence lifetime of PHPNPs, DLS-Zeta sizer, UV-visible and fluorescence titration with and without Sn(2+) helped to propose a suitable mechanism of fluorescence enhancement of nanoparticles by Sn(2+) and their binding ability during complexation. The fluorescence enhancement effect of PHPNPs induced by Sn(2+) is further used to develop an analytical method for detection of Sn(2+) from aqueous medium in environmental samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Fluorimetric detection of Sn2 + ion in aqueous medium using Salicylaldehyde based nanoparticles and application to natural samples analysis

NASA Astrophysics Data System (ADS)

Patil, Kishor S.; Mahajan, Prasad G.; Patil, Shivajirao R.

2017-01-01

The fluorescent 2-[(E)-(2-phenylhydrazinylidene)methyl]phenol nanoparticles (PHPNPs) were prepared by a simple reprecipitation method. The prepared PHPNPs examined by Dynamic Light Scattering show narrower particle size distribution having an average particle size of 93.3 nm. The Scanning Electron Microphotograph shows distinct spherical shaped morphology of nanoparticles. The blue shift in UV-absorption and fluorescence spectra of PHPNPs with respect to corresponding spectra of PHP in acetone solution indicates H- aggregates and Aggregation Induced Enhanced Emission (AIEE) for nanoparticles. The nanoparticles show selective tendency towards the recognition of Sn2 + ions by enhancing the fluorescence intensity preference to Cu2 +, Fe3 +, Fe2 +, Ni2 +, NH4+, Ca2 +, Pb2 +, Hg2 + and Zn2 + ions, which actually seem to quench the fluorescence of nanoparticles. The studies on Langmuir adsorption plot, fluorescence lifetime of PHPNPs, DLS-Zeta sizer, UV-visible and fluorescence titration with and without Sn2 + helped to propose a suitable mechanism of fluorescence enhancement of nanoparticles by Sn2 + and their binding ability during complexation. The fluorescence enhancement effect of PHPNPs induced by Sn2 + is further used to develop an analytical method for detection of Sn2 + from aqueous medium in environmental samples.

Selective detection of Co2+ by fluorescent nano probe: Diagnostic approach for analysis of environmental samples and biological activities

NASA Astrophysics Data System (ADS)

Mahajan, Prasad G.; Dige, Nilam C.; Desai, Netaji K.; Patil, Shivajirao R.; Kondalkar, Vijay V.; Hong, Seong-Karp; Lee, Ki Hwan

2018-06-01

Nowadays scientist over the world are engaging to put forth improved methods to detect metal ion in an aqueous medium based on fluorescence studies. A simple, selective and sensitive method was proposed for detection of Co2+ ion using fluorescent organic nanoparticles. We synthesized a fluorescent small molecule viz. 4,4‧-{benzene-1,4-diylbis-[(Z)methylylidenenitrilo]}dibenzoic acid (BMBA) to explore its suitability as sensor for Co2+ ion and biocompatibility in form of nanoparticles. Fluorescence nanoparticles (BMBANPs) prepared by simple reprecipitation method. Aggregation induced enhanced emission of BMBANPs exhibits the narrower particle size of 68 nm and sphere shape morphology. The selective fluorescence quenching was observed by addition of Co2+ and does not affected by presence of other coexisting ion solutions. The photo-physical properties, viz. UV-absorption, fluorescence emission, and lifetime measurements are in support of ligand-metal interaction followed by static fluorescence quenching phenomenon in emission of BMBANPs. Finally, we develop a simple analytical method for selective and sensitive determination of Co2+ ion in environmental samples. The cell culture E. coli, Bacillus sps., and M. tuberculosis H37RV strain in the vicinity of BMBANPs indicates virtuous anti-bacterial and anti-tuberculosis activity which is of additional novel application shown by prepared nanoparticles.

Validation of high-throughput measurement system with microwave-assisted extraction, fully automated sample preparation device, and gas chromatography-electron capture detector for determination of polychlorinated biphenyls in whale blubber.

PubMed

Fujita, Hiroyuki; Honda, Katsuhisa; Hamada, Noriaki; Yasunaga, Genta; Fujise, Yoshihiro

2009-02-01

Validation of a high-throughput measurement system with microwave-assisted extraction (MAE), fully automated sample preparation device (SPD), and gas chromatography-electron capture detector (GC-ECD) for the determination of polychlorinated biphenyls (PCBs) in minke whale blubber was performed. PCB congeners accounting for > 95% of the total PCBs burden in blubber were efficiently extracted with a small volume (20 mL) of n-hexane using MAE due to simultaneous saponification and extraction. Further, the crude extract obtained by MAE was rapidly purified and automatically substituted to a small volume (1 mL) of toluene using SPD without using concentrators. Furthermore, the concentration of PCBs in the purified and concentrated solution was accurately determined by GC-ECD. Moreover, the result of accuracy test using a certified material (SRM 1588b; Cod liver oil) showed good agreement with the NIST certified concentration values. In addition, the method quantification limit of total-PCB in whale blubbers was 41 ng g(-1). This new measurement system for PCBs takes only four hours. Consequently, it indicated this method is the most suitable for the monitoring and screening of PCBs in the conservation of the marine ecosystem and safe distribution of foods.

Site-Specific Preparation of Intact Solid–Liquid Interfaces by Label-Free In Situ Localization and Cryo-Focused Ion Beam Lift-Out

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

Zachman, Michael J.; Asenath-Smith, Emily; Estroff, Lara A.

Abstract Scanning transmission electron microscopy (STEM) allows atomic scale characterization of solid–solid interfaces, but has seen limited applications to solid–liquid interfaces due to the volatility of liquids in the microscope vacuum. Although cryo-electron microscopy is routinely used to characterize hydrated samples stabilized by rapid freezing, sample thinning is required to access the internal interfaces of thicker specimens. Here, we adapt cryo-focused ion beam (FIB) “lift-out,” a technique recently developed for biological specimens, to prepare intact internal solid–liquid interfaces for high-resolution structural and chemical analysis by cryo-STEM. To guide the milling process we introduce a label-freein situmethod of localizing subsurface structuresmore » in suitable materials by energy dispersive X-ray spectroscopy (EDX). Monte Carlo simulations are performed to evaluate the depth-probing capability of the technique, and show good qualitative agreement with experiment. We also detail procedures to produce homogeneously thin lamellae, which enable nanoscale structural, elemental, and chemical analysis of intact solid–liquid interfaces by analytical cryo-STEM. This work demonstrates the potential of cryo-FIB lift-out and cryo-STEM for understanding physical and chemical processes at solid–liquid interfaces.« less

Some characteristics of matrix-assisted UV laser desorption/ionization mass spectrometric analysis of large proteins

NASA Astrophysics Data System (ADS)

Perera, I. K.; Kantartzoglou, S.; Dyer, P. E.

1996-12-01

We have performed experiments to explore the characteristics of the matrix-assisted laser desorption/ionization (MALDI) process and to ascertain optimal operational conditions for observing intact molecular ions of large proteins. In this study, several methods have been adopted for the preparation of analyte samples. Of these, the samples prepared with the simple dried-droplet method were found to be the most suitable for the generation of the large molecular clusters, while the near-uniform spin-coated samples were observed to produce highly reproducible molecular ion signals of relatively high mass resolutions. A resulting mass spectrum which illustrates the formation of cluster ions up to the 26-mer [26M+H]+ of bovine insulin corresponding to a mass of about 150,000 Da, is presented. The effect of fluence on the extent of clustering of protein molecules has been studied, the results revealing the existence of an optimum fluence for detecting the large cluster ions. Investigations have also indicated that the use of polyethylene-coated metallic substrates as sample supports can considerably reduce the fragmentation of the matrix/analyte molecular ions and the desorption of "neat" MALDI matrices deposited on these polyethylene-coated sample probes enhance their aggregation, forming up to the heptamer [7M+H]+ of the matrix, ferulic acid. The dependence of the mass resolution on the applied acceleration voltage and the desorption fluence has been examined and the results obtained are discussed in terms of a simple analysis of the linear time-of-flight mass spectrometer. A spectrum of chicken egg lysozyme (M~14,306) displaying the high mass resolutions (M/[Delta]M~690) that can be attained when the mass spectrometer is operated in the reflectron mode is also presented.

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).

Comparison of hard tissues that are useful for DNA analysis in forensic autopsy.

PubMed

Kaneko, Yu; Ohira, Hiroshi; Tsuda, Yukio; Yamada, Yoshihiro

2015-11-01

Forensic analysis of DNA from hard tissues can be important when investigating a variety of cases resulting from mass disaster or criminal cases. This study was conducted to evaluate the most suitable tissues, method and sample size for processing of hard tissues prior to DNA isolation. We also evaluated the elapsed time after death in relation to the quantity of DNA extracted. Samples of hard tissues (37 teeth, 42 skull, 42 rib, and 39 nails) from 42 individuals aged between 50 and 83 years were used. The samples were taken from remains following forensic autopsy (from 2 days to 2 years after death). To evaluate the integrity of the nuclear DNA isolated, the percentage of allele calls for short tandem repeat profiles were compared between the hard tissues. DNA typing results indicated that until 1 month after death, any of the four hard tissue samples could be used as an alternative to teeth, allowing analysis of all of the loci. However, in terms of the sampling site, collection method and sample size adjustment, the rib appeared to be the best choice in view of the ease of specimen preparation. Our data suggest that the rib could be an alternative hard tissue sample for DNA analysis of human remains. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

Ultrapure glass optical waveguide development in microgravity by the sol-gel process

NASA Technical Reports Server (NTRS)

Mukherjee, S. P.

1980-01-01

The alkali-borosilicate system was selected as the glass system for the preparation of ultrapure low loss glasses suitable for optical communication. The effect of different oxide contents on the absorption loss was critically reviewed. One composition was chosen to develop the gel preparation procedure in the alkali-borosilicate system. In addition, several procedures for the preparation of gels based on two different approaches were developed. The influence of different preparation parameters were investigated qualitatively. Several conclusions are drawn from the results.

Development and validation of an ultra-performance liquid chromatography quadrupole time of flight mass spectrometry method for rapid quantification of free amino acids in human urine.

PubMed

Joyce, Richard; Kuziene, Viktorija; Zou, Xin; Wang, Xueting; Pullen, Frank; Loo, Ruey Leng

2016-01-01

An ultra-performance liquid chromatography quadrupole time of flight mass spectrometry (UPLC-qTOF-MS) method using hydrophilic interaction liquid chromatography was developed and validated for simultaneous quantification of 18 free amino acids in urine with a total acquisition time including the column re-equilibration of less than 18 min per sample. This method involves simple sample preparation steps which consisted of 15 times dilution with acetonitrile to give a final composition of 25 % aqueous and 75 % acetonitrile without the need of any derivatization. The dynamic range for our calibration curve is approximately two orders of magnitude (120-fold from the lowest calibration curve point) with good linearity (r (2) ≥ 0.995 for all amino acids). Good separation of all amino acids as well as good intra- and inter-day accuracy (<15 %) and precision (<15 %) were observed using three quality control samples at a concentration of low, medium and high range of the calibration curve. The limits of detection (LOD) and lower limit of quantification of our method were ranging from approximately 1-300 nM and 0.01-0.5 µM, respectively. The stability of amino acids in the prepared urine samples was found to be stable for 72 h at 4 °C, after one freeze thaw cycle and for up to 4 weeks at -80 °C. We have applied this method to quantify the content of 18 free amino acids in 646 urine samples from a dietary intervention study. We were able to quantify all 18 free amino acids in these urine samples, if they were present at a level above the LOD. We found our method to be reproducible (accuracy and precision were typically <10 % for QCL, QCM and QCH) and the relatively high sample throughput nature of this method potentially makes it a suitable alternative for the analysis of urine samples in clinical setting.

A Sensitive DNA Capacitive Biosensor Using Interdigitated Electrodes

PubMed Central

Wang, Lei; Veselinovic, Milena; Yang, Lang; Geiss, Brian J.; Dandy, David S.; Chen, Tom

2017-01-01

This paper presents a label-free affinity-based capacitive biosensor using interdigitated electrodes. Using an optimized process of DNA probe preparation to minimize the effect of contaminants in commercial thiolated DNA probe, the electrode surface was functionalized with the 24-nucleotide DNA probes based on the West Nile virus sequence (Kunjin strain). The biosensor has the ability to detect complementary DNA fragments with a detection limit down to 20 DNA target molecules (1.5 aM range), making it suitable for a practical point-of-care (POC) platform for low target count clinical applications without the need for amplification. The reproducibility of the biosensor detection was improved with efficient covalent immobilization of purified single-stranded DNA probe oligomers on cleaned gold microelectrodes. In addition to the low detection limit, the biosensor showed a dynamic range of detection from 1 μL−1 to 105 μL−1 target molecules (20 to 2 million targets), making it suitable for sample analysis in a typical clinical application environment. The binding results presented in this paper were validated using fluorescent oligomers. PMID:27619528

Plastic fats from sal, mango and palm oil by lipase catalyzed interesterification.

PubMed

Shankar Shetty, Umesha; Sunki Reddy, Yella Reddy; Khatoon, Sakina

2014-02-01

Speciality plastic fats with no trans fatty acids suitable for use in bakery and as vanaspati substitute were prepared by interesterification of blends of palm stearin (PSt) with sal and mango fats using Lipozyme TLIM lipase as catalyst. The blends containing PSt/sal or PSt/mango showed short melting range and hence are not suitable as bakery shortenings. Lipase catalysed interesterification extended the plasticity or melting range of all the blends. The blends containing higher proportion of PSt with sal fat (50/50) were harder having high solids at and above body temperature and hence cannot be used as bakery shortenings. The blends with PSt/sal (30-40/60-70) after interesterification showed melting profiles similar to those of commercial hydrogenated bakery fats. Similarly, the blends containing PSt/mango (30-40/60-70) after interesterification also showed melting profiles similar to those of commercial hydrogenated shortenings. The slip melting point and solidification characteristics also confirm the plastic nature of these samples. The improvement in plasticity after interesterification is due to formation of higher melting as well as lower melting triglycerides during lipase catalysed interesterification.

Detection of IL-6 by magnetic nanoparticles grown with the assistance of mid-infrared lighting.

PubMed

Jiang, Xiufeng; Zhang, Ye; Miao, Xiaofei; Li, Zenghui; Bao, Zengtao; Wang, Tong

2013-01-01

Nanomedical systems have attracted considerable attention primarily due to suitability in applications for specific cell selection through biomolecular targeting and rare cell detection enhancement in a diverse, multicellular population. In the present study, magnetic nanoparticles were prepared for use in high accuracy cell sensing. Magnetic nanoparticle growth was assisted by mid-infrared lighting. By this mechanism, a narrow window, estimated to be 2%, was achieved for the dimension distribution of grown nanoparticles. Combined with silicon nanowire (SiNW) transistors, a sensor with ultra high sensitivity for the detection of specific potential low abundance biomarkers has been achieved, which has been specifically used to detect interleukin-6 (IL-6) at extremely low concentrations. A novel biosensor with high sensitivity has been fabricated and utilized in the detection of IL-6 at 75 fM to 50 pM. The system consists of an SiNW transistor and magnetic nanoparticles with even dimension distribution. The novel sensor system is suitable for quantifying IL-6 at low concentrations in protein samples.

Materials for storage and release of hydrogen and methods for preparing and using same

DOEpatents

Autrey, Thomas S [West Richland, WA; Gutowska, Anna [Richland, WA; Shin, Yongsoon [Richland, WA; Li, Liyu [Richland, WA

2008-01-08

The invention relates to materials for storing and releasing hydrogen and methods for preparing and using same. The materials exhibit fast release rates at low release temperatures and are suitable as fuel and/or hydrogen sources for a variety of applications such as automobile engines.

Preparation of Conducting Polymers by Electrochemical Methods and Demonstration of a Polymer Battery

ERIC Educational Resources Information Center

Goto, Hiromasa; Yoneyama, Hiroyuki; Togashi, Fumihiro; Ohta, Reina; Tsujimoto, Akitsu; Kita, Eiji; Ohshima, Ken-ichi

2008-01-01

The electrochemical polymerization of aniline and pyrrole, and demonstrations of electrochromism and the polymer battery effect, are presented as demonstrations suitable for high school and introductory chemistry at the university level. These demonstrations promote student interest in the electrochemical preparation of conducting polymers, where…

A Paradigm for EST Materials Preparation.

ERIC Educational Resources Information Center

Carreon, Edwina S.; Balarbar, Corazon V.

In many countries, suitable English for special purposes (ESP) textbooks and materials are difficult to find. ESP teachers and program coordinators often must develop their own materials, but preparing such materials requires training. One model that has served as a guide to numerous ESP materials projects is the Hutchinson and Waters' model. This…

Improving a Lecture-Size Molecular Model Set by Repurposing Used Whiteboard Markers

ERIC Educational Resources Information Center

Dragojlovic, Veljko

2015-01-01

Preparation of an inexpensive model set from whiteboard markers and either HGS molecular model set or atoms made of wood is described. The model set is relatively easy to prepare and is sufficiently large to be suitable as an instructor set for use in lectures.

Leonardite char adsorbents

DOEpatents

Knudson, Curtis L.

1993-01-01

A process of preparing lignite (low rank) coal filter material, suitable for use in lieu of more expensive activated carbon filter materials, is disclosed. The process comprises size reducing Leonardite coal material to a suitable filtering effective size, and thereafter heating the size reduced Leonardite preferably to at least 750.degree. C. in the presence of a flow of an inert gas.

Leonardite char adsorbents

DOEpatents

Knudson, C.L.

1993-10-19

A process of preparing lignite (low rank) coal filter material, suitable for use in lieu of more expensive activated carbon filter materials, is disclosed. The process comprises size reducing Leonardite coal material to a suitable filtering effective size, and thereafter heating the size reduced Leonardite preferably to at least 750 C in the presence of a flow of an inert gas. 1 figure.

Comparative study of a novel application of automated HR HPV assay and stability in a previously untested Preservative media.

