Sample records for simple preparation method

  1. New Tools to Prepare ACE Cross-section Files for MCNP Analytic Test Problems

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

    Brown, Forrest B.

    Monte Carlo calculations using one-group cross sections, multigroup cross sections, or simple continuous energy cross sections are often used to: (1) verify production codes against known analytical solutions, (2) verify new methods and algorithms that do not involve detailed collision physics, (3) compare Monte Carlo calculation methods with deterministic methods, and (4) teach fundamentals to students. In this work we describe 2 new tools for preparing the ACE cross-section files to be used by MCNP ® for these analytic test problems, simple_ace.pl and simple_ace_mg.pl.

  2. A simple agar plate preparation for effective transfer of Ureaplasma colonies onto nitrocellulose membranes for colony immunoblotting.

    PubMed

    Zimmerman, Carl-Ulrich R; Stiedl, Thomas; Spergser, Joachim; Rosengarten, Renate

    2014-09-01

    A simple method for preparing agar plates is presented, which allows an efficient transfer of Ureaplasma colonies to nitrocellulose membranes for subsequent immunological detection. This simple and reproducible procedure was used to demonstrate antigenic variation in the phase-variable mba-locus of Ureaplasma parvum serovar 3. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. [Developments in preparation and experimental method of solid phase microextraction fibers].

    PubMed

    Yi, Xu; Fu, Yujie

    2004-09-01

    Solid phase microextraction (SPME) is a simple and effective adsorption and desorption technique, which concentrates volatile or nonvolatile compounds from liquid samples or headspace of samples. SPME is compatible with analyte separation and detection by gas chromatography, high performance liquid chromatography, and other instrumental methods. It can provide many advantages, such as wide linear scale, low solvent and sample consumption, short analytical times, low detection limits, simple apparatus, and so on. The theory of SPME is introduced, which includes equilibrium theory and non-equilibrium theory. The novel development of fiber preparation methods and relative experimental techniques are discussed. In addition to commercial fiber preparation, different newly developed fabrication techniques, such as sol-gel, electronic deposition, carbon-base adsorption, high-temperature epoxy immobilization, are presented. Effects of extraction modes, selection of fiber coating, optimization of operating conditions, method sensitivity and precision, and systematical automation, are taken into considerations in the analytical process of SPME. A simple perspective of SPME is proposed at last.

  4. A convenient Simple Method for Synthesis of Meta-iodobenzylguanidine (MIBG).

    PubMed

    Sheikholislam, Zahra; Soleimani, Zohreh; Moghimi, Abolghasem; Shahhosseini, Soraya

    2013-01-01

    Radioiodinated meta-iodobenzylguanidine (MIBG) is one of the important radiopharmaceuticals in Nuclear Medicine. [(123/131)I] MIBG is used for imaging of Adrenal medulla, studying heart sympathetic nerves, treatment of pheochromacytoma and neuroblastoma. For clinical application, radioiodinated MIBG is prepared through isotopic exchange method, which includes replacement of radioactive iodine in a nucleophilic substitution reaction with cold iodine ((127)I). The unlabelled MIBG hemisulfate is synthesized by the procedure described by Wieland et al. (1980). The availability of a more practical and cost-effective procedure for MIBG preparation encouraged us to study the MIBG synthesis methods. In this study the preparation of MIBG through different methods were evaluated and a new method, which is one step, simple and cost-effective is introduced. The method has ability to be scaled up for production of unlabelled MIBG.

  5. [Simple method for precognition of drug interaction between oral iron and phenolic hydroxyl group-containing drugs].

    PubMed

    Sunagane, Nobuyoshi; Yoshinobu, Etsuko; Murayama, Nobuko; Terawaki, Yasufumi; Kamimura, Naoki; Uruno, Tsutomu

    2005-02-01

    In the present study, we devised a simple method for detecting the drug interaction between oral iron preparations and phenolic hydroxyl group-containing drugs, using the coloring reaction as indicator, due to the formation of complexes or chelates. In the method, oral iron preparations and test drugs in amounts as much as single dose for adults were added to 10 ml of purified water to make sample suspensions for testing. Thirty minutes after mixing an oral iron suspension and a test drug suspension, the change of color in the mixture was observed macroscopically and graded as 0 to 3, with a marked color change judged as grade 3 and no color change as grade 0. Screening of 14 test drugs commonly used orally was carried out. When using sodium ferrous citrate preparations as oral iron, 5 were classified as grade 3, 2 as grade 2, 4 as grade 1, and 3 as grade 0, respectively. To verify usefulness of the method, the interactions suggested by screening were pharmacokinetically assessed by measuring serum concentrations of the drug in mice. When a levodopa or droxidopa preparation, judged as grade 3 in screening, was concomitantly administered with an iron preparation, a significant reduction in bioavailability of the test drug was observed, indicating possible drug interaction between the test drug and oral iron. Combined administration of an acetaminophen preparation, judged as grade 1, and oral iron preparation showed no influence on the bioavailability of the test drug, implying no detectable interactions between them. In conclusion, the simple method devised in the present study is useful for precognition of drug interactions between oral iron preparations and phenolic hydroxyl group-containing drugs, and the drugs with a higher grade in screening may induce drug interactions with oral iron.