PubMed

Morel, Mike E; McBride, Simon E; Gomez, Maria P

2017-12-01

The suitability and stability of cervical cells in Novaprep media (NHQ) for certain HPV assays is unknown. We evaluated the accuracy of an automated HPV assay (Abbott RealTime HR HPV) for cervical cells prepared in NHQ and NHQ with a pre-treatment to mimic a worst case clinical use, compared to the assay manufacturers media; repeatability and reproducibility of HPV results and the stability of detectable HPV in NHQ over time compared to CE marked liquid based cytology preservatives. Cell lines were used to simulate patient samples. Cells stored in NHQ produced accurate, repeatable and reproducible results. Stability in NHQ was comparable to the best performing LBC, with at least 7 months' stability at 18-25°C, 2-8°C, -20°C and -80°C; and at least 3 months' stability at 40°C. Similar results were obtained for pre-treated NHQ except only 3.5 months' stability at 18-25°C. Cell line samples in all media and concentrations tested were detected appropriately by the assay. Based on this first stage validation analytical study, cervical cells stored in NHQ are suitable for the Realtime HPV assay. There should be no reservations for inclusion of NHQ in any further validation and clinical performance evaluation of this assay. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

Preparation and characterization of PTFE coating in new polymer quartz piezoelectric crystal sensor for testing liquor products

NASA Astrophysics Data System (ADS)

Gu, Yu; Li, Qiang

2015-07-01

A new method was developed based on the electron beam vacuum dispersion (EBVD) technology to prepare the PTFE polymer coating of the new polymer quartz piezoelectric crystal sensor for testing liquor products. The new method was applied in the new EBVD equipment which we designed. A real-time system monitoring the polymer coating’s thickness was designed for the new EBVD equipment according to the quartz crystal microbalance (QCM) principle, playing an important role in preparing stable and uniform PTFE polymer coatings of the same thickness. 30 pieces of PTFE polymer coatings on the surface of the quartz crystal basis were prepared with the PTFE polymer ultrafine powder (purity ≥ 99.99%) as the starting material. We obtained 30 pieces of new PTFE polymer sensors. By using scanning electron microscopy (SEM), the structure of the PTFE polymer coating’s column clusters was studied. One sample from the 30 pieces of new PTFE polymer sensors was analysed by SEM in four scales, i.e., 400×, 1000×, 10000×, and 25000×. It was shown that under the condition of high bias voltage and low bias current, uniformly PTFE polymer coating could be achieved, which indicates that the new EBVD equipment is suitable for mass production of stable and uniform polymer coating. Project supported by the National High Technology Research and Development Program of China (Grant No. 2013AA030901).

In vivo evaluation of titanium-prepared platelet-rich fibrin (T-PRF): a new platelet concentrate.

PubMed

Tunalı, Mustafa; Özdemir, Hakan; Küçükodacı, Zafer; Akman, Serhan; Fıratlı, Erhan

2013-07-01

We have developed a new, titanium-prepared, platelet-rich fibrin (T-PRF) together with the protocol for forming it, which is based on the hypothesis that titanium tubes may be more effective at activating platelets than the glass tubes used by Chouckroun in his platelet-rich fibrin (PRF) method. The aim of this study was to find a suitable animal model in which to evaluate the method and to investigate the efficacy of T-PRF for wound healing. Blood samples from 6 rabbits were used to confirm the protocol for formation of T-PRF. We evaluated T-PRF or T-PRF-like clots morphologically using scanning electron microscopy (EM). Blood samples from 5 rabbits were used to develop an experiment in which to evaluate the effects of T-PRF on wound healing. The mucoperiosteal flaps were filled with autologous T-PRF membranes from the vestibule in the anterior mandibular regions. Samples collected from the surgical sites were stained with haematoxylin and eosin. We found a mature fibrin network in T-PRF clots that had been centrifuged for 15 min at 3500 rpm and, 15 days after placement of the membrane, we found newly-forming connective tissue and islets of bony tissue in the T-PRF membrane. These results show that T-PRF could induce the formation of new bone with new connective tissue in a rabbit model of wound healing within 30 days of treatment. Published by Elsevier Ltd.

Single hair analysis of small molecules using MALDI-triple quadrupole MS imaging and LC-MS/MS: investigations on opportunities and pitfalls.

PubMed

Poetzsch, Michael; Steuer, Andrea E; Roemmelt, Andreas T; Baumgartner, Markus R; Kraemer, Thomas

2014-12-02

Single hair analysis normally requires extensive sample preparation microscale protocols including time-consuming steps like segmentation and extraction. Matrix assisted laser desorption and ionization mass spectrometric imaging (MALDI-MSI) was shown to be an alternative tool in single hair analysis, but still, questions remain. Therefore, an investigation of MALDI-MSI in single hair analysis concerning the extraction process, usage of internal standard (IS), and influences on the ionization processes were systematically investigated to enable the reliable application to hair analysis. Furthermore, single dose detection, quantitative correlation to a single hair, and hair strand LC-MS/MS results were performed, and the performance was compared to LC-MS/MS single hair monitoring. The MALDI process was shown to be independent from natural hair color and not influenced by the presence of melanin. Ionization was shown to be reproducible along and in between different hair samples. MALDI image intensities in single hair and hair snippets showed good semiquantitative correlation to zolpidem hair concentrations obtained from validated routine LC-MS/MS methods. MALDI-MSI is superior to LC-MS/MS analysis when a fast, easy, and cheap sample preparation is necessary, whereas LC-MS/MS showed higher sensitivity with the ability of single dose detection for zolpidem. MALDI-MSI and LC-MS/MS segmental single hair analysis showed good correlation, and both are suitable for consumption monitoring of drugs of abuse with a high time resolution.

Application of mercapto-silica polymerized high internal phase emulsions for the solid-phase extraction and preconcentration of trace lead(II).

PubMed

Su, Rihui; Ruan, Guihua; Chen, Zhengyi; Du, Fuyou; Li, Jianping

2015-12-01

A new class of solid-phase extraction column prepared with grafted mercapto-silica polymerized high internal phase emulsion particles was used for the preconcentration of trace lead. First, mercapto-silica polymerized high internal phase emulsion particles were synthesized by using high internal phase emulsion polymerization and carefully assembled in a polyethylene syringe column. The influences of various parameters including adsorption pH value, adsorption and desorption solvents, flow rate of the adsorption and desorption procedure were optimized, respectively, and the suitable uploading sample volumes, adsorption capacity, and reusability of solid phase extraction column were also investigated. Under the optimum conditions, Pb(2+) could be preconcentrated quantitatively over a wide pH range (2.0-5.0). In the presence of foreign ions, such as Na(+) , K(+) , Ca(2+) , Zn(2+) , Mg(2+) , Cu(2+) , Fe(2+) , Cd(2+) , Cl(-) and NO3 (-) , Pb(2+) could be recovered successfully. The prepared solid-phase extraction column performed with high stability and desirable durability, which allowed more than 100 replicate extractions without measurable changes of performance. The feasibility of the developed method was further validated by the extraction of Pb(2+) in rice samples. At three spiked levels of 40.0, 200 and 800 μg/kg, the average recoveries for Pb(2+) in rice samples ranged from 87.3 to 105.2%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Highly transparent, flexible, and thermally stable superhydrophobic ORMOSIL aerogel thin films.

PubMed

Budunoglu, Hulya; Yildirim, Adem; Guler, Mustafa O; Bayindir, Mehmet

2011-02-01

We report preparation of highly transparent, flexible, and thermally stable superhydrophobic organically modified silica (ORMOSIL) aerogel thin films from colloidal dispersions at ambient conditions. The prepared dispersions are suitable for large area processing with ease of coating and being directly applicable without requiring any pre- or post-treatment on a variety of surfaces including glass, wood, and plastics. ORMOSIL films exhibit and retain superhydrophobic behavior up to 500 °C and even on bent flexible substrates. The surface of the films can be converted from superhydrophobic (contact angle of 179.9°) to superhydrophilic (contact angle of <5°) by calcination at high temperatures. The wettability of the coatings can be changed by tuning the calcination temperature and duration. The prepared films also exhibit low refractive index and high porosity making them suitable as multifunctional coatings for many application fields including solar cells, flexible electronics, and lab on papers.

Pelletizing/reslurrying as a means of distributing and firing clean coal. Final quarterly technical progress report No. 5, July 1, 1991--September 30, 1991

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

Conkle, H.N.; Raghavan, J.K.; Smit, F.J.

1991-11-21

The objective of this study is to develop technology that permits the practical and economic preparation, storage, handling, and transportation of coal pellets, which can be reslurried into Coal water fuels (CWF) suitable for firing in small- and medium-size commercial and industrial boilers, furnaces, and engines. The project includes preparing coal pellets and capsules from wet filter cake that can be economically stored, handled, transported, and reslurried into a CWF that can be suitably atomized and fired at the user site. The wet cakes studied were prepared from ultra-fine (95% -325 mesh) coal beneficiated by advanced froth-flotation techniques. The coalsmore » studied included two eastern bituminous coals, one from Virginia (Elkhorn) and one from Illinois (Illinois No. 6) and one western bituminous coal from Utah (Sky Line coal).« less

Evaluation of groundwater quality and its suitability for drinking and agricultural use in Thanjavur city, Tamil Nadu, India.

PubMed

Nagarajan, R; Rajmohan, N; Mahendran, U; Senthamilkumar, S

2010-12-01

As groundwater is a vital source of water for domestic and agricultural activities in Thanjavur city due to lack of surface water resources, groundwater quality and its suitability for drinking and agricultural usage were evaluated. In this study, 102 groundwater samples were collected from dug wells and bore wells during March 2008 and analyzed for pH, electrical conductivity, temperature, major ions, and nitrate. Results suggest that, in 90% of groundwater samples, sodium and chloride are predominant cation and anion, respectively, and NaCl and CaMgCl are major water types in the study area. The groundwater quality in the study site is impaired by surface contamination sources, mineral dissolution, ion exchange, and evaporation. Nitrate, chloride, and sulfate concentrations strongly express the impact of surface contamination sources such as agricultural and domestic activities, on groundwater quality, and 13% of samples have elevated nitrate content (>45 mg/l as NO(3)). PHREEQC code and Gibbs plots were employed to evaluate the contribution of mineral dissolution and suggest that mineral dissolution, especially carbonate minerals, regulates water chemistry. Groundwater suitability for drinking usage was evaluated by the World Health Organization and Indian standards and suggests that 34% of samples are not suitable for drinking. Integrated groundwater suitability map for drinking purposes was created using drinking water standards based on a concept that if the groundwater sample exceeds any one of the standards, it is not suitable for drinking. This map illustrates that wells in zones 1, 2, 3, and 4 are not fit for drinking purpose. Likewise, irrigational suitability of groundwater in the study region was evaluated, and results suggest that 20% samples are not fit for irrigation. Groundwater suitability map for irrigation was also produced based on salinity and sodium hazards and denotes that wells mostly situated in zones 2 and 3 are not suitable for irrigation. Both integrated suitability maps for drinking and irrigation usage provide overall scenario about the groundwater quality in the study area. Finally, the study concluded that groundwater quality is impaired by man-made activities, and proper management plan is necessary to protect valuable groundwater resources in Thanjavur city.

Optical biosensor technologies for molecular diagnostics at the point-of-care

NASA Astrophysics Data System (ADS)

Schotter, Joerg; Schrittwieser, Stefan; Muellner, Paul; Melnik, Eva; Hainberger, Rainer; Koppitsch, Guenther; Schrank, Franz; Soulantika, Katerina; Lentijo-Mozo, Sergio; Pelaz, Beatriz; Parak, Wolfgang; Ludwig, Frank; Dieckhoff, Jan

2015-05-01

Label-free optical schemes for molecular biosensing hold a strong promise for point-of-care applications in medical research and diagnostics. Apart from diagnostic requirements in terms of sensitivity, specificity, and multiplexing capability, also other aspects such as ease of use and manufacturability have to be considered in order to pave the way to a practical implementation. We present integrated optical waveguide as well as magnetic nanoparticle based molecular biosensor concepts that address these aspects. The integrated optical waveguide devices are based on low-loss photonic wires made of silicon nitride deposited by a CMOS compatible plasma-enhanced chemical vapor deposition (PECVD) process that allows for backend integration of waveguides on optoelectronic CMOS chips. The molecular detection principle relies on evanescent wave sensing in the 0.85 μm wavelength regime by means of Mach-Zehnder interferometers, which enables on-chip integration of silicon photodiodes and, thus, the realization of system-on-chip solutions. Our nanoparticle-based approach is based on optical observation of the dynamic response of functionalized magneticcore/ noble-metal-shell nanorods (`nanoprobes') to an externally applied time-varying magnetic field. As target molecules specifically bind to the surface of the nanoprobes, the observed dynamics of the nanoprobes changes, and the concentration of target molecules in the sample solution can be quantified. This approach is suitable for dynamic real-time measurements and only requires minimal sample preparation, thus presenting a highly promising point-of-care diagnostic system. In this paper, we present a prototype of a diagnostic device suitable for highly automated sample analysis by our nanoparticle-based approach.

Validation of the Filovirus Plaque Assay for Use in Preclinical Studies

PubMed Central

Shurtleff, Amy C.; Bloomfield, Holly A.; Mort, Shannon; Orr, Steven A.; Audet, Brian; Whitaker, Thomas; Richards, Michelle J.; Bavari, Sina

2016-01-01

A plaque assay for quantitating filoviruses in virus stocks, prepared viral challenge inocula and samples from research animals has recently been fully characterized and standardized for use across multiple institutions performing Biosafety Level 4 (BSL-4) studies. After standardization studies were completed, Good Laboratory Practices (GLP)-compliant plaque assay method validation studies to demonstrate suitability for reliable and reproducible measurement of the Marburg Virus Angola (MARV) variant and Ebola Virus Kikwit (EBOV) variant commenced at the United States Army Medical Research Institute of Infectious Diseases (USAMRIID). The validation parameters tested included accuracy, precision, linearity, robustness, stability of the virus stocks and system suitability. The MARV and EBOV assays were confirmed to be accurate to ±0.5 log10 PFU/mL. Repeatability precision, intermediate precision and reproducibility precision were sufficient to return viral titers with a coefficient of variation (%CV) of ≤30%, deemed acceptable variation for a cell-based bioassay. Intraclass correlation statistical techniques for the evaluation of the assay’s precision when the same plaques were quantitated by two analysts returned values passing the acceptance criteria, indicating high agreement between analysts. The assay was shown to be accurate and specific when run on Nonhuman Primates (NHP) serum and plasma samples diluted in plaque assay medium, with negligible matrix effects. Virus stocks demonstrated stability for freeze-thaw cycles typical of normal usage during assay retests. The results demonstrated that the EBOV and MARV plaque assays are accurate, precise and robust for filovirus titration in samples associated with the performance of GLP animal model studies. PMID:27110807

MALDI-based intact spore mass spectrometry of downy and powdery mildews.

PubMed

Chalupová, Jana; Sedlářová, Michaela; Helmel, Michaela; Rehulka, Pavel; Marchetti-Deschmann, Martina; Allmaier, Günter; Sebela, Marek

2012-08-01

Fast and easy identification of fungal phytopathogens is of great importance in agriculture. In this context, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) has emerged as a powerful tool for analyzing microorganisms. This study deals with a methodology for MALDI-TOF MS-based identification of downy and powdery mildews representing obligate biotrophic parasites of crop plants. Experimental approaches for the MS analyses were optimized using Bremia lactucae, cause of lettuce downy mildew, and Oidium neolycopersici, cause of tomato powdery mildew. This involved determining a suitable concentration of spores in the sample, selection of a proper MALDI matrix, looking for the optimal solvent composition, and evaluation of different sample preparation methods. Furthermore, using different MALDI target materials and surfaces (stainless steel vs polymer-based) and applying various conditions for sample exposure to the acidic MALDI matrix system were investigated. The dried droplet method involving solvent evaporation at room temperature was found to be the most suitable for the deposition of spores and MALDI matrix on the target and the subsequent crystallization. The concentration of spore suspension was optimal between 2 and 5 × 10(9) spores per ml. The best peptide/protein profiles (in terms of signal-to-noise ratio and number of peaks) were obtained by combining ferulic and sinapinic acids as a mixed MALDI matrix. A pretreatment of the spore cell wall with hydrolases was successfully introduced prior to MS measurements to obtain more pronounced signals. Finally, a novel procedure was developed for direct mass spectra acquisition from infected plant leaves. Copyright © 2012 John Wiley & Sons, Ltd.

7 CFR 91.19 - General requirements of suitable samples.

Code of Federal Regulations, 2011 CFR

2011-01-01

... the analyses requested. (b) Each sample must be identified with the following information: (1) Product... other information which is required by the specific program under which analysis or test is performed. ... LABORATORY TESTING PROGRAMS SERVICES AND GENERAL INFORMATION Samples § 91.19 General requirements of suitable...

7 CFR 91.19 - General requirements of suitable samples.

Code of Federal Regulations, 2012 CFR

2012-01-01

... the analyses requested. (b) Each sample must be identified with the following information: (1) Product... other information which is required by the specific program under which analysis or test is performed. ... LABORATORY TESTING PROGRAMS SERVICES AND GENERAL INFORMATION Samples § 91.19 General requirements of suitable...

7 CFR 91.19 - General requirements of suitable samples.

Code of Federal Regulations, 2013 CFR

2013-01-01

... the analyses requested. (b) Each sample must be identified with the following information: (1) Product... other information which is required by the specific program under which analysis or test is performed. ... LABORATORY TESTING PROGRAMS SERVICES AND GENERAL INFORMATION Samples § 91.19 General requirements of suitable...

7 CFR 91.19 - General requirements of suitable samples.

Code of Federal Regulations, 2010 CFR

2010-01-01

... the analyses requested. (b) Each sample must be identified with the following information: (1) Product... other information which is required by the specific program under which analysis or test is performed. ... LABORATORY TESTING PROGRAMS SERVICES AND GENERAL INFORMATION Samples § 91.19 General requirements of suitable...

7 CFR 91.19 - General requirements of suitable samples.

Code of Federal Regulations, 2014 CFR

2014-01-01

... the analyses requested. (b) Each sample must be identified with the following information: (1) Product... other information which is required by the specific program under which analysis or test is performed. ... LABORATORY TESTING PROGRAMS SERVICES AND GENERAL INFORMATION Samples § 91.19 General requirements of suitable...

Development and evaluation of a collection apparatus for recoil products for study of the deexcitation process of (235m)U.

PubMed

Shigekawa, Y; Kasamatsu, Y; Shinohara, A

2016-05-01

The nucleus (235m)U is an isomer with extremely low excitation energy (76.8 eV) and decays dominantly through the internal conversion (IC) process. Because outer-shell electrons are involved in the IC process, the decay constant of (235m)U depends on its chemical environment. We plan to study the deexcitation process of (235m)U by measuring the energy spectra of IC electrons in addition to the decay constants for various chemical forms. In this paper, the preparation method of (235m)U samples from (239)Pu by using alpha-recoil energy is reported. A Collection Apparatus for Recoil Products was fabricated, and then collection efficiencies under various conditions were determined by collecting (224)Ra recoiling out of (228)Th electrodeposited and precipitated sources. The pressure in the apparatus (vacuum or 1 atm of N2 gas) affected the variations of the collection efficiencies depending on the negative voltage applied to the collector. The maximum values of the collection efficiencies were mainly affected by the thickness of the (228)Th sources. From these results, the suitable conditions of the (239)Pu sources for preparation of (235m)U were determined. In addition, dissolution efficiencies were determined by washing collected (224)Ra with solutions. When (224)Ra was collected in 1 atm of N2 gas and dissolved with polar solutions such as water, the dissolution efficiencies were nearly 100%. The method of rapid dissolution of recoil products would be applicable to rapid preparation of short-lived (235m)U samples for various chemical forms.

The reaction pathway of membrane-bound rat liver mitochondrial monoamine oxidase

PubMed Central

Houslay, Miles D.; Tipton, Keith F.

1973-01-01

1. A preparation of a partly purified mitochondrial outer-membrane fraction suitable for kinetic investigations of monoamine oxidase is described. 2. An apparatus suitable for varying the O2 concentration in a spectrophotometer cuvette is described. 3. The reaction catalysed by the membrane-bound enzyme is shown to proceed by a double-displacement (Ping Pong) mechanism, and a formal mechanism is proposed. 4. KCN, NaN3, benzyl cyanide and 4-cyanophenol are shown to be reversible inhibitors of the enzyme. 5. The non-linear reciprocal plot obtained with impure preparations of benzylamine, which is typical of high substrate inhibition, is shown to be due to aldehyde contamination of the substrate. PMID:4778271

Adaptation of micro-diffusion method for the analysis of (15) N natural abundance of ammonium in samples with small volume.

PubMed

Zhang, Shasha; Fang, Yunting; Xi, Dan

2015-07-30

There are several preparation methods for the measurement of the nitrogen (N) isotopic composition of ammonium (NH4 (+) ) in different types of samples (freshwater, saltwater and soil extracts). The diffusion method is the most popular and it involves NH4 (+) in solutions being released under alkaline conditions and then immediately trapped by an acidified filter. However, the traditional preparation is designed for samples with large volume and relatively high N concentrations. The performance of diffusion for small-volume samples (e.g., a few milliliters) remains unknown. We examined the overall performance of micro-diffusion on 5 mL samples on varying the incubation time, temperature and initial NH4 (+) concentration. The trapped ammonia was chemically converted into nitrous oxide (N2 O) with hypobromite and hydroxylamine in sequence. The produced N2 O was analyzed by a commercially available purge and cryogenic trap system coupled to an isotope ratio mass spectrometer. We found that diffusion can be complete with no more than 7 days of treatment at 37 °C. Increasing the temperature to 50 °C and the incubation time to 11 days did not improve the overall performance. There were no significant differences in the overall performance during diffusion with NH4 (+) concentrations from 15 to 60 μM. The blank size was relatively large, and the N contamination might come from the reagents especially KCl salts. The method presented here combines micro-diffusion and hypobromite oxidation and hydroxylamine reduction. It is suitable for samples with small volume and low NH4 (+) concentrations. Our study demonstrates that the NH4 (+) concentrations in samples can be as low as 15 μM, and a volume of 5 mL is sufficient for this method. We suggest that this method can be used for the routine determination of (15) N/(14) N for either natural abundance or (15) N-enriched NH4 (+) . Copyright © 2015 John Wiley & Sons, Ltd.

Method for preparing actinide nitrides

DOEpatents

Bryan, G.H.; Cleveland, J.M.; Heiple, C.R.

1975-12-01

Actinide nitrides, and particularly plutonium and uranium nitrides, are prepared by reacting an ammonia solution of an actinide compound with an ammonia solution of a reactant or reductant metal, to form finely divided actinide nitride precipitate which may then be appropriately separated from the solution. The actinide nitride precipitate is particularly suitable for forming nuclear fuels.

Equation typing: Guidelines for Mass-11 users and others

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

Jackson, C.L.

1989-06-01

A number of problems have been experienced by Sandia secretaries and others in the preparation of equations. This report is a self- paced/''how-to'' manual designed to provide detailed explanations on the preparation of equations using Mass-11 and the typewriter and is suitable for either classroom training or on-the-job use.

38 CFR 61.80 - General operation requirements for supportive housing and service centers.

Code of Federal Regulations, 2014 CFR

2014-07-01

... provided to permit use of essential electrical appliances while assuring safety from fire; (10) All food preparation areas must contain suitable space and equipment to store, prepare, and serve food in a sanitary... program's ability to provide a successful outcome for veterans. (7) Corrective Action(s): When necessary...

38 CFR 61.80 - General operation requirements for supportive housing and service centers.

Code of Federal Regulations, 2013 CFR

2013-07-01

... provided to permit use of essential electrical appliances while assuring safety from fire; (10) All food preparation areas must contain suitable space and equipment to store, prepare, and serve food in a sanitary... program's ability to provide a successful outcome for veterans. (7) Corrective Action(s): When necessary...

Isotopically pure magnesium isotope-24 is prepared from magnesium-24 oxide

NASA Technical Reports Server (NTRS)

Chellew, N. R.; Schilb, J. D.; Steunenberg, R. K.

1968-01-01

Apparatus is used to prepare isotopically pure magnesium isotope-24, suitable for use in neutron scattering and polarization experiments. The apparatus permits thermal reduction of magnesium-24 oxide with aluminum and calcium oxide, and subsequent vaporization of the product metal in vacuum. It uses a resistance-heated furnace tube and cap assembly.

Artemisinin nanoformulation suitable for intravenous injection: Preparation, characterization and antimalarial activities.

PubMed

Ibrahim, Nehal; Ibrahim, Hany; Sabater, Alicia Moreno; Mazier, Dominique; Valentin, Alexis; Nepveu, Françoise

2015-11-30

More than 40 years after its discovery, artemisinin has become the most promising antimalarial agent. However, no intravenous formulation is available due to its poor aqueous solubility. Here, we report the preparation, characterization, and in vitro and in vivo biological evaluation of biodegradable albumin-bound artemisinin nanoparticles. The nanoparticles were prepared by a combination of a bottom-up and a top-down processes and characterized by different spectroscopic techniques. The preparation process was optimized to develop a nanoformulation with the smallest possible diameter and good homogeneity suitable for intravenous injection enabling direct contact of artemisinin with infected erythrocytes. Chemically and physically stable artemisinin nanoparticles were obtained with excellent entrapment efficiency. In in vitro experiments, the artemisinin nanoformulation was interestingly more effective than non-formulated artemisinin. In Plasmodiumm falciparum-infected 'humanized' mice, the nanoparticles proved to be highly effective with 96% parasitemia inhibition at 10mg/kg/day, prolonging mean survival time without recrudescence. This nanoparticulate albumin-bound system allows the intravenous administration of artemisinin for the first time without harsh organic solvents or cosolvents with 100% bioavailability. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation and in vitro function of granulocyte concentrates for transfusion to neonates using the IBM 2991 blood processor.

PubMed

Goldfinger, D; Medici, M A; Hsi, R; McPherson, J; Connelly, M

1983-01-01

Clinical studies have suggested that granulocyte transfusions may be of value in the treatment of septic neonatal patients who present with severe granulocytopenia. We have developed a protocol for the preparation of granulocyte concentrates from freshly collected units of whole blood, using an automated blood cell processor. The red cells were washed with saline. Then, the buffy coats were collected from the washed red cells and studied for their suitability as granulocyte concentrates for neonatal transfusion. The mean number of granulocytes per concentrate was 1.6 X 10(9) in a mean volume of 25 ml. Studies of granulocyte function, including viability, random mobility, chemotaxis, phagocytosis and nitro-blue tetrazolium reduction, demonstrated that the granulocytes were functionally unimpaired following preparation of the concentrates. These studies suggest that concentrates of functional granulocytes, suitable for transfusion to neonatal patients, can be prepared from fresh units of whole blood, using a cell processor. This procedure is more cost-effective than leukapheresis and allows for delivery of granulocytes for transfusion in a more timely fashion.

Self-nanoemulsifying performance of two grades of Lauroglycol (Lauroglycol-90 and Lauroglycol-FCC) in the presence of mixed nonionic surfactants.

PubMed

Shakeel, Faiyaz; Haq, Nazrul; Alanazi, Fars K; Alsarra, Ibrahim A

2014-11-01

The present study was undertaken to evaluate the impact of various combinations of nonionic surfactants on self-nanoemulsifying performance of two grades of Lauroglycol (Lauroglycol-90 and Lauroglycol-FCC) in glibenclamide (GBN) nanoemulsion. Formulations (L1-L30) were prepared by spontaneous emulsification method. Prepared formulations were subjected to thermodynamic stability and self-nanoemulsification test. Results of thermodynamic stability and self-nanoemulsification tests were confirmed by further characterization of these formulations in terms of droplet size, viscosity, refractive index and % transmittance. Formulations prepared with Labrasol, HCO-60 and Gelucire-44/14 were found to be suitable for self-emulsifying drug delivery system only whereas those prepared with Tween-80 and Cremophor-EL were found to be suitable for self-nanoemulsifying or self-microemulsifying drug delivery system of GBN with respect to Lauroglycol-90 or Lauroglycol-FCC. Formulation L24 (Lauroglycol-FCC/Tween-80/ethanol/water) was optimized as best formulation for self-nanoemulsifying drug delivery system of GBN. These results indicated that Tween-80 could be the best surfactant in terms of self-nanoemulsification.

New radiocarbon measurement methods in the Hertelendi Laboratory, Hungary

NASA Astrophysics Data System (ADS)

Janovics, Róbert; Major, István; Rinyu, László; Veres, Mihály; Molnár, Mihály

2013-04-01

In this paper we present two very different and novel methods for C-14 measurement from dissolved inorganic carbonate (DIC) of water samples. A new LSC sample preparation method for liquid scintillation C-14 measurements was implemented in the ATOMKI. The first method uses direct absorption into a special absorbent (Carbosorb E®) and a following liquid scintillation measurement. Typical sample size is 20-40 litre of water. The developed CO2 absorption method is fast, and simple. The C-14 activities is measured by an ultra low background LSC (TRI-CARB 3170 TR/SL, Perkin Elmer) including quenching parameter (tSIE).The corresponding limit of C-14 dating is 31200 year. Several tests were executed with old borehole CO2 gas without significant content of C-14 and also performed on samples of known C-14 activities between 29 and 7000 pMC, previously measured by GPC. The combined uncertainty of the described determination is about 2 % in the case of recent carbon. It is a very cost-effective and easy to use method based on a novel and simple static absorption process for the CO2 extracted from groundwater. The other very sensitive method is based on accelerator mass spectrometry (AMS) using gas ion source. This method does not require graphite generation and a small volume of water sample (1-20mL) is enough for the radiocarbon measurement. The procedure is very similar to pre-treatment of carbonate contained sample preparation for stable isotope measurement with gasbench technique. We applied a MICADAS type accelerator mass spectrometry (AMS) with gas ion source for C-14 analysis. The radiocarbon content of water was sat free with phosphoric acid and then the headspace gas was rinsed vials. The whole measurement needs only 20 min of each sample. The precision of measurement is better than 1% for modern samples. The preparation is vastly reduced compared to the other AMS methods and principally allows fully automated measurements of groundwater samples with an auto-sampler. The presented two new methods can be suitable for C-14 measurements and dating of hydrological, and environmental samples as well. The new AMS facility in ATOMKI (Debrecen, Hungary) using an EnvironMICADAS AMS system with gas ion source has a great potential in groundwater C-14 analyses. The research was supported by the by TÁMOP-4.2.2.A-11/1/KONV and the Hungarian NSF (OTKA MB08-A 81515)

Astro Academy: Principia--Using Tracker to Analyse Experiments Undertaken by Tim Peake on the International Space Station

ERIC Educational Resources Information Center

Mobbs, Robin

2016-01-01

While on the International Space Station, Tim Peake undertook and recorded video files of experiments suitable for physics teaching coordinated by the National Space Academy. This article describes how the video of these experiments was prepared for use with tracking software. The tracking files of the videos are suitable for use by teachers or…

Polarographic study on the presence of antibiotics in food.

PubMed

Bottari, Emilio; Colombi, Massimiliano; De Bernardis, Chiara; Festa, Maria Rosa; Rampino, Vittorio

2018-07-01

EU and Italian laws dealing for the presence of antibiotics or, more in general, drags in food established limits for different kinds of food. Suitable rules exist about the medical treatment of cattle in relation to the production of milk and meat. The adoption of a procedure to check the respect of the law limits is necessary. In this paper, the presence of different classes of antibiotics in milk and in homogenised meat is investigated. Generally, HPLC methods are applied for this purpose. In this paper, the application of polarographic analysis is studied and the results are compared with the chromatographic ones. The comparison is relative to all the phases of analysis including the sample preparation. The results show the advantage of the proposed procedure.

MnFe2O4/CdSe magneto-fluorescent nanocomposite for possible biomedical applications

NASA Astrophysics Data System (ADS)

Chandunika, R. K.; Vijayaraghavan, R.; Sahu, Niroj Kumar

2018-04-01

Acombined superparamagnetic and fluorescent MnFe2O4/CdSe multifunctional nanocompositehas been prepared by suitable surface functionalizationswith citric acid, polyethyleneimine(PEI) and thioglycolic acid (ThA).and the samples were characterized by XRD, FT-IR, TEM, Zeta Potential, VSM, UV-Vis and PL spectroscopy. MnFe2O4 crystalizes with average size of 38.6 nm whereas CdSe with average size of 2.03 nm. In composite, the CdSe quantum dots (QD) are homogeneously distributed in the matrix of porous MnFe2O4 nanoparticles. Thenanocomposites are well dispersed in aqueous solvent and possess significant magnetic and luminescence properties which may be utilised for magnetic resonance imaging and luminescence tagging of biomolecules.

Development of europium doped BaSO4 TL OSL dual phosphor for radiation dosimetry applications

NASA Astrophysics Data System (ADS)

Patle, Anita; Patil, R. R.; Kulkarni, M. S.; Bhatt, B. C.; Moharil, S. V.

2015-08-01

This paper presents the results on the preparation and characterization of Europium-doped Barium sulfate (BaSO4: Eu) TL /OSL dual phosphor. The OSL sensitivity was found to be 11% of the commercially available Al2O3: C, using area integration method. The sample also shows good TL sensitivity and the dosimetric peak appears around 190°C with a shoulder at 282°C. After OSL readout, No change in the TL glow curve is observed. Since the observed TL peaks are not responsible for the observed OSL, good OSL as well as TL sensitivity and low fading will make this phosphor suitable for applications in radiation dosimetry using OSL as well as TL.

Normal and reverse flow injection–spectrophotometric determination of thiamine hydrochloride in pharmaceutical preparations using diazotized metoclopramide

PubMed Central

Al Abachi, Mouayed Q.; Hadi, Hind

2012-01-01

Simple and sensitive normal and reverse flow injection methods for spectrophotometric determination of thiamine hydrochloride (THC) at the microgram level were proposed and optimized. Both methods are based on the reaction between THC and diazotized metoclopramide in alkaline medium. Beer’s law was obeyed over the range of 10–300 and 2–90 μg/mL, the limits of detection were 2.118 and 0.839 μg/mL and the sampling rates were 80 and 95 injections per hour for normal and reverse flow injection methods respectively. The application of both methods to commercially available pharmaceuticals produced acceptable results. The flow system is suitable for application in quality control processes. PMID:29403765

Compositional control of continuously graded anode functional layer

NASA Astrophysics Data System (ADS)

McCoppin, J.; Barney, I.; Mukhopadhyay, S.; Miller, R.; Reitz, T.; Young, D.

2012-10-01

In this work, solid oxide fuel cells (SOFC's) are fabricated with linear-compositionally graded anode functional layers (CGAFL) using a computer-controlled compound aerosol deposition (CCAD) system. Cells with different CGAFL thicknesses (30 um and 50 um) are prepared with a continuous compositionally graded interface deposited between the electrolyte and anode support current collecting regions. The compositional profile was characterized using energy dispersive X-ray spectroscopic mapping. An analytical model of the compound aerosol deposition was developed. The model predicted compositional profiles for both samples that closely matched the measured profiles, suggesting that aerosol-based deposition methods are capable of creating functional gradation on length scales suitable for solid oxide fuel cell structures. The electrochemical performances of the two cells are analyzed using electrochemical impedance spectroscopy (EIS).

A combination dielectric and acoustic laboratory instrument for petrophysics

NASA Astrophysics Data System (ADS)

Josh, Matthew

2017-12-01

Laboratory testing of rock samples is the primary method for establishing the physics models which relate the rock properties (i.e. porosity, fluid permeability, pore-fluid and saturation) essential to evaluating a hydrocarbon reservoir, to the physical properties (resistivity, nuclear magnetic resonance, dielectric permittivity and acoustic properties) which can be measured with borehole logging instrumentation. Rock samples usually require machining to produce a suitable geometry for each test as well as specific sample preparation, e.g. multiple levels of saturation and chemical treatments, and this leads to discrepancies in the condition of the sample between different tests. Ideally, multiphysics testing should occur on one sample simultaneously so that useful correlations between data sets can be more firmly established. The world’s first dielectric and acoustic combination cell has been developed at CSIRO, so that a sample may be machined and prepared, then measured to determine the dielectric and acoustic properties simultaneously before atmospheric conditions in the laboratory affect the level of hydration in the sample. The dielectric measurement is performed using a conventional three-terminal parallel plate capacitor which can operate from 40 Hz up to 110 MHz, with modified electrodes incorporating a 4 MHz P-wave piezo crystal. Approximately 10 (acoustic P-) wavelengths interact with a typical (10 mm thick) sample so that the user may reliably ‘pick’ the P-wave arrival times with acceptable resolution. Experimental evidence indicates that the instrument is able to resolve 0.25 mm thickness in a Teflon sample test piece. For a number of engineering materials including Teflon and glass and also for a geological samples (Donnybrook sandstone from Western Australia) there is a perfectly linear relationship between both capacitance and P-wave arrival time with sample thickness. Donnybrook sandstone has a consistently linear increase in dielectric permittivity and P-wave velocity with saturation consistent with the Gassmann-Hill prediction. Both the dielectric permittivity and P-wave velocity are faster parallel to the bedding plane than orthogonal to the bedding plane in a shale from the Cooper Basin, Australia.