  6. [Isolation and purification of seven catechin compounds from fresh tea leaves by semi-preparative liquid chromatography].

    PubMed

    Gong, Zhihong; Chen, Si; Gao, Jiangtao; Li, Meihong; Wang, Xiaxia; Lin, Jun; Yu, Xiaomin

    2017-11-08

    An effective and simple method was established to simultaneously purify seven tea catechins (gallocatechin (GC), epigallocatechin (EGC), catechin (C), epigallocatechin-3- O -gallate (EGCG), epicatechin (EC), epigallocatechin-3- O -(3- O -methyl)-gallate (EGCG3"Me) and epicatechin-3- O -gallate (ECG)) from fresh tea leaves by semi-preparative high performance liquid chromatography (HPLC). Fresh leaves of Tieguanyin tea were successively extracted with methanol and chloroform. Then crude catechins were precipitated from the aqueous fraction of chloroform extraction by adding lead subacetate. Crude catechins were used for the isolation of the seven target catechin compounds by semi-preparative HPLC. Methanol-water and acetonitrile-water were sequentially used as mobile phases. After two rounds of semi-preparative HPLC, all target compounds were achieved with high purities (>90%). The proposed method was tested on two additional tea cultivars and showed similar results. This method demonstrated a simple and efficient strategy based on solvent extraction, ion precipitation and semi-preparative HPLC for the preparation of multiple catechins from tea leaves.

  7. Evaluation of a QuECHERS-like extraction approach for the determination of PBDEs in mussels by immuno-assay-based screening methods

    USDA-ARS?s Scientific Manuscript database

    A sample preparation method was evaluated for the determination of polybrominated diphenyl ethers (PBDEs) in mussel samples, by using colorimetric and electrochemical immunoassay-based screening methods. A simple sample preparation in conjunction with a rapid screening method possesses the desired c...

  8. The structural properties of barium cobalt hexaferrite powder prepared by a simple heat treatment method

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

    Chauhan, Chetna, E-mail: chetna.chauhan@nirmauni.ac.in; Jotania, Rajshree, E-mail: rbjotania@gmail.com

    2016-05-06

    The W-type barium hexaferrite was prepared using a simple heat treatment method. The precursor was calcinated at 650°C for 3 hours and then slowly cooled to room temperature in order to obtain barium cobalt hexaferrite powder. The prepared powder was characterised by different experimental techniques like XRD, FTIR and SEM. The X-ray diffractogram of the sample shows W-and M phases. The particle size calculated by Debye Scherrer formula. The FTIR spectra of the sample was taken at room temperature by using KBr pallet method which confirms the formation of hexaferrite phase. The morphological study on the hexaferrite powder was carriedmore » out by SEM analysis.« less

  9. Dehydration Polymerization for Poly(hetero)arene Conjugated Polymers.

    PubMed

    Mirabal, Rafael A; Vanderzwet, Luke; Abuadas, Sara; Emmett, Michael R; Schipper, Derek

    2018-02-18

    The lack of scalable and sustainable methods to prepare conjugated polymers belies their importance in many enabling technologies. Accessing high-performance poly(hetero)arene conjugated polymers by dehydration has remained an unsolved problem in synthetic chemistry and has historically required transitional-metal coupling reactions. Herein, we report a dehydration method that allows access to conjugated heterocyclic materials. By using the technique, we have prepared a series of small molecules and polymers. The reaction avoids using transition metals, proceeds at room temperature, the only required reactant is a simple base and water is the sole by-product. The dehydration reaction is technically simple and provides a sustainable and straightforward method to prepare conjugated heteroarene motifs. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. 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.

  11. [Prognostic value on recovery rates for the application of sperm preparation techniques and their evaluation in sperm function].

    PubMed

    Barroso, Gerardo; Chaya, Miguel; Bolaños, Rubén; Rosado, Yadira; García León, Fernando; Ibarrola, Eduardo

    2005-05-01

    To evaluate sperm recovery and total sperm motility in three different sperm preparation techniques (density gradient, simple washing and swim-up). A total of 290 subjects were randomly evaluated from November 2001 to March 2003. The density gradient method required Isolate (upper and lower layers). Centrifugation was performed at 400 g for 10 minutes and evaluation was done using the Makler counting chamber. The simple washing method included the use of HTF-M complemented with 7.5% of SSS, with centrifugation at 250 g, obtaining at the end 0.5 mL of the sperm sample. The swim-up method required HTF-M complemented with 7.5% of SSS, with an incubation period of 60 minutes at 37 degrees C. The demographic characteristics evaluated through their standard error, 95% ICC, and 50th percentile were similar. The application of multiple comparison tests and analysis of variance showed significant differences between the sperm preparations before and after capacitation. It was observed a superior recovery rate with the density gradient and swim-up methods; nevertheless, the samples used for the simple washing method showed a diminished sperm recovery from the original sample. Sperm preparation techniques have become very useful in male infertility treatments allowing higher sperm recovery and motility rates. The seminal parameters evaluated from the original sperm sample will determine the best sperm preparation technique in those patients who require it.