Influence of Cu-Cr substitution on structural, morphological, electrical and magnetic properties of magnesium ferrite

NASA Astrophysics Data System (ADS)

Yonatan Mulushoa, S.; Murali, N.; Tulu Wegayehu, M.; Margarette, S. J.; Samatha, K.

2018-03-01

Cu-Cr substituted magnesium ferrite materials (Mg1 - xCuxCrxFe21 - xO4 with x = 0.0-0.7) have been synthesized by the solid state reaction method. XRD analysis revealed the prepared samples are cubic spinel with single phase face centered cubic. A significant decrease of ∼41.15 nm in particle size is noted in response to the increase in Cu-Cr substitution level. The room temperature resistivity increases gradually from 0.553 × 105 Ω cm (x = 0.0) to 0.105 × 108 Ω cm (x = 0.7). Temperature dependent DC-electrical resistivity of all the samples, exhibits semiconductor like behavior. Cu-Cr doped materials can be suitable to limit the eddy current losses. VSM result shows pure and doped magnesium ferrite particles show soft ferrimagnetic nature at room temperature. The saturation magnetization of the samples decreases initially from 34.5214 emu/g for x = 0.0 to 18.98 emu/g (x = 0.7). Saturation magnetization, remanence and coercivity are decreased with doping, which may be due to the increase in grain size.

The OSIRIS-REx Mission Sample Site Selection Process

NASA Astrophysics Data System (ADS)

Beshore, Edward C.; Lauretta, Dante

2014-11-01

In September of 2016, the OSIRIS-REx (Origins, Spectral Interpretation, Resource Identification, Security, REgolith eXplorer) spacecraft will depart for asteroid (101955) Bennu, and in doing so, will turn an important corner in the exploration of the solar system. After arriving at Bennu in the fall of 2018, OSIRIS-REx will undertake a program of observations designed to select a site suitable for retrieving a sample that will be returned to the Earth in 2023. The third mission in NASA’s New Frontiers program, OSIRIS-REx will return over 60 grams from Bennu’s surface.OSIRIS-REx is unique because the science team will have an operational role to play in preparing data products needed to select a sample site. These include products used to ensure flight system safety — topographic maps and shape models, temperature measurements, maps of hazards — as well as assessments of sampleability and science value. The timing and production of these will be presented, as will the high-level decision-making tools and processes for the interim and final site selection processes.

The analysis of carbohydrates in milk powder by a new "heart-cutting" two-dimensional liquid chromatography method.

PubMed

Ma, Jing; Hou, Xiaofang; Zhang, Bing; Wang, Yunan; He, Langchong

2014-03-01

In this study, a new"heart-cutting" two-dimensional liquid chromatography method for the simultaneous determination of carbohydrate contents in milk powder was presented. In this two dimensional liquid chromatography system, a Venusil XBP-C4 analysis column was used in the first dimension ((1)D) as a pre-separation column, a ZORBAX carbohydrates analysis column was used in the second dimension ((2)D) as a final-analysis column. The whole process was completed in less than 35min without a particular sample preparation procedure. The capability of the new two dimensional HPLC method was demonstrated in the determination of carbohydrates in various brands of milk powder samples. A conventional one dimensional chromatography method was also proposed. The two proposed methods were both validated in terms of linearity, limits of detection, accuracy and precision. The comparison between the results obtained with the two methods showed that the new and completely automated two dimensional liquid chromatography method is more suitable for milk powder sample because of its online cleanup effect involved. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

A bio-material: mechanical behaviour of LDPE-Al2O3-TiO2

NASA Astrophysics Data System (ADS)

Dhabale, R.; Jatti, V. S.

2016-09-01

Polymer composites are prominent candidate for polymeric bio-composites due to its low cost, high strength and ease of manufacturing. However, they suffer from low mechanical properties such as high wear rate and low hardness. In view of this, present study focuses on the synthesis of hybrid bio polymer matrix composites using low density polyethylene as matrix material with reinforcing material namely, alumina and titanium oxide. The samples were fabricated as per ASTM standard by varying the percentage of reinforcing particles using injection moulding machine. Various tests namely, tensile, flexural, impact, hardness, wear, SEM and corrosion were conducted on the prepared samples. On the basis of the experimental results, it can be concluded that injection moulding process can fabricate defect free cast samples. Polymer matrix composites of 70%LDPE +10% TiO2 +20% Al2O3 composition is biocompatible and a good candidate for biomaterial. Thus based on the inference of this study the above polymer matrix composite is suitable for orthopaedic applications and can be applied on hard and soft tissues of implantable materials in a human body.

Bacterial Contamination into Ready-to-Eat Foods Sold in Middle Thailand.

PubMed

Ananchaipattana, Chiraporn; Bari, Md Latiful; Inatsu, Yasuhiro

2016-01-01

　Bacterial contamination in ready-to-eat (RTE) foods prepared and sold by small businesses in middle Thailand was surveyed. The 135 samples were randomly purchased from open markets and supermarkets in Bangkok and Pathum Thani provinces during May 2013 to February 2015. The results indicated that the rate of contamination in cooked pork, chicken meat and cooked aquatic items were 13/39 (33%), 18/45 (40%) and 14/57 (25%), respectively and the rate of bacterial contamination of collected samples from open market and supermarket were 26/67 (39%) and 19/68 (27%), respectively. Therefore, no statistically significant difference of contamination rate between two kinds of market or among three categories of food. The most contaminated pathogenic bacteria was Staphylococcus aureus 27/135 (20%) while that of Salmonella spp. was the lowest 5/135 (4%) in each categories of collected food samples. Implementation of suitable hygienic practices in the small food businesses are thought to be required to reduce the risk of foodborne illnesses caused by the consumption of RTE foods sold in middle Thailand.

Gas chromatographic determination of polycyclic aromatic hydrocarbons in water and smoked rice samples after solid-phase microextraction using multiwalled carbon nanotube loaded hollow fiber.

PubMed

Matin, Amir Abbas; Biparva, Pourya; Gheshlaghi, Mohammad

2014-12-29

A novel solid-phase microextraction fiber was prepared based on multiwalled carbon nanotubes (MWCNTs) loaded on hollow fiber membrane pores. Stainless steel wire was used as unbreakable support. The major advantages of the proposed fiber are its (a) high reproducibility due to the uniform structure of the hollow fiber membranes, (b) high extraction capacity related to the porous structure of the hollow fiber and outstanding adsorptive characteristics of MWCNTs. The proposed fiber was applied for the microextraction of five representative polycyclic aromatic hydrocarbons (PAHs) from aqueous media (river and hubble-bubble water) and smoked rice samples followed by gas chromatographic determination. Analytical merits of the method, including high correlation coefficients [(0.9963-0.9992) and (0.9982-0.9999)] and low detection limits [(9.0-13.0ngL(-1)) and (40.0-150.0ngkg(-1))] for water and rice samples, respectively, made the proposed method suitable for the ultra-trace determination of PAHs. Copyright © 2014 Elsevier B.V. All rights reserved.

Fractal diffusion in high temperature polymer electrolyte fuel cell membranes

NASA Astrophysics Data System (ADS)

Hopfenmüller, Bernhard; Zorn, Reiner; Holderer, Olaf; Ivanova, Oxana; Lehnert, Werner; Lüke, Wiebke; Ehlers, Georg; Jalarvo, Niina; Schneider, Gerald J.; Monkenbusch, Michael; Richter, Dieter

2018-05-01

The performance of fuel cells depends largely on the proton diffusion in the proton conducting membrane, the core of a fuel cell. High temperature polymer electrolyte fuel cells are based on a polymer membrane swollen with phosphoric acid as the electrolyte, where proton conduction takes place. We studied the proton diffusion in such membranes with neutron scattering techniques which are especially sensitive to the proton contribution. Time of flight spectroscopy and backscattering spectroscopy have been combined to cover a broad dynamic range. In order to selectively observe the diffusion of protons potentially contributing to the ion conductivity, two samples were prepared, where in one of the samples the phosphoric acid was used with hydrogen replaced by deuterium. The scattering data from the two samples were subtracted in a suitable way after measurement. Thereby subdiffusive behavior of the proton diffusion has been observed and interpreted in terms of a model of fractal diffusion. For this purpose, a scattering function for fractal diffusion has been developed. The fractal diffusion dimension dw and the Hausdorff dimension df have been determined on the length scales covered in the neutron scattering experiments.

Monitoring of the microbiota profile in nukadoko, a naturally fermented rice bran bed for pickling vegetables.

PubMed

Ono, Hiroshi; Nishio, Shoko; Tsurii, Jun; Kawamoto, Tetsuhiro; Sonomoto, Kenji; Nakayama, Jiro

2014-11-01

Nukadoko is a fermented rice bran mash traditionally used for pickling vegetables in Japan. To date, the production of both homemade and commercial nukadoko depends on natural fermentation without using starter cultures. Here, we monitored chemical and microbiological changes in the initial batch fermentation of nukadoko. Nukadoko samples were prepared by spontaneous fermentation of four different brands of rice bran, and microbiome dynamics were analyzed for 2 months. In the first week, non-Lactobacillales lactic acid bacteria (LAB) species, which differed among the samples, grew proportionally to pH decrease and lactate increase. Thereafter, Lactobacillus plantarum started growing and consumed residual sugars, causing further lactate increase in nukadoko. Finally, microbial communities in all tested nukadoko samples were dominated by L. plantarum. Taken together, our results suggest that the mixture of the fast-growing LAB species and slow-growing L. plantarum may be used as a suitable starter culture to promote the initial fermentation of nukadoko. Copyright © 2014 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

Evaluation of metal ion absorptive characteristics of three types of plastic sample bags used for pecipitation sampling

USGS Publications Warehouse

Good, A.B.; Schroder, L.J.

1984-01-01

Simulated precipitation samples containing 16 metal ions were prepared at 4 pH values. Absorptive characteristics of polypropylene, polyethylene, and polyester/polyolefin sacks were evaluated at pH 3.5, 4.0, 4.5, and 5.0. Simulated precipitation was in contact with the sacks for 17 days, and subsamples were removed for chemical analysis at 3, 7, 10, 14, and 17 days after initial contact. All three types of plastic sacks absorbed Fe throughout the entire pH range. Polypropylene and polyethylene absorbed Pb throughout the entire pH range; polyester/polyolefin sacks absorbed Pb at pH 4.0 or greater. All plastic sacks also absorbed Cu, Mo, and V at pH 4.5 and 5.0. Leaching the plastic sacks with 0.7 percent HNO3 did not result in 100 percent of Cu, Fe, Pb, and V. These sacks would be suitable collection vessels for Ba, Be, Ca, Cd, Co, Li, Mg, Mn, Na Sr and Zn in precipitation through the pH range of 3.5 to 5.0.

Visible-blind ultraviolet photodetectors on porous silicon carbide substrates

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

Naderi, N.; Hashim, M.R., E-mail: roslan@usm.my

2013-06-01

Highlights: • Highly reliable UV detectors are fabricated on porous silicon carbide substrates. • The optical properties of samples are enhanced by increasing the current density. • The optimized sample exhibits enhanced sensitivity to the incident UV radiation. - Abstract: Highly reliable visible-blind ultraviolet (UV) photodetectors were successfully fabricated on porous silicon carbide (PSC) substrates. High responsivity and high photoconductive gain were observed in a metal–semiconductor–metal ultraviolet photodetector that was fabricated on an optimized PSC substrate. The PSC samples were prepared via the UV-assisted photo-electrochemical etching of an n-type hexagonal silicon carbide (6H-SiC) substrate using different etching current densities. Themore » optical results showed that the current density is an outstanding etching parameter that controls the porosity and uniformity of PSC substrates. A highly porous substrate was synthesized using a suitable etching current density to enhance its light absorption, thereby improving the sensitivity of UV detector with this substrate. The electrical characteristics of fabricated devices on optimized PSC substrates exhibited enhanced sensitivity and responsivity to the incident radiation.« less

LC-MS based analysis of endogenous steroid hormones in human hair.

PubMed

Gao, Wei; Kirschbaum, Clemens; Grass, Juliane; Stalder, Tobias

2016-09-01

The quantification of endogenous steroid hormone concentrations in hair is increasingly used as a method for obtaining retrospective information on long-term integrated hormone exposure. Several different analytical procedures have been employed for hair steroid analysis, with liquid chromatography-mass spectrometry (LC-MS) being recognized as a particularly powerful analytical tool. Several methodological aspects affect the performance of LC-MS systems for hair steroid analysis, including sample preparation and pretreatment, steroid extraction, post-incubation purification, LC methodology, ionization techniques and MS specifications. Here, we critically review the differential value of such protocol variants for hair steroid hormones analysis, focusing on both analytical quality and practical feasibility issues. Our results show that, when methodological challenges are adequately addressed, LC-MS protocols can not only yield excellent sensitivity and specificity but are also characterized by relatively simple sample processing and short run times. This makes LC-MS based hair steroid protocols particularly suitable as a high-quality option for routine application in research contexts requiring the processing of larger numbers of samples. Copyright © 2016 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.

Determination of Carbonyl Compounds in Cork Agglomerates by GDME-HPLC-UV: Identification of the Extracted Compounds by HPLC-MS/MS.

PubMed

Brandão, Pedro Francisco; Ramos, Rui Miguel; Almeida, Paulo Joaquim; Rodrigues, José António

2017-02-08

A new approach is proposed for the extraction and determination of carbonyl compounds in solid samples, such as wood or cork materials. Cork products are used as building materials due to their singular characteristics; however, little is known about its aldehyde emission potential and content. Sample preparation was done by using a gas-diffusion microextraction (GDME) device for the direct extraction of volatile aldehydes and derivatization with 2,4-dinitrophenylhydrazine. Analytical determination of the extracts was done by HPLC-UV, with detection at 360 nm. The developed methodology proved to be a reliable tool for aldehyde determination in cork agglomerate samples with suitable method features. Mass spectrometry studies were performed for each sample, which enabled the identification, in the extracts, of the derivatization products of a total of 13 aldehydes (formaldehyde, acetaldehyde, furfural, propanal, 5-methylfurfural, butanal, benzaldehyde, pentanal, hexanal, trans-2-heptenal, heptanal, octanal, and trans-2-nonenal) and 4 ketones (3-hydroxy-2-butanone, acetone, cyclohexanone, and acetophenone). This new analytical methodology simultaneously proved to be consistent for the identification and determination of aldehydes in cork agglomerates and a very simple and straightforward procedure.

Dosimetry characteristics of HDPE-SWCNT nanocomposite for real time application

NASA Astrophysics Data System (ADS)

Malekie, Shahryar; Ziaie, Farhood; Feizi, Shahzad; Esmaeli, Abdolreza

2016-10-01

In this experimental work, different dosimetric characteristics of high density polyethylene-single wall carbon nanotube nanocomposite were investigated. The nanocomposite samples were prepared with different nanotube contents of 0.22, 0.25, and 0.39 weight percentages which were before, exactly in, and after percolation region of the nanocomposite, respectively. The samples were exposed to 60Co gamma radiation source over the dose rate of 65-214 mGy/min, while the applied bias was 100 V. A linear response achieved for the sample contained 0.25 nanotube wt% verified that the percolation threshold is the optimum point for dosimetric purposes. The current-voltage characteristics curve measured for 0.25 CNT wt% nanocomposite showed that the behavior of this sample was bias polarity independent. Also, the results showed that the response of this nanocomposite was energy-independent. The maximum discrepancy of photocurrent due to angular variation within 0-90° with respect to beam incidence and the reproducibility of the response were measured as 5.4% and 0.8%, respectively. The stability study showed that this material may be suitable for protection dose level control. Therefore, this kind of nanocomposite requiring calibration can be used as a real-time dosimeter.

Camel molar tooth enamel response to gamma rays using EPR spectroscopy.

PubMed

El-Faramawy, N A; El-Somany, I; Mansour, A; Maghraby, A M; Eissa, H; Wieser, A

2018-03-01

Tooth enamel samples from molar teeth of camel were prepared using a combined procedure of mechanical and chemical tooth treatment. Based on electron paramagnetic resonance (EPR) spectroscopy, the dose response of tooth enamel samples was examined and compared to that of human enamel. The EPR dose response of the tooth enamel samples was obtained through irradiation to gamma doses from 1 Gy up to 100 kGy. It was found that the radiation-induced EPR signal increased linearly with gamma dose for all studied tooth enamel samples, up to about 15 kGy. At higher doses, the dose response curve leveled off. The results revealed that the location of the native signal of camel tooth enamel was similar to that of enamel from human molars at 2.00644, but different from that of enamel from cows and goats. In addition, the peak-to-peak width (ΔH pp ) for human and camel molar teeth was similar. It was also found that the response of camel enamel to gamma radiation was 36% lower than that of human enamel. In conclusion, the results indicate the suitability of camel teeth for retrospective gamma dosimetry.

Crystallized InBiS3 thin films with enhanced optoelectronic properties

NASA Astrophysics Data System (ADS)

Ali, N.; Hussain, Arshad; Ahmed, R.; Omar, M. Firdaus Bin; Sultan, M.; Fu, Yong Qing

2018-04-01

In this paper, a one-step thermal evaporation approach was used for fabrication of indium bismuth sulphide thin films, and the synergetic effects of co-evaporation of two sources (indium granules and Bi2S3 powders) were investigated using different characterization techniques. X-ray diffraction (XRD) analysis confirmed the crystalline orthorhombic structure for the post-annealed samples. Surface roughness and crystal size of the obtained film samples were increased with increasing annealing temperatures. Analysis using X-ray photoelectron spectroscopy showed the formation of the InBiS3 structure for the obtained films, which is also confirmed by the XRD results. The optical absorption coefficient value of the annealed samples was found to be in the order of 105 cm-1 in the visible region of the solar spectrum. The optical band gap energy and electrical resistivity of the fabricated samples were observed to decrease (from 2.2 to 1.3 eV, and from 0.3 to 0.01 Ω-cm, respectively) with increasing annealing temperatures (from 200 to 350 °C), indicating the suitability of the prepared InBiS3 thin films for solar cell applications.

Accelerator mass spectrometry of Strontium-90 for homeland security, environmental monitoring, and human health

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

Tumey, S J; Brown, T A; Hamilton, T F

2008-03-03

Strontium-90 is one of the most hazardous materials managed by agencies charged with protecting the public from radiation. Traditional radiometric methods have been limited by low sample throughput and slow turnaround times. Mass spectrometry offers the advantage of shorter analysis times and the ability to measure samples immediately after processing, however conventional mass spectrometric techniques are susceptible to molecular isobaric interferences that limit their overall sensitivity. In contrast, accelerator mass spectrometry is insensitive to molecular interferences and we have therefore begun developing a method for determination of {sup 90}Sr by accelerator mass spectrometry. Despite a pervasive interference from {sup 90}Zr,more » our initial development has yielded an instrumental background of {approx} 10{sup 8} atoms (75 mBq) per sample. Further refinement of our system (e.g., redesign of our detector, use of alternative target materials) is expected to push the background below 10{sup 6} atoms, close to the theoretical limit for AMS. Once we have refined our system and developed suitable sample preparation protocols, we will utilize our capability in applications to homeland security, environmental monitoring, and human health.« less

From IEDs to AIDS? Detection of HIV in human corpses by rapid screening tests after suspected intentional transmission in terrorist attacks.

PubMed

Frickmann, Hagen; Wulff, B; Loderstædt, U; Hagen, R M; Sturm, D; Polywka, S

2013-12-01

We evaluated the feasibility of intentional transmission of HIV by means of suicide bombing and rape as a terrorist tactic in asymmetric conflicts by evaluating the recognised optimum conditions for biological warfare. We also estimated the suitability of a fourth-generation rapid test for HIV detection in the blood of dead terrorists killed in the completion of their mission. The feasibility of deliberate transmission of HIV for terroristic ends was evaluated on the basis of published experience from passive biological warfare research. In addition, blood from four recently deceased HIV-positive patients and four HIV-negative control corpses, stored at 4°C in a mortuary, was analysed at 12, 24, 36 and 48 h postmortem by rapid serological testing. The feasibility of HIV infection for terroristic purposes was established. The fourth-generation HIV rapid test we evaluated identified all HIV-positive samples and was negative for all HIV-negative samples. Rapid HIV testing from the remains of dead terrorists in the deployed military environment is possible. Samples should be acquired quickly, basic sample preparation is advisable and consequent decisions concerning postexposure prophylaxis should take into account the diagnostic gap in early infections.

Multiplex PCR method for MinION and Illumina sequencing of Zika and other virus genomes directly from clinical samples

PubMed Central

Quick, Josh; Grubaugh, Nathan D; Pullan, Steven T; Claro, Ingra M; Smith, Andrew D; Gangavarapu, Karthik; Oliveira, Glenn; Robles-Sikisaka, Refugio; Rogers, Thomas F; Beutler, Nathan A; Burton, Dennis R; Lewis-Ximenez, Lia Laura; de Jesus, Jaqueline Goes; Giovanetti, Marta; Hill, Sarah; Black, Allison; Bedford, Trevor; Carroll, Miles W; Nunes, Marcio; Alcantara, Luiz Carlos; Sabino, Ester C; Baylis, Sally A; Faria, Nuno; Loose, Matthew; Simpson, Jared T; Pybus, Oliver G; Andersen, Kristian G; Loman, Nicholas J

2018-01-01

Genome sequencing has become a powerful tool for studying emerging infectious diseases; however, genome sequencing directly from clinical samples without isolation remains challenging for viruses such as Zika, where metagenomic sequencing methods may generate insufficient numbers of viral reads. Here we present a protocol for generating coding-sequence complete genomes comprising an online primer design tool, a novel multiplex PCR enrichment protocol, optimised library preparation methods for the portable MinION sequencer (Oxford Nanopore Technologies) and the Illumina range of instruments, and a bioinformatics pipeline for generating consensus sequences. The MinION protocol does not require an internet connection for analysis, making it suitable for field applications with limited connectivity. Our method relies on multiplex PCR for targeted enrichment of viral genomes from samples containing as few as 50 genome copies per reaction. Viral consensus sequences can be achieved starting with clinical samples in 1-2 days following a simple laboratory workflow. This method has been successfully used by several groups studying Zika virus evolution and is facilitating an understanding of the spread of the virus in the Americas. PMID:28538739

Analysis of land suitability for urban development in Ahwaz County in southwestern Iran using fuzzy logic and analytic network process (ANP).

PubMed

Malmir, Maryam; Zarkesh, Mir Masoud Kheirkhah; Monavari, Seyed Masoud; Jozi, Seyed Ali; Sharifi, Esmail

2016-08-01

The ever-increasing development of cities due to population growth and migration has led to unplanned constructions and great changes in urban spatial structure, especially the physical development of cities in unsuitable places, which requires conscious guidance and fundamental organization. It is therefore necessary to identify suitable sites for future development of cities and prevent urban sprawl as one of the main concerns of urban managers and planners. In this study, to determine the suitable sites for urban development in the county of Ahwaz, the effective biophysical and socioeconomic criteria (including 27 sub-criteria) were initially determined based on literature review and interviews with certified experts. In the next step, a database of criteria and sub-criteria was prepared. Standardization of values and unification of scales in map layers were done using fuzzy logic. The criteria and sub-criteria were weighted by analytic network process (ANP) in the Super Decision software. Next, the map layers were overlaid using weighted linear combination (WLC) in the GIS software. According to the research findings, the final land suitability map was prepared with five suitability classes of very high (5.86 %), high (31.93 %), medium (38.61 %), low (17.65 %), and very low (5.95 %). Also, in terms of spatial distribution, suitable lands for urban development are mainly located in the central and southern parts of the Ahwaz County. It is expected that integration of fuzzy logic and ANP model will provide a better decision support tool compared with other models. The developed model can also be used in the land suitability analysis of other cities.

Centrifugal partition chromatography: A preparative tool for isolation and purification of xylindein from Chlorociboria aeruginosa.

PubMed

Boonloed, Anukul; Weber, Genevieve L; Ramzy, Kelly M; Dias, Veronica R; Remcho, Vincent T

2016-12-23

A centrifugal partition chromatography (CPC) method was developed for the preparative-scale isolation and purification of xylindein from the wood-staining fungi, Chlorociboria aeruginosa. Xylindein, a blue-green pigment naturally secreted from the hyphae and fruiting bodies of the fungus, has great value in the decorative wood industry and textile coloration. Xylindein has great potential for use as a fluorescent labeling agent as well as in organic semiconductor applications. However, a primary limitation of xylindein is its poor solubility in most common HPLC solvents. Consequently, it is arduous to purify using preparative liquid chromatography or solid-phase extraction (SPE). Support-free, liquid-liquid chromatographic methods, including CPC, where solutes are separated based on their different distribution coefficients (K D ) between two immiscible solvent systems, are promising alternatives for the purification of the compound on a preparative scale. In this work, a new biphasic solvent system suitable for CPC separation of xylindein was developed. Various groups of solvents were assessed for their suitability as xylindein extractants. A new solvent system suitable for CPC separation of xylindein, composed of heptane/THF/MEK/acetonitrile/acetic acid/water, was developed. This solvent system yielded a K D value for xylindein of 1.54±0.04, as determined by HPLC (n=3). The compositions of the upper phase and lower phase of the solvent system were determined by Heteronuclear Single Quantum Correlation (HSQC) NMR and proton NMR. A CPC system, equipped with a fraction collector, was used for the isolation of xylindein from crude extracts. The xylindein fractions isolated by the CPC were then analyzed using HPLC and presented as a fractogram. Based on the CPC fractogram, the purified xylindein fractions were achieved after 30min CPC separation time, yielding 71% extraction efficiency. The developed CPC method allowed for isolation of this naturally sourced xylindein in amounts suitable for further study. Copyright © 2016 Elsevier B.V. All rights reserved.

Suitability of different containers for the sampling and storage of biogas and biomethane for the determination of the trace-level impurities--A review.

PubMed

Arrhenius, Karine; Brown, Andrew S; van der Veen, Adriaan M H

2016-01-01

The traceable and accurate measurement of biogas impurities is essential in order to robustly assess compliance with the specifications for biomethane being developed by CEN/TC408. An essential part of any procedure aiming to determinate the content of impurities is the sampling and the transfer of the sample to the laboratory. Key issues are the suitability of the sample container and minimising the losses of impurities during the sampling and analysis process. In this paper, we review the state-of-the-art in biogas sampling with the focus on trace impurities. Most of the vessel suitability studies reviewed focused on raw biogas. Many parameters need to be studied when assessing the suitability of vessels for sampling and storage, among them, permeation through the walls, leaks through the valves or physical leaks, sorption losses and adsorption effects to the vessel walls, chemical reactions and the expected initial concentration level. The majority of these studies looked at siloxanes, for which sampling bags, canisters, impingers and sorbents have been reported to be fit-for-purpose in most cases, albeit with some limitations. We conclude that the optimum method requires a combination of different vessels to cover the wide range of impurities commonly found in biogas, which have a wide range of boiling points, polarities, water solubilities, and reactivities. The effects from all the parts of the sampling line must be considered and precautions must be undertaken to minimize these effects. More practical suitability tests, preferably using traceable reference gas mixtures, are needed to understand the influence of the containers and the sampling line on sample properties and to reduce the uncertainty of the measurement. Copyright © 2015 Elsevier B.V. All rights reserved.

Quantitative aspects of microchip isotachophoresis for high precision determination of main components in pharmaceuticals.

PubMed

Hradski, Jasna; Chorváthová, Mária Drusková; Bodor, Róbert; Sabo, Martin; Matejčík, Štefan; Masár, Marián

2016-12-01

Although microchip electrophoresis (MCE) is intended to provide reliable quantitative data, so far there is only limited attention paid to these important aspects. This study gives a general overview of key aspects to be followed to reach high-precise determination using isotachophoresis (ITP) on the microchip with conductivity detection. From the application point of view, the procedure for the determination of acetate, a main component in the pharmaceutical preparation buserelin acetate, was developed. Our results document that run-to-run fluctuations in the sample injection volume limit the reproducibility of quantitation based on the external calibration. The use of a suitable internal standard (succinate in this study) improved the repeatability of the precision of acetate determination from six to eight times. The robustness of the procedure was studied in terms of impact of fluctuations in various experimental parameters (driving current, concentration of the leading ions, pH of the leading electrolyte and buffer impurities) on the precision of the ITP determination. The use of computer simulation programs provided means to assess the ITP experiments using well-defined theoretical models. A long-term validity of the calibration curves on two microchips and two MCE equipments was verified. This favors ITP over other microchip electrophoresis techniques, when chip-to-chip or equipment-to-equipment transfer of the analytical method is required. The recovery values in the range of 98-101 % indicate very accurate determination of acetate in buserelin acetate, which is used in the treatment of hormone-dependent tumors. This study showed that microchip ITP is suitable for reliable determination of main components in pharmaceutical preparations.

Preparation and characterization of hierarchical porous carbons derived from solid leather waste for supercapacitor applications.

PubMed

Konikkara, Niketha; Kennedy, L John; Vijaya, J Judith

2016-11-15

Utilization of crust leather waste (CLW) as precursors for the preparation of hierarchical porous carbons (HPC) were investigated. HPCs were prepared from CLW by pre-carbonization followed by chemical activation using KOH at relatively high temperatures. Textural properties of HPC's showed an extent of micro-and mesoporosity with maximum BET surface area of 716m(2)/g. Inducements of graphitic planes in leather waste derived carbons were observed from X-ray diffraction and HR-TEM analysis. Microstructure, thermal behavior and surface functional groups were identified using FT-Raman, thermo gravimetric analysis and FT-IR techniques. HPCs were evaluated for electrochemical properties by cyclic voltammetry (CV), galvanostatic charge/discharge (GCD) and electrochemical impedance spectroscopy (EIS) by three electrode system. CLC9 sample showed a maximum capacitance of 1960F/g in 1M KCl electrolyte. Results achieved from rectangular curves of CV, GCD symmetric curves and Nyquist plots show that the leather waste carbon is suitable to fabricate supercapacitors as it possess high specific capacitance and electrochemical cycle stability. The present study proposes an effective method for solid waste management in leather industry by the way of converting toxic leather waste to new graphitic porous carbonaceous materials as a potential candidate for energy storage devices. Copyright © 2016 Elsevier B.V. All rights reserved.

Inner ear tissue preservation by rapid freezing: Improving fixation by high-pressure freezing and hybrid methods

PubMed Central

Bullen, A.; Taylor, R.R.; Kachar, B.; Moores, C.; Fleck, R.A.; Forge, A.

2014-01-01

In the preservation of tissues in as ‘close to life’ state as possible, rapid freeze fixation has many benefits over conventional chemical fixation. One technique by which rapid freeze-fixation can be achieved, high pressure freezing (HPF), has been shown to enable ice crystal artefact-free freezing and tissue preservation to greater depths (more than 40 μm) than other quick-freezing methods. Despite increasingly becoming routine in electron microscopy, the use of HPF for the fixation of inner ear tissue has been limited. Assessment of the quality of preservation showed routine HPF techniques were suitable for preparation of inner ear tissues in a variety of species. Good preservation throughout the depth of sensory epithelia was achievable. Comparison to chemically fixed tissue indicated that fresh frozen preparations exhibited overall superior structural preservation of cells. However, HPF fixation caused characteristic artefacts in stereocilia that suggested poor quality freezing of the actin bundles. The hybrid technique of pre-fixation and high pressure freezing was shown to produce cellular preservation throughout the tissue, similar to that seen in HPF alone. Pre-fixation HPF produced consistent high quality preservation of stereociliary actin bundles. Optimising the preparation of samples with minimal artefact formation allows analysis of the links between ultrastructure and function in inner ear tissues. PMID:25016142

Preparation and testing of a tetra-amine copper(II) chitosan bead system for enhanced phosphate remediation.

PubMed

Kumar, Ilango Aswin; Viswanathan, Natrayasamy

2018-03-01

A tetra-amine copper(II) chitosan bead system (TAC@CS composite beads) was developed by grafting tetra-amine copper(II) (TAC) with chitosan (CS) and utilized for phosphate removal. The prepared TAC@CS composite beads possess enhanced phosphate sorption capacity (SC) of 41.42 ± 0.071 mg/g than copper grafted chitosan (Cu@CS) composite, TAC and chitosan which were found to be 37.01 ± 0.803, 33.20 ± 0.650 and 7.24 ± 0.059 mg/g respectively. In batch mode, various adsorption influencing parameters like contact time, initial phosphate concentration, solution pH, co-anions and temperature were optimized for maximum phosphate sorption. The prepared adsorbents were characterized by FTIR, XRD, UV-Visible, SEM and EDAX analysis. The adsorption isotherms and thermodynamic parameters of the adsorbent were studied. The feasible phosphate uptake mechanism of TAC@CS biocomposite beads was reported. The reusability studies of TAC@CS composite beads were carried out using NaOH as elutant. The suitability of TAC@CS composite beads at field conditions was tested with phosphate contaminated field water samples collected from nearby areas of Dindigul district. Copyright © 2017 Elsevier Ltd. All rights reserved.

Preparation of Ag-containing diamond-like carbon films on the interior surface of tubes by a combined method of plasma source ion implantation and DC sputtering

NASA Astrophysics Data System (ADS)

Hatada, R.; Flege, S.; Bobrich, A.; Ensinger, W.; Dietz, C.; Baba, K.; Sawase, T.; Watamoto, T.; Matsutani, T.

2014-08-01

Adhesive diamond-like carbon (DLC) films can be prepared by plasma source ion implantation (PSII), which is also suitable for the treatment of the inner surface of a tube. Incorporation of a metal into the DLC film provides a possibility to change the characteristics of the DLC film. One source for the metal is DC sputtering. In this study PSII and DC sputtering were combined to prepare DLC films containing low concentrations of Ag on the interior surfaces of stainless steel tubes. A DLC film was deposited using a C2H4 plasma with the help of an auxiliary electrode inside of the tube. This electrode was then used as a target for the DC sputtering. A mixture of the gases Ar and C2H4 was used to sputter the silver. By changing the gas flow ratios and process time, the resulting Ag content of the films could be varied. Sample characterizations were performed by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, atomic force microscopy and Raman spectroscopy. Additionally, a ball-on-disk test was performed to investigate the tribological properties of the films. The antibacterial activity was determined using Staphylococcus aureus bacteria.

Multiclass mycotoxin analysis in edible oils using a simple solvent extraction method and liquid chromatography with tandem mass spectrometry.

PubMed

Eom, Taeyong; Cho, Hyun-Deok; Kim, Junghyun; Park, Mihee; An, Jinyoung; Kim, Moosung; Kim, Sheen-Hee; Han, Sang Beom

2017-11-01

A simple and rapid method for the simultaneous determination of 11 mycotoxins - aflatoxins B 1 , B 2 , G 1 and G 2 ; fumonisins B 1 , B 2 and B 3 ; ochratoxin A; zearalenone; deoxynivalenol; and T-2 toxin - in edible oils was established using liquid chromatography tandem mass spectrometry (LC-MS/MS). In this study, QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe), QuEChERS with dispersive liquid-liquid microextraction, and solvent extraction were examined for sample preparation. Among these methods, solvent extraction with a mixture of formic acid/acetonitrile (5/95, v/v) successfully extracted all target mycotoxins. Subsequently, a defatting process using n-hexane was employed to remove the fats present in the edible oil samples. Mass spectrometry was carried out using electrospray ionisation in polarity switching mode with multiple reaction monitoring. The developed LC-MS/MS method was validated by assessing the specificity, linearity, recovery, limit of quantification (LOQ), accuracy and precision with reference to Commission Regulation (EC) 401/2006. Mycotoxin recoveries of 51.6-82.8% were achieved in addition to LOQs ranging from 0.025 ng/g to 1 ng/g. The edible oils proved to be relatively uncomplicated matrices and the developed method was applied to 9 edible oil samples, including soybean oil, corn oil and rice bran oil, to evaluate potential mycotoxin contamination. The levels of detection were significantly lower than the international regulatory standards. Therefore, we expect that our developed method, based on simple, two-step sample preparation process, will be suitable for the large-scale screening of mycotoxin contamination in edible oils.

Combinatorial Solid-Phase Synthesis of Aromatic Oligoamides: A Research-Based Laboratory Module for Undergraduate Organic Chemistry

ERIC Educational Resources Information Center

Fuller, Amelia A.

2016-01-01

A five-week, research-based experiment suitable for second-semester introductory organic laboratory students is described. Each student designs, prepares, and analyzes a combinatorial array of six aromatic oligoamides. Molecules are prepared on solid phase via a six-step synthetic sequence, and purities and identities are determined by analysis of…

Attrition resistant bulk iron catalysts and processes for preparing and using same

DOEpatents

Jothimurugesan, Kandaswamy [Ponca City, OK; Goodwin, Jr., James G.; Gangwal, Santosh K [Cary, NC

2007-08-21

An attrition resistant precipitated bulk iron catalyst is prepared from iron oxide precursor and a binder by spray drying. The catalysts are preferably used in carbon monoxide hydrogenation processes such as Fischer-Tropsch synthesis. These catalysts are suitable for use in fluidized-bed reactors, transport reactors and, especially, slurry bubble column reactors.

Survival and growth response of white spruce stock types to site preparation in Alaska

Treesearch

Andrew Youngblood; Elizabeth Cole; Michael Newton

2011-01-01

To identify suitable methods for reforestation, we evaluated the interacting effects of past disturbance, stock types, and site preparation treatments on white spruce (Picea glauca (Moench) Voss) seedling survival and growth across a range of sites in Alaska. Replicated experiments were established in five regions. At each site, two complete...

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

Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry.

PubMed

Grate, Jay W; Gonzalez, Jhanis J; O'Hara, Matthew J; Kellogg, Cynthia M; Morrison, Samuel S; Koppenaal, David W; Chan, George C-Y; Mao, Xianglei; Zorba, Vassilia; Russo, Richard E

2017-09-08

Solid sampling and analysis methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), are challenged by matrix effects and calibration difficulties. Matrix-matched standards for external calibration are seldom available and it is difficult to distribute spikes evenly into a solid matrix as internal standards. While isotopic ratios of the same element can be measured to high precision, matrix-dependent effects in the sampling and analysis process frustrate accurate quantification and elemental ratio determinations. Here we introduce a potentially general solid matrix transformation approach entailing chemical reactions in molten ammonium bifluoride (ABF) salt that enables the introduction of spikes as tracers or internal standards. Proof of principle experiments show that the decomposition of uranium ore in sealed PFA fluoropolymer vials at 230 °C yields, after cooling, new solids suitable for direct solid sampling by LA. When spikes are included in the molten salt reaction, subsequent LA-ICP-MS sampling at several spots indicate that the spikes are evenly distributed, and that U-235 tracer dramatically improves reproducibility in U-238 analysis. Precisions improved from 17% relative standard deviation for U-238 signals to 0.1% for the ratio of sample U-238 to spiked U-235, a factor of over two orders of magnitude. These results introduce the concept of solid matrix transformation (SMT) using ABF, and provide proof of principle for a new method of incorporating internal standards into a solid for LA-ICP-MS. This new approach, SMT-LA-ICP-MS, provides opportunities to improve calibration and quantification in solids based analysis. Looking forward, tracer addition to transformed solids opens up LA-based methods to analytical methodologies such as standard addition, isotope dilution, preparation of matrix-matched solid standards, external calibration, and monitoring instrument drift against external calibration standards.

Groundwater quality assessment using geospatial and statistical tools in Salem District, Tamil Nadu, India

NASA Astrophysics Data System (ADS)

Arulbalaji, P.; Gurugnanam, B.

2017-10-01

The water quality study of Salem district, Tamil Nadu has been carried out to assess the water quality for domestic and irrigation purposes. For this purpose, 59 groundwater samples were collected and analyzed for pH, electrical conductivity (EC), total dissolved solids (TDS), major anions (HCO3 -, CO3 -, F-, Cl-, NO2 - + NO3 -, and SO4 2-), major cations (Ca2+ Mg2+, Na+, and K+), alkalinity (ALK), and hardness (HAR). To assess the water quality, the following chemical parameters were calculated based on the analytical results, such as Piper plot, water quality index (WQI), sodium adsorption ratio (SAR), magnesium hazard (MH), Kelly index (KI), and residual sodium carbonate (RSC). Wilcox diagram represents that 23% of the samples are excellent to good, 40% of the samples are good to permissible, 10% of the samples are permissible to doubtful, 24% of the samples are doubtful unsuitable, and only 3% of the samples are unsuitable for irrigation. SAR values shows that 52% of the samples indicate high-to-very high and low-to-medium alkali water. KI values indicate good quality (30%) and not suitable (70%) for irrigation purposes. RSC values indicate that 89% of samples are suitable for irrigation purposes. MH reveals that 17% suitable and 83% samples are not suitable for irrigation purposes and for domestic purposes the excellent (8%), good (48%), and poor (44%). The agricultural waste, fertilizer used, soil leaching, urban runoff, livestock waste, and sewages are the sources of poor water quality. Some samples are not suitable for irrigation purposes due to high salinity, hardness, and magnesium concentration. In general, the groundwater of the Salem district was polluted by agricultural activities, anthropogenic activities, ion exchange, and weathering.

Determination of heavy metals and halogens in plastics from electric and electronic waste.

PubMed

Dimitrakakis, Emmanouil; Janz, Alexander; Bilitewski, Bernd; Gidarakos, Evangelos

2009-10-01

The presence of hazardous substances and preparations in small waste electrical and electronic equipment (sWEEE) found in the residual household waste stream of the city of Dresden, Germany has been investigated. The content of sWEEE plastics in heavy metals and halogens is determined using handheld X-ray fluorescence analysis (HXRF), elemental analysis by means of atomic absorption spectrometry (AAS) and ion exchange chromatography (IEC). Mean value of results for heavy metals in samples (n=51) by AAS are 17.4 mg/kg for Pb, 5.7 mg/kg for Cd, 8.4 mg/kg for Cr. The mass fraction of an additive as shown by HXRF (n=161) can vary over a wide range. Precise deductions as regards sWEEE plastics content in hazardous substances and preparations cannot be made. Additional research would be expedient regarding the influence of hazardous substances to recycling processes, in particular regarding the contamination of clean fractions in the exit streams of a WEEE treatment plant. Suitable standards for calibrating HXRF for use on EEE plastics or complex electr(on)ic components do not exist and should be developed.

Barbell-shaped stir bar sorptive extraction using dummy template molecularly imprinted polymer coatings for analysis of bisphenol A in water.

PubMed

Liu, Ruimei; Feng, Feng; Chen, Guolin; Liu, Zhimin; Xu, Zhigang

2016-07-01

This study reports the development of a novel dummy template molecularly imprinted polymer (MIP)-coated barbell-shaped stir bar. The MIP stir bar coatings were prepared by using 2,2-bis(4-hydroxyphenyl)butane (BPB), 4,4'-dihydroxydiphenylmethane (BPF), 4-tert-butylphenol (PTBP), and tetrabromobisphenol A (TBBA) as dummy templates using a capillary in situ polymerization method. Uniform coatings can be prepared controllably. The method is simple, easy, and reproducible. The barbell-shaped stir bar was developed by using medical silicone tubes as wheels. The wheels could be removed and reinstalled when necessary; therefore, the barbell-shaped stir bar was easy to disassemble and reassemble. The novel MIP-coated stir bar showed good selectivity for the target analyte, bisphenol A (BPA). The established method is selective and sensitive with a lower detection limit for BPA of 0.003 μg/L. The dummy template MIP-coated stir bar is suitable for trace BPA analysis in real environmental water samples without template leakage. The novel stir bar can be used at least 100 times.

One-step Synthesis of Highly Luminescent Nitrogen-doped Carbon Dots for Selective and Sensitive Detection of Mercury(II) Ions and Cellular Imaging.

PubMed

Liu, Ying; Liao, Mei; He, Xueling; Liu, Xia; Kou, Xingming; Xiao, Dan

2015-01-01

In this paper, nitrogen-doped carbon dots (N-CDs) with high quantum yield (QY) of 40.5% were prepared through a facile and straightforward hydrothermal route. The as-prepared N-CDs exhibited excellent photoluminescence properties, good water-solublity and photostability, negligible cytotoxicity and favourable biocompatibility. Such N-CDs were found to serve as an effective fluorescent sensor for selective and sensitive detection of Hg(2+) in a wide linear response concentration range of 0 - 8 μM with a limit of detection (LOD) of 0.087 μM and could be applied to the determination of Hg(2+) in environmental water samples. The corresponding mechanisms were discussed in detail. Moreover, another attractive finding was that the N-CDs showed satisfactory performance in bioimaging before and after the addition of Hg(2+) in human lung cancer PC14 cells. With excellent sensitivity, selectivity and biocompatibility, such cheap carbonmaterials are potentially suitable for monitoring of Hg(2+) in environmental applications and promising for biological applications.

Steady state preparative multiple dual mode counter-current chromatography: Productivity and selectivity. Theory and experimental verification.

PubMed

Kostanyan, Artak E; Erastov, Andrey A

2015-08-07

In the steady state (SS) multiple dual mode (MDM) counter-current chromatography (CCC), at the beginning of the first step of every cycle the sample dissolved in one of the phases is continuously fed into a CCC device over a constant time, not exceeding the run time of the first step. After a certain number of cycles, the steady state regime is achieved, where concentrations vary over time during each cycle, however, the concentration profiles of solutes eluted with both phases remain constant in all subsequent cycles. The objective of this work was to develop analytical expressions to describe the SS MDM CCC separation processes, which can be helpful to simulate and design these processes and select a suitable compromise between the productivity and the selectivity in the preparative and production CCC separations. Experiments carried out using model mixtures of compounds from the GUESSmix with solvent system hexane/ethyl acetate/methanol/water demonstrated a reasonable agreement between the predictions of the theory and the experimental results. Copyright © 2015 Elsevier B.V. All rights reserved.

Self-Supporting, Hydrophobic, Ionic Liquid-Based Reference Electrodes Prepared by Polymerization-Induced Microphase Separation.

PubMed

Chopade, Sujay A; Anderson, Evan L; Schmidt, Peter W; Lodge, Timothy P; Hillmyer, Marc A; Bühlmann, Philippe

2017-10-27

Interfaces of ionic liquids and aqueous solutions exhibit stable electrical potentials over a wide range of aqueous electrolyte concentrations. This makes ionic liquids suitable as bridge materials that separate in electroanalytical measurements the reference electrode from samples with low and/or unknown ionic strengths. However, methods for the preparation of ionic liquid-based reference electrodes have not been explored widely. We have designed a convenient and reliable synthesis of ionic liquid-based reference electrodes by polymerization-induced microphase separation. This technique allows for a facile, single-pot synthesis of ready-to-use reference electrodes that incorporate ion conducting nanochannels filled with either 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide or 1-dodecyl-3-methylimidazolium bis(trifluoromethyl sulfonyl)imide as ionic liquid, supported by a mechanically robust cross-linked polystyrene phase. This synthesis procedure allows for the straightforward design of various reference electrode geometries. These reference electrodes exhibit a low resistance as well as good reference potential stability and reproducibility when immersed into aqueous solutions varying from deionized, purified water to 100 mM KCl, while requiring no correction for liquid junction potentials.

Shielding small-field high-energy electron beams in cancer treatment

NASA Astrophysics Data System (ADS)

Farahani, M.; Eichmiller, F. C.; McLaughlin, W. L.

1994-04-01

The purpose of this study was to find an effective material that can be prepared quickly and easily prior to small-field electron-beam treatments so that lesions of the head and neck can be treated with minimal irradiation of the surrounding healthy tissue. Conventional preparation of custom anatomical prosthetic radiation shields, which are usually metal alloy masks, has been time-consuming and uncomfortable for the patients. New materials, made from light-body Reprosil TM (L. L. Caulk) filled with fine metal powder consisting of 70% Ag-30% Cu alloy, can be made by blending 90% (w/w) metal powder with 10% polysiloxane base and adding the polymerization catalyst separately. These combinations were mixed to form comfortably fitted shielding composites of different thicknesses. The electron-beam attenuation properties of slabs of this material were studied by irradiating calibrated radiochromic film (GafChromic TM) dosimeters behind different thicknesses of composite samples with small-field 13-, 15- and 18-MeV electron beams from a therapeutic linear accelerator. The results showed that this material can suitably attenuate high-energy electron beams when used in reasonable thicknesses.

[Effects of annealing temperature on the structure and optical properties of ZnMgO films prepared by atom layer deposition].

PubMed

Sun, Dong-Xiao; Li, Jin-Hua; Fang, Xuan; Chen, Xin-Ying; Fang, Fang; Chu, Xue-Ying; Wei, Zhi-Peng; Wang, Xiao-Hua

2014-07-01

In the present paper, we report the research on the effects of annealing temperature on the crystal quality and optical properties of ZnMgO films deposited by atom layer deposition(ALD). ZnMgO films were prepared on quartz substrates by ALD and then some of the samples were treated in air ambient at different annealing temperature. The effects of annealing temperature on the crystal quality and optical properties of ZnMgO films were characterized by X-ray diffraction (XRD), photoluminescence (PL) and ultraviolet-visible (UV-Vis) absorption spectra. The XRD results showed that the crystal quality of ZnMgO films was significantly improved when the annealing temperature was 600 degrees C, meanwhile the intensity of(100) diffraction peak was the strongest. Combination of PL and UV-Vis absorption measurements showed that it can strongly promote the Mg content increasing in ZnMgO films and increase the band gap of films. So the results illustrate that suitable annealing temperature can effectively improve the crystal quality and optical properties of ZnMgO films.

Study of the effect of ZnO film on some properties of clear and color window glass

NASA Astrophysics Data System (ADS)

Hamead, Alaa A. Abdul; Ahmed, Sura S.; Khdheer, Mena F.

2018-05-01

In the current research, a samples of transparent color and colorless window glass were prepared, (includes metal transition oxides) for construction applications. A nano-film layer of zinc oxide ZnO was deposited by spray pyrolysis technique for use in sustainability applications prepared. Structural properties (x-ray diffraction XRD, scanning electron microscopy SEM and atomic force microscopy AFM), and thermal properties, as well as optical properties and the effect of weathering conditions on applied film on clear and colored glass were examined. The results showed that the deposition film had a thickness of less than 90nm and that it was crystallized with high optical transparently, that was not significantly affected after deposited the ZnO nano film. While thermal insulation decreased significantly after deposition, and the effect of the weather conditions was very low as the ZnO coating was not affected, as the thermal insulation did not change after exposure to accelerated air conditions. Make it suitable in glass applications for buildings in vertical construction.

Development of low fat potato chips through microwave processing.

PubMed

Joshi, A; Rudra, S G; Sagar, V R; Raigond, P; Dutt, S; Singh, B; Singh, B P

2016-08-01

Since snacks high in fats are known to be a significant source of fat and energy intake, these have been put in high dietary restraint category. Therefore, an attempt was made to process potato chips through microwave processing without incorporation of any oil in potato chips. Microwave processing of potato chips was done using microwave power varying from 180 to 600 W using constant sample size. Among eleven different drying models, Parabolic model was found to be the best fit through non-linear regression analysis to illustrate drying kinetics of potato chips. The structural, textural and colour attributes of microwaved potato chips were similar to commercial fried potato chips. It was found that at 600 W after 2.5-3.0 min of processing, potato chips gained the fracturability and crispiness index as that of commercial fried chips. Microwave processing was found suitable for processing of potato chips with low fat content (~3.09 vs 35.5 % in commercial preparation) and with acceptable sensory scores (≥7.6 on 9.0 point on hedonic scale vs 8.0 of control preparation).

Preparation of a Ytterbium-tagged Gunshot Residue Standard for Quality Control in the Forensic Analysis of GSR.

PubMed

Hearns, Nigel G R; Laflèche, Denis N; Sandercock, Mark L

2015-05-01

Preparation of a ytterbium-tagged gunshot residue (GSR) reference standard for scanning electron microscopy and energy dispersive X-ray spectroscopic (SEM-EDS) microanalysis is reported. Two different chemical markers, ytterbium and neodymium, were evaluated by spiking the primers of 38 Special ammunition cartridges (no propellant, no projectile) and discharging them onto 12.7 mm diameter aluminum SEM pin stubs. Following SEM-EDS microanalysis, the majority of tri-component particles containing lead, barium, and antimony (PbBaSb) were successfully tagged with the chemical marker. Results demonstrate a primer spiked with 0.75% weight percent of ytterbium nitrate affords PbBaSb particles characteristic of GSR with a ytterbium inclusion efficiency of between 77% and 100%. Reproducibility of the method was verified, and durability of the ytterbium-tagged tri-component particles under repeated SEM-EDS analysis was also tested. The ytterbium-tagged PbBaSb particles impart synthetic traceability to a GSR reference standard and are suitable for analysis alongside case work samples, as a positive control for quality assurance purposes. © 2015 American Academy of Forensic Sciences.

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...

Automated blood-sample handling in the clinical laboratory.

PubMed

Godolphin, W; Bodtker, K; Uyeno, D; Goh, L O

1990-09-01

The only significant advances in blood-taking in 25 years have been the disposable needle and evacuated blood-drawing tube. With the exception of a few isolated barcode experiments, most sample-tracking is performed through handwritten or computer-printed labels. Attempts to reduce the hazards of centrifugation have resulted in air-tight lids or chambers, the use of which is time-consuming and cumbersome. Most commonly used clinical analyzers require serum or plasma, distributed into specialized containers, unique to that analyzer. Aliquots for different tests are prepared by handpouring or pipetting. Moderate to large clinical laboratories perform so many different tests that even multi-analyzers performing multiple analyses on a single sample may account for only a portion of all tests ordered for a patient. Thus several aliquots of each specimen are usually required. We have developed a proprietary serial centrifuge and blood-collection tube suitable for incorporation into an automated or robotic sample-handling system. The system we propose is (a) safe--avoids or prevents biological danger to the many "handlers" of blood; (b) small--minimizes the amount of sample taken and space required to adapt to the needs of satellite and mobile testing, and direct interfacing with analyzers; (c) serial--permits each sample to be treated according to its own "merits," optimizes throughput, and facilitates flexible automation; and (d) smart--ensures quality results through monitoring and intelligent control of patient identification, sample characteristics, and separation process.

Elemental levels in tree-bark and epiphytic-lichen transplants at a mixed environment in mainland Portugal, and comparisons with an in situ lichen.

PubMed

Pacheco, A M G; Freitas, M C; Baptista, M S; Vasconcelos, M T S D; Cabral, J P

2008-01-01

Samples of Platanus hybrida Brot. bark and Flavoparmelia caperata (L.) Hale thalli, from a clean area in northern Portugal (Baião), were transplanted into an exposure location at the south-western Atlantic coast, impacted by urban-industrial emissions (Sines), for a 10-month long experiment. Bark pieces were confined into nylon bags (2-mm mesh), and lichen thalli kept with their bark substrate (Pinus pinaster (Ait.) Sol.). Every two months, a double set of transplants (one for bark, one for lichens) was brought back into the laboratory, together with native samples of Evernia prunastri (L.) Ach. Following suitable cleansing and preparation procedures, field samples were put through INAA for elemental assessment. The results indicate that, regardless of signal magnitude, (1) concentrations in bark and lichen transplants are significantly correlated with atmospheric deposition for an appreciable number of elements; (2) there are a number of significant correlations between transplanted and native samples, and again between the latter and the deposition; and (3) the elements with biological patterns that follow the deposition in either transplanted or native samples (Co, V) are the very ones whose bioaccumulation seems to benefit from an alternation of wet-dry periods, which fits the precipitation record of the test site during the exposure term.

Determination of renewable energy yield from mixed waste material from the use of novel image analysis methods.

PubMed

Wagland, S T; Dudley, R; Naftaly, M; Longhurst, P J

2013-11-01

Two novel techniques are presented in this study which together aim to provide a system able to determine the renewable energy potential of mixed waste materials. An image analysis tool was applied to two waste samples prepared using known quantities of source-segregated recyclable materials. The technique was used to determine the composition of the wastes, where through the use of waste component properties the biogenic content of the samples was calculated. The percentage renewable energy determined by image analysis for each sample was accurate to within 5% of the actual values calculated. Microwave-based multiple-point imaging (AutoHarvest) was used to demonstrate the ability of such a technique to determine the moisture content of mixed samples. This proof-of-concept experiment was shown to produce moisture measurement accurate to within 10%. Overall, the image analysis tool was able to determine the renewable energy potential of the mixed samples, and the AutoHarvest should enable the net calorific value calculations through the provision of moisture content measurements. The proposed system is suitable for combustion facilities, and enables the operator to understand the renewable energy potential of the waste prior to combustion. Copyright © 2013 Elsevier Ltd. All rights reserved.

Reliable quantification of phthalates in environmental matrices (air, water, sludge, sediment and soil): a review.

PubMed

Net, Sopheak; Delmont, Anne; Sempéré, Richard; Paluselli, Andrea; Ouddane, Baghdad

2015-05-15

Because of their widespread application, phthalates or phthalic acid esters (PAEs) are ubiquitous in the environment. Their presence has attracted considerable attention due to their potential impacts on ecosystem functioning and on public health, so their quantification has become a necessity. Various extraction procedures as well as gas/liquid chromatography and mass spectrometry detection techniques are found as suitable for reliable detection of such compounds. However, PAEs are ubiquitous in the laboratory environment including ambient air, reagents, sampling equipment, and various analytical devices, that induces difficult analysis of real samples with a low PAE background. Therefore, accurate PAE analysis in environmental matrices is a challenging task. This paper reviews the extensive literature data on the techniques for PAE quantification in natural media. Sampling, sample extraction/pretreatment and detection for quantifying PAEs in different environmental matrices (air, water, sludge, sediment and soil) have been reviewed and compared. The concept of "green analytical chemistry" for PAE determination is also discussed. Moreover useful information about the material preparation and the procedures of quality control and quality assurance are presented to overcome the problem of sample contamination and these encountered due to matrix effects in order to avoid overestimating PAE concentrations in the environment. Copyright © 2015 Elsevier B.V. All rights reserved.

Normalization of RNA-seq data using factor analysis of control genes or samples

PubMed Central

Risso, Davide; Ngai, John; Speed, Terence P.; Dudoit, Sandrine

2015-01-01

Normalization of RNA-seq data has proven essential to ensure accurate inference of expression levels. Here we show that usual normalization approaches mostly account for sequencing depth and fail to correct for library preparation and other more-complex unwanted effects. We evaluate the performance of the External RNA Control Consortium (ERCC) spike-in controls and investigate the possibility of using them directly for normalization. We show that the spike-ins are not reliable enough to be used in standard global-scaling or regression-based normalization procedures. We propose a normalization strategy, remove unwanted variation (RUV), that adjusts for nuisance technical effects by performing factor analysis on suitable sets of control genes (e.g., ERCC spike-ins) or samples (e.g., replicate libraries). Our approach leads to more-accurate estimates of expression fold-changes and tests of differential expression compared to state-of-the-art normalization methods. In particular, RUV promises to be valuable for large collaborative projects involving multiple labs, technicians, and/or platforms. PMID:25150836

Thermal buffering performance of composite phase change materials applied in low-temperature protective garments

NASA Astrophysics Data System (ADS)

Yang, Kai; Jiao, Mingli; Yu, Yuanyuan; Zhu, Xueying; Liu, Rangtong; Cao, Jian

2017-07-01

Phase change material (PCM) is increasingly being applied in the manufacturing of functional thermo-regulated textiles and garments. This paper investigated the thermal buffering performance of different composite PCMs which are suitable for the application in functional low-temperature protective garments. First, according to the criteria selecting PCM for functional textiles/garments, three kinds of pure PCM were selected as samples, which were n-hexadecane, n-octadecane and n-eicosane. To get the adjustable phase change temperature range and higher phase change enthalpy, three kinds of composite PCM were prepared using the above pure PCM. To evaluate the thermal buffering performance of different composite PCM samples, the simulated low-temperature experiments were performed in the climate chamber, and the skin temperature variation curves in three different low temperature conditions were obtained. Finally composite PCM samples’ thermal buffering time, thermal buffering capacity and thermal buffering efficiency were calculated. Results show that the comprehensive thermal buffering performance of n-octadecane and n-eicosane composite PCM is the best.

Round robin test on quantification of amyloid-β 1-42 in cerebrospinal fluid by mass spectrometry.

PubMed

Pannee, Josef; Gobom, Johan; Shaw, Leslie M; Korecka, Magdalena; Chambers, Erin E; Lame, Mary; Jenkins, Rand; Mylott, William; Carrillo, Maria C; Zegers, Ingrid; Zetterberg, Henrik; Blennow, Kaj; Portelius, Erik

2016-01-01

Cerebrospinal fluid (CSF) amyloid-β 1-42 (Aβ42) is an important biomarker for Alzheimer's disease, both in diagnostics and to monitor disease-modifying therapies. However, there is a great need for standardization of methods used for quantification. To overcome problems associated with immunoassays, liquid chromatography-tandem mass spectrometry (LC-MS/MS) has emerged as a critical orthogonal alternative. We compared results for CSF Aβ42 quantification in a round robin study performed in four laboratories using similar sample preparation methods and LC-MS instrumentation. The LC-MS results showed excellent correlation between laboratories (r(2) >0.98), high analytical precision, and good correlation with enzyme-linked immunosorbent assay (r(2) >0.85). The use of a common reference sample further decreased interlaboratory variation. Our results indicate that LC-MS is suitable for absolute quantification of Aβ42 in CSF and highlight the importance of developing a certified reference material. Copyright © 2016 The Alzheimer's Association. Published by Elsevier Inc. All rights reserved.

Method for detection of long-lived radioisotopes in small biochemical samples

DOEpatents

Turteltaub, K.W.; Vogel, J.S.; Felton, J.S.; Gledhill, B.L.; Davis, J.C.

1994-11-22

Disclosed is a method for detection of long-lived radioisotopes in small biochemical samples, comprising: a. selecting a biological host in which radioisotopes are present in concentrations equal to or less than those in the ambient biosphere, b. preparing a long-lived radioisotope labeled reactive chemical specie, c. administering the chemical specie to the biologist host in doses sufficiently low to avoid significant overt damage to the biological system, d. allowing a period of time to elapse sufficient for dissemination and interaction of the chemical specie with the host throughout the biological system of the host, e. isolating a reacted fraction of the biological substance from the host in a manner sufficient to avoid contamination of the substance from extraneous sources, f. converting the fraction of biological substance by suitable means to a material which efficiently produces charged ions in at least one of several possible ion sources without introduction of significant isotopic fractionation, and, g. measuring the radioisotope concentration in the material by means of direct isotopic counting. 5 figs.

Evaluation of a headspace solid-phase microextraction method for the analysis of ignitable liquids in fire debris.

PubMed

Fettig, Ina; Krüger, Simone; Deubel, Jan H; Werrel, Martin; Raspe, Tina; Piechotta, Christian

2014-05-01

The chemical analysis of fire debris represents a crucial part in fire investigations to determine the cause of a fire. A headspace solid-phase microextraction (HS-SPME) procedure for the detection of ignitable liquids in fire debris using a fiber coated with a mixture of three different sorbent materials (Divinylbenzene/Carboxen/Polydimethylsiloxane, DVB/CAR/PDMS) is described. Gasoline and diesel fuel were spiked upon a preburnt matrix (wood charcoal), extracted and concentrated with HS-SPME and then analyzed with gas chromatography/mass spectrometry (GC/MS). The experimental conditions--extraction temperature, incubation and exposure time--were optimized. To assess the applicability of the method, fire debris samples were prepared in the smoke density chamber (SDC) and a controlled-atmosphere cone calorimeter. The developed methods were successfully applied to burnt particleboard and carpet samples. The results demonstrate that the procedure that has been developed here is suitable for detecting these ignitable liquids in highly burnt debris. © 2013 American Academy of Forensic Sciences.

Simulated Tip Rub Testing of Low-Density Metal Foam

NASA Technical Reports Server (NTRS)

Bowman, Cheryl L.; Jones, Michael G.

2009-01-01

Preliminary acoustic studies have indicated that low-density, open-cell, metal foams may be suitable acoustic liner material for noise suppression in high by-pass engines. Metal foam response under simulated tip rub conditions was studied to assess whether its durability would be sufficient for the foam to serve both as a rub strip above the rotor as well as an acoustic treatment. Samples represented four metal alloys, nominal cell dimensions ranging from 60 to 120 cells per inch (cpi), and relative densities ranging from 3.4 to 10 percent. The resulting rubbed surfaces were relatively smooth and the open cell structure of the foam was not adversely affected. Sample relative density appeared to have significant influence on the forces induced by the rub event. Acoustic responses of various surface preparations were measured using a normal incidence tube. The results of this study indicate that the foam s open-cell structure was retained after rubbing and that the acoustic absorption spectra variation was minimal.

Method for detection of long-lived radioisotopes in small biochemical samples

DOEpatents

Turteltaub, Kenneth W.; Vogel, John S.; Felton, James S.; Gledhill, Barton L.; Davis, Jay C.

1994-01-01

Disclosed is a method for detection of long-lived radioisotopes in small bio-chemical samples, comprising: a. selecting a biological host in which radioisotopes are present in concentrations equal to or less than those in the ambient biosphere, b. preparing a long-lived radioisotope labeled reactive chemical specie, c. administering said chemical specie to said biologist host in doses sufficiently low to avoid significant overt damage to the biological system thereof, d. allowing a period of time to elapse sufficient for dissemination and interaction of said chemical specie with said host throughout said biological system of said host, e. isolating a reacted fraction of the biological substance from said host in a manner sufficient to avoid contamination of said substance from extraneous sources, f. converting said fraction of biological substance by suitable means to a material which efficiently produces charged ions in at least one of several possible ion sources without introduction of significant isotopic fractionation, and, g. measuring the radioisotope concentration in said material by means of direct isotopic counting.

Preparation of poly-L-lysine functionalized magnetic nanoparticles and their influence on viability of cancer cells

NASA Astrophysics Data System (ADS)

Khmara, I.; Koneracka, M.; Kubovcikova, M.; Zavisova, V.; Antal, I.; Csach, K.; Kopcansky, P.; Vidlickova, I.; Csaderova, L.; Pastorekova, S.; Zatovicova, M.

2017-04-01

This study was aimed at development of biocompatible amino-functionalized magnetic nanoparticles as carriers of specific antibodies able to detect and/or target cancer cells. Poly-L-lysine (PLL)-modified magnetic nanoparticle samples with different PLL/Fe3O4 content were prepared and tested to define the optimal PLL/Fe3O4 weight ratio. The samples were characterized for particle size and morphology (SEM, TEM and DLS), and surface properties (zeta potential measurements). The optimal PLL/Fe3O4 weight ratio of 1.0 based on both zeta potential and DLS measurements was in agreement with the UV/VIS measurements. Magnetic nanoparticles with the optimal PLL content were conjugated with antibody specific for the cancer biomarker carbonic anhydrase IX (CA IX), which is induced by hypoxia, a physiologic stress present in solid tumors and linked with aggressive tumor behavior. CA IX is localized on the cell surface with the antibody-binding epitope facing the extracellular space and is therefore suitable for antibody-based targeting of tumor cells. Here we showed that PLL/Fe3O4 magnetic nanoparticles exhibit cytotoxic activities in a cell type-dependent manner and bind to cells expressing CA IX when conjugated with the CA IX-specific antibody. These data support further investigations of the CA IX antibody-conjugated, magnetic field-guided/activated nanoparticles as tools in anticancer strategies.

Oak kombucha protects against oxidative stress and inflammatory processes.

PubMed

Vázquez-Cabral, B D; Larrosa-Pérez, M; Gallegos-Infante, J A; Moreno-Jiménez, M R; González-Laredo, R F; Rutiaga-Quiñones, J G; Gamboa-Gómez, C I; Rocha-Guzmán, N E

2017-06-25

Black tea infusion is the common substrate for preparing kombucha; however other sources such as oak leaves infusions can be used for the same purpose. Almost any white oak species have been used for medicinal applications by some ethnic groups in Mexico and could be also suitable for preparing kombucha analogues from oak (KAO). The objective of this research was to investigate the antioxidant activity and anti-inflammatory effects of KAO by examining its modulation ability on macrophage-derived TNF-alpha and IL-6. Herbal infusions from oak and black tea were fermented by kombucha consortium during seven days at 28 °C. Chemical composition was determined by LC-ESI-MS/MS. The antioxidant activity of samples against oxidative damage caused by H 2 O 2 in monocytes activated (macrophages) was explored. Additionally, it was determined the anti-inflammatory activity using lipopolysaccharide (LPS) - stimulated macrophages; in particular, the nitric oxide (NO), TNF-alpha, and IL-6 production was assessed. Levels of pro-inflammatory cytokines IL-6 and TNF-alpha were significantly reduced by the sample treatment. Likewise, NO production was lower in treatment with kombucha and KAO compared with LPS-stimulated macrophages. Fermented beverages of oak effectively down-regulated the production of NO, while pro-inflammatory cytokines (TNF-alpha and IL-6) in macrophages were stimulated with LPS. Additionally, phytochemical compounds present in KAO decrease oxidative stress. Copyright © 2017 Elsevier B.V. All rights reserved.

Relationship between surface property and catalytic application of amorphous NiP/Hβ catalyst for n-hexane isomerization

NASA Astrophysics Data System (ADS)

Chen, Jinshe; Duan, Zunbin; Song, Zhaoyang; Zhu, Lijun; Zhou, Yulu; Xiang, Yuzhi; Xia, Daohong

2017-12-01

The amorphous NiP nanoparticles were synthesized and a novel amorphous NiP/Hβ catalyst was prepared successfully further. Due to the superior surface property of amorphous NiP/Hβ catalyst, it exhibited good catalytic application for n-hexane isomerization. The catalytic activity of amorphous NiP/Hβ catalyst was close to that of the prepared Pt/Hβ sample, and better than that of commercial catalyst and crystalline Ni2P/Hβ catalyst. What's more, the amorphous NiP/Hβ catalyst shows high resistance to different sulfur compounds and water on account of its unique surface property. The effect of loading amounts on surface property and catalytic performance was investigated, and the structure-function relationship among them was studied ulteriorly. The results demonstrate that loading amounts have effect on textural property and surface acid property, which further affect the catalytic performance. The 10 wt.% NiP/Hβ sample has appropriate pore structure and acid property with uniformly dispersed NiP nanoparticles on surface, which is helpful for providing suitable synergistic effect. The effects of reaction conditions on surface reactions and the mechanism for n-hexane isomerization were investigated further. Based on these results, the amorphous NiP/Hβ catalyst with superior surface property probably pavesa way to overcome the drawbacks of traditional noble metal catalyst, which shows good catalytic application prospects.

Fabrication of hierarchical porous ZnO-Al2O3 microspheres with enhanced adsorption performance

NASA Astrophysics Data System (ADS)

Lei, Chunsheng; Pi, Meng; Xu, Difa; Jiang, Chuanjia; Cheng, Bei

2017-12-01

Hierarchical porous ZnO-Al2O3 microspheres were fabricated through a simple hydrothermal route. The as-prepared hierarchical porous ZnO-Al2O3 composites were utilized as adsorbents to remove organic dye Congo red (CR) from water. The ZnO-Al2O3 composites had morphology of microspheres with diameters in the range of 12-16 μm, which were assembled by nanosheets with thicknesses of approximately 60 nm. The adsorption kinetics of CR onto the ZnO-Al2O3 composites was properly fitted by the pseudo-second-order kinetic model. The equilibrium adsorption data were perfectly described by the Langmuir isotherm and had a maximum adsorption capacity that reached 397 mg/g, which was significantly higher than the value of the pure alumina (Al2O3) and zinc oxide (ZnO) samples. The superior CR removal efficiency of the ZnO-Al2O3 composites was attributed to its well-developed hierarchical porous structures and larger specific surface area (201 m2/g), which were conducive to the diffusion and adsorption of CR molecules. Moreover, the regeneration study reveals that the ZnO-Al2O3 composites have suitable stability and reusability. The results also indicate that the as-prepared sample can act as a highly effective adsorbent in anionic dye removal from wastewater.

A new carbon-based magnetic material for the dispersive solid-phase extraction of UV filters from water samples before liquid chromatography-tandem mass spectrometry analysis.

PubMed

Piovesana, Susy; Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Samperi, Roberto; Zenezini Chiozzi, Riccardo; Laganà, Aldo

2017-07-01

Magnetic solid-phase extraction is one of the most promising new extraction methods for liquid samples before ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis. Several types of materials, including carbonaceous ones, have been prepared for this purpose. In this paper, for the first time, the preparation, characterization, and sorption capability of Fe 3 O 4 -graphitized carbon black (mGCB) composite toward some compounds of environmental interest were investigated. The synthesized mGCB consisted of micrometric GCB particles with 55 m 2  g -1 surface area bearing some carbonyl and hydroxyl functionalities and the surface partially decorated by Fe 3 O 4 microparticles. The prepared mGCB was firstly tested as an adsorbent for the extraction from surface water of 50 pollutants, including estrogens, perfluoroalkyl compounds, UV filters, and quinolones. The material showed good affinity to many of the tested compounds, except carboxylates and glucoronates; however, some compounds were difficult to desorb. Ten UV filters belonging to the chemical classes of benzophenones and p-aminobenzoates were selected, and parameters were optimized for the extraction of these compounds from surface water before UHPLC-MS/MS determination. Then, the method was validated in terms of linearity, trueness, intra-laboratory precision, and detection and quantification limits. In summary, the method performance (trueness, expressed as analytical recovery, 85-114%; RSD 5-15%) appears suitable for the determination of the selected compounds at the level of 10-100 ng L -1 , with detection limits in the range of 1-5 ng L -1 . Finally, the new method was compared with a published one, based on conventional solid-phase extraction with GCB, showing similar performance in real sample analysis. Graphical Abstract Workflow of the analytical method based on magnetic solid-phase extraction followed by LC-MS/MS determination.

Effect of the type of brewing water on the chemical composition, sensory quality and antioxidant capacity of Chinese teas.

PubMed

Xu, Yong-Quan; Zou, Chun; Gao, Ying; Chen, Jian-Xin; Wang, Fang; Chen, Gen-Sheng; Yin, Jun-Feng

2017-12-01

The physicochemical characteristics, sensory quality, and antioxidant activity of tea infusions prepared with purified water (PW), mineral water (MW), mountain spring water (MSW), and tap water (TW) from Hangzhou were investigated. The results showed that the taste quality, catechin concentration, and antioxidant capacity of green, oolong, and black tea infusions prepared using MW and TW were significantly lower than those prepared using PW. Extraction of catechins and caffeine was reduced with high-conductivity water, while high pH influenced the stability of catechins. PW and MSW were more suitable for brewing green and oolong teas, while MSW, with low pH and moderate ion concentration, was the most suitable water for brewing black tea. Lowering the pH of mineral water partially improved the taste quality and increased the concentration of catechins in the infusions. These results aid selection of the most appropriate water for brewing Chinese teas. Copyright © 2016 Elsevier Ltd. All rights reserved.

Actively preparing for pregnancy is associated with healthier lifestyle of women during the preconception period.

PubMed

Poels, Marjolein; van Stel, Henk F; Franx, Arie; Koster, Maria P H

2017-07-01

To assess whether actively preparing for pregnancy by women is associated with lifestyle changes during the preconception period. retrospective cross-sectional study. primary care community midwifery practice in the Netherlands. convenience sample of 283 women who received antenatal care. the association between pregnancy preparation (defined as searching for information and/or consulting a healthcare provider) and preconception lifestyle changes (healthier diet, folic acid, alcohol and tobacco cessation) was measured and adjusted for age, body mass index and educational level. Almost 60% (n=160) of women acquired preconception information themselves and 25% (n=68) consulted a healthcare provider regarding their pregnancy wish. The former group was significantly more likely to quit drinking (adjusted OR 5.46 (95% CI 1.76-16.96)), improve their diet (adjusted OR 7.84 (95% CI 3.03-20.30)) and use folic acid (adjusted OR 3.90 (95% CI 2.00-7.62)) compared with women who did not prepare for pregnancy. Effect sizes were even larger for women who (also) consulted a healthcare provider with regard to folic acid use, healthier diet and smoking cessation. gathering preconception information, either by women themselves or by means of a PCC consult, is associated with women positively changing lifestyles during the preconception period. we recommend to not solely focus interventions on increasing the uptake of PCC consults, yet providing a suitable offer of preconception health information, which enables women to properly inform themselves. Copyright © 2017 Elsevier Ltd. All rights reserved.

Preparative enantiomer separation of dichlorprop with a cinchona-derived chiral selector employing centrifugal partition chromatography and high-performance liquid chromatography: a comparative study.

PubMed

Gavioli, Elena; Maier, Norbert M; Minguillón, Cristina; Lindner, Wolfgang

2004-10-01

A countercurrent chromatography protocol for support-free preparative enantiomer separation of the herbicidal agent 2-(2,4-dichlorphenoxy)propionic acid (dichlorprop) was developed utilizing a purposefully designed, highly enantioselective chiral stationary-phase additive (CSPA) derived from bis-1,4-(dihydroquinidinyl)phthalazine. Guided by liquid-liquid extraction experiments, a solvent system consisting of 10 mM CSPA in methyl tert-butyl ether and 100 mM sodium phosphate buffer (pH 8.0) was identified as a suitable stationary/mobile-phase combination. This solvent system provided an ideal compromise among stationary-phase retention, enantioselectivity, and well-balanced analyte distribution behavior. Using a commercial centrifugal partition chromatography instrument, complete enantiomer separations of up to 366 mg of racemic dichlorprop could be achieved, corresponding to a sample load being equivalent to the molar amount of CSPA employed. Comparison of the preparative performance characteristics of the CPC protocol with that of a HPLC separation using a silica-supported bis-1,4-(dihydroquinidinyl)phthalazine chiral stationary phase CSP revealed comparable loading capacities for both techniques but a significantly lower solvent consumption for CPC. With respect to productivity, HPLC was found to be superior, mainly due to inherent flow rate restrictions of the CPC instrument. Given that further progress in instrumental design and engineering of dedicated, highly enantioselective CSPAs can be achieved, CPC may offer a viable alternative to CSP-based HPLC for preparative-scale enantiomer separation.

Preparation of fatty acid methyl esters for gas-chromatographic analysis of marine lipids: insight studies.

PubMed

Carvalho, Ana P; Malcata, F Xavier

2005-06-29

Assays for fatty acid composition in biological materials are commonly carried out by gas chromatography, after conversion of the lipid material into the corresponding methyl esters (FAME) via suitable derivatization reactions. Quantitative derivatization depends on the type of catalyst and processing conditions employed, as well as the solubility of said sample in the reaction medium. Most literature pertinent to derivatization has focused on differential comparison between alternative methods; although useful to find out the best method for a particular sample, additional studies on factors that may affect each step of FAME preparation are urged. In this work, the influence of various parameters in each step of derivatization reactions was studied, using both cod liver oil and microalgal biomass as model systems. The accuracies of said methodologies were tested via comparison with the AOCS standard method, whereas their reproducibility was assessed by analysis of variance of (replicated) data. Alkaline catalysts generated lower levels of long-chain unsaturated FAME than acidic ones. Among these, acetyl chloride and BF(3) were statistically equivalent to each other. The standard method, which involves alkaline treatment of samples before acidic methylation with BF(3), provided equivalent results when compared with acidic methylation with BF(3) alone. Polarity of the reaction medium was found to be of the utmost importance in the process: intermediate values of polarity [e.g., obtained by a 1:1 (v/v) mixture of methanol with diethyl ether or toluene] provided amounts of extracted polyunsaturated fatty acids statistically higher than those obtained via the standard method.

Parallel evaluation of broad virus detection methods.

PubMed

Modrof, Jens; Berting, Andreas; Kreil, Thomas R

2014-01-01

The testing for adventitious viruses is of critical importance during development and production of biological products. The recent emergence and ongoing development of broad virus detection methods calls for an evaluation of whether these methods can appropriately be implemented into current adventitious agent testing procedures. To assess the suitability of several broad virus detection methods, a comparative experimental study was conducted: four virus preparations, which were spiked at two different concentrations each into two different cell culture media, were sent to four investigators in a blinded fashion for analysis with broad virus detection methods such as polymerase chain reaction-electrospray ionization mass spectrometry (PCR-ESI/MS), microarray, and two approaches utilizing massively parallel sequencing. The results that were reported by the investigators revealed that all methods were able to identify the majority of samples correctly (mean 83%), with a surprisingly narrow range among the methods, that is, between 72% (PCR-ESI/MS) and 95% (microarray). In addition to the correct results, a variety of unexpected assignments were reported for a minority of samples, again with little variation regarding the methods used (range 20-45%), while false negatives were reported for 0-25% of the samples. Regarding assay sensitivity, the viruses were detected by all methods included in this study at concentrations of about 4-5 log10 quantitative PCR copies/mL, and probably with higher sensitivity in some cases. In summary, the broad virus detection methods investigated were shown to be suitable even for detection of relatively low virus concentrations. However, there is also some potential for the production of false-positive as well as false-negative assignments, which indicates the requirement for further improvements before these methods can be considered for routine use. © PDA, Inc. 2014.

Physico-chemical stability of busulfan in injectable solutions in various administration packages.

PubMed

Houot, Mélanie; Poinsignon, Vianney; Mercier, Lionel; Valade, Cyril; Desmaris, Romain; Lemare, François; Paci, Angelo

2013-03-01

Busulfan is used as part of a conditioning regimen prior to hematopoietic stem cell transplantation for the treatment of certain cancers and immune deficiency syndromes. Due to its instability in aqueous preparations, busulfan for infusion is prepared from a concentrate and has a relatively short shelf life once prepared. The purpose of this study was to identify the most suitable storage container and temperature to maximize the shelf life of busulfan therapeutic infusions prepared from Busilvex(®). Busilvex(®) 6 mg/mL was diluted to 0.55 mg/mL with 0.9 % NaCl and aliquots dispensed into polypropylene syringes, polyvinyl chloride bags, and glass bottles. Three storage temperatures were evaluated: 2-8 °C, 13-15 °C (thermostatically controlled chamber), and room temperature (20 ± 5 °C). At set time points, samples were analysed for busulfan content, using a high-performance liquid chromatography (HPLC) system with ultraviolet detection. The change in pH and osmolarity on storage was also determined, and solutions were inspected visually for formation of a precipitate or colour change. To determine the contribution of precipitation to loss of busulfan content on storage, samples from one time series were treated with the solvent dimethylacetamide prior to HPLC separation and quantitation of busulfan. The results of the active substance content monitoring study over a 48-h period demonstrate that busulfan solution is stable at a 5 % threshold, at 2-8 °C for 16 h in syringes, 14 h in glass bottles, and 6 h in bags. In addition, the period of stability decreases as the temperature increases (4 h at 20 ± 5 °C). The solution is considered to be stable, subject to precipitation liable to be observed regardless of the temperature. The best stability was observed for busulfan solutions placed at 2-8 °C in syringes. This study demonstrated that precipitation, in addition to hydrolysis, has a significant influence on the busulfan content.

Determination of residual acetone and acetone related impurities in drug product intermediates prepared as Spray Dried Dispersions (SDD) using gas chromatography with headspace autosampling (GCHS).

PubMed

Quirk, Emma; Doggett, Adrian; Bretnall, Alison

2014-08-05

Spray Dried Dispersions (SDD) are uniform mixtures of a specific ratio of amorphous active pharmaceutical ingredient (API) and polymer prepared via a spray drying process. Volatile solvents are employed during spray drying to facilitate the formation of the SDD material. Following manufacture, analytical methodology is required to determine residual levels of the spray drying solvent and its associated impurities. Due to the high level of polymer in the SDD samples, direct liquid injection with Gas Chromatography (GC) is not a viable option for analysis. This work describes the development and validation of an analytical approach to determine residual levels of acetone and acetone related impurities, mesityl oxide (MO) and diacetone alcohol (DAA), in drug product intermediates prepared as SDDs using GC with headspace (HS) autosampling. The method development for these analytes presented a number of analytical challenges which had to be overcome before the levels of the volatiles of interest could be accurately quantified. GCHS could be used after two critical factors were implemented; (1) calculation and application of conversion factors to 'correct' for the reactions occurring between acetone, MO and DAA during generation of the headspace volume for analysis, and the addition of an equivalent amount of polymer into all reference solutions used for quantitation to ensure comparability between the headspace volumes generated for both samples and external standards. This work describes the method development and optimisation of the standard preparation, the headspace autosampler operating parameters and the chromatographic conditions, together with a summary of the validation of the methodology. The approach has been demonstrated to be robust and suitable to accurately determine levels of acetone, MO and DAA in SDD materials over the linear concentration range 0.008-0.4μL/mL, with minimum quantitation limits of 20ppm for acetone and MO, and 80ppm for DAA. Copyright © 2014 Elsevier B.V. All rights reserved.

Thiolate-Capped CdSe/ZnS Core-Shell Quantum Dots for the Sensitive Detection of Glucose.

PubMed

Abd Rahman, Samsulida; Ariffin, Nurhayati; Yusof, Nor Azah; Abdullah, Jaafar; Mohammad, Faruq; Ahmad Zubir, Zuhana; Nik Abd Aziz, Nik Mohd Azmi

2017-07-01

A semiconducting water-soluble core-shell quantum dots (QDs) system capped with thiolated ligand was used in this study for the sensitive detection of glucose in aqueous samples. The QDs selected are of CdSe-coated ZnS and were prepared in house based on a hot injection technique. The formation of ZnS shell at the outer surface of CdSe core was made via a specific process namely, SILAR (successive ionic layer adsorption and reaction). The distribution, morphology, and optical characteristics of the prepared core-shell QDs were assessed by transmission electron microscopy (TEM) and spectrofluorescence, respectively. From the analysis, the results show that the mean particle size of prepared QDs is in the range of 10-12 nm and that the optimum emission condition was displayed at 620 nm. Further, the prepared CdSe/ZnS core shell QDs were modified by means of a room temperature ligand-exchange method that involves six organic ligands, L -cysteine, L -histidine, thio-glycolic acid (TGA or mercapto-acetic acid, MAA), mercapto-propionic acid (MPA), mercapto-succinic acid (MSA), and mercapto-undecanoic acid (MUA). This process was chosen in order to maintain a very dense water solubilizing environment around the QDs surface. From the analysis, the results show that the CdSe/ZnS capped with TGA (CdSe/ZnS-TGA) exhibited the strongest fluorescence emission as compared to others; hence, it was tested further for the glucose detection after their treatment with glucose oxidase (GOx) and horseradish peroxidase (HRP) enzymes. Here in this study, the glucose detection is based on the fluorescence quenching effect of the QDs, which is correlated to the oxidative reactions occurred between the conjugated enzymes and glucose. From the analysis of results, it can be inferred that the resultant GOx:HRP/CdSe/ZnS-TGA QDs system can be a suitable platform for the fluorescence-based determination of glucose in the real samples.

PREPARATION OF HIGH-DENSITY, COMPACTIBLE THORIUM OXIDE PARTICLES

DOEpatents

McCorkle, K.H.; Kleinsteuber, A.T.; Schilling, C.E.; Dean, O.C.

1962-05-22

A method is given for preparing millimeter-size, highdensity thorium oxide particles suitable for fabrication into nuclear reactor feel elements by means of vibratory compaction. A thorium oxide gel containing 3.7 to 7 weight per cent residual volatile nitrate and water is prepared by drying a thorium oxide sol. The gel is then slowly heated to a temperature of about 450DEC, and the resulting gel fragments are calcined. The starting sol is prepared by repeated dispersion of oxalate-source thorium oxide in a nitrate system or by dispersion of steam-denitrated thorium oxide in water. (AEC)

Journeys to School Leadership: How Action Learning Identified What Participants Valued in a Year-Long Australian Leadership Development Program Centered on Principles of Good Practice

ERIC Educational Resources Information Center

McCulla, Norman; Degenhardt, Leoni

2016-01-01

The need to identify and suitably prepare teachers to undertake school leadership roles especially as principals is now well documented in the literature. Similarly documented is the general concern about the lack of suitable applicants willing to consider the role. This study raised the question of what might be learnt when a…

Development and in vitro/in vivo evaluation of a novel benznidazole liquid dosage form using a quality-by-design approach.

PubMed

Santos Souza, Higo Fernando; Real, Daniel; Leonardi, Darío; Rocha, Sandra Carla; Alonso, Victoria; Serra, Esteban; Silber, Ariel Mariano; Salomon, Claudio Javier

2017-12-01

To develop an alcohol-free solution suitable for children of benznidazole, the drug of choice for treatment of Chagas disease. In a quality-by-design approach, a systematic optimisation procedure was carried out to estimate the values of the factors leading to the maximum drug concentration. The formulations were analysed in terms of chemical and physical stability and drug content. The final preparation was subjected to an in vivo palatability assay. Mice were infected and treated orally in a murine model. The results showed that benznidazole solubility increased up to 18.38 mg/ml in the optimised co-solvent system. The final formulation remained stable at all three temperatures tested, with suitable drug content and no significant variability. Palatability of the preparation was improved by taste masking of BZL. In vivo studies showed that both parasitaemia and mortality diminished, particularly at a dose of 40 mg/kg/day. Quality by design was a suitable approach to formulate a co-solvent system of benznidazole. The in vivo studies confirmed the suitability of the optimised such solutions to diminish both parasitaemia and mortality. Thus, this novel alternative should be taken into account for further clinical evaluation in all age ranges. © 2017 John Wiley & Sons Ltd.