  12. A facile one-pot solvothermal method for synthesis of magnetically recoverable Pd-Fe3O4 hybrid nanocatalysts for the Mizoroki-Heck reaction

    NASA Astrophysics Data System (ADS)

    Zhen, Fangchen; Ran, Maofei; Chu, Wei; Jiang, Chengfa; Sun, Wenjing

    2018-03-01

    Pd-Fe3O4 hybrid nanostructures were prepared using a simple one-pot hydrothermal method. The prepared materials were characterized by Fourier transform-infrared spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy, inductively coupled plasma, N2 adsorption-desorption, and vibrating sample magnetometry. This self-assembled nanosystem acted as an efficient magnetically recyclable noble metal-based multi-functional nanocatalyst. It showed excellent catalytic activity and stability for the Heck reaction of iodobenzene and styrene under mild conditions. The methods used to prepare the Pd-Fe3O4 catalysts were simple and low-cost, which will be useful for the large-scale development and application of a magnetically recoverable Pd catalyst.

  13. Simple Sodium Dodecyl Sulfate-Assisted Sample Preparation Method for LC-MS-based Proteomic Applications

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

    Zhou, Jianying; Dann, Geoffrey P.; Shi, Tujin

    2012-03-10

    Sodium dodecyl sulfate (SDS) is one of the most popular laboratory reagents used for highly efficient biological sample extraction; however, SDS presents a significant challenge to LC-MS-based proteomic analyses due to its severe interference with reversed-phase LC separations and electrospray ionization interfaces. This study reports a simple SDS-assisted proteomic sample preparation method facilitated by a novel peptide-level SDS removal protocol. After SDS-assisted protein extraction and digestion, SDS was effectively (>99.9%) removed from peptides through ion substitution-mediated DS- precipitation with potassium chloride (KCl) followed by {approx}10 min centrifugation. Excellent peptide recovery (>95%) was observed for less than 20 {mu}g of peptides.more » Further experiments demonstrated the compatibility of this protocol with LC-MS/MS analyses. The resulting proteome coverage from this SDS-assisted protocol was comparable to or better than those obtained from other standard proteomic preparation methods in both mammalian tissues and bacterial samples. These results suggest that this SDS-assisted protocol is a practical, simple, and broadly applicable proteomic sample processing method, which can be particularly useful when dealing with samples difficult to solubilize by other methods.« less

  14. Preparation and Optoelectrical Properties of p-CuO/n-Si Heterojunction by a Simple Sol-Gel Method

    NASA Astrophysics Data System (ADS)

    He, Bo; Xu, Jing; Ning, Huanpo; Zhao, Lei; Xing, Huaizhong; Chang, Chien-Cheng; Qin, Yuming; Zhang, Lei

    The Cuprous oxide (CuO) thin film was prepared on texturized Si wafer by a simple sol-gel method to fabricate p-CuO/n-Si heterojunction photoelectric device. The novel sol-gel method is very cheap and convenient. The structural, optical and electrical properties of the CuO film were studied by X-ray diffraction (XRD), Scanning Electron Microscope (SEM), X-ray photoelectron spectroscopy (XPS), UV-Vis spectrophotometer and Hall effect measurement. A good nonlinear rectifying behavior is obtained for the p-CuO/n-Si heterojunction. Under reverse bias, good photoelectric behavior is obtained.

  15. Preparation and characterizations of activated carbon monolith from rubber wood and its effect on supercapacitor performances

    NASA Astrophysics Data System (ADS)

    Taer, E.; Taslim, R.; Deraman, M.

    2016-02-01

    Preparation of activated carbon monolith (ACM) from rubber wood was investigated. Two kind of preparation method were carried out by pre-carbonized of rubber wood saw dust and rubber wood material as it is naturally. The samples were prepared with pelletizing method and small cutting of rubber wood in cross sectional method. Both of samples were characterized by physical and electrochemical technique. The physical properties such as morphology and porosity were investigated. The electrochemical properties of both samples such as equivalent series resistances (ESR) and specific capacitances were also compared. In conclusion, this study showed that both of different preparation method would propose a simple method of ACM electrode preparation technique for supercapacitor applications.

  16. An alternative simple method for preparing and preserving cross-section of leaves and roots in herbaceous plants: Case study in Orchidaceae

    NASA Astrophysics Data System (ADS)

    Metusala, D.

    2017-07-01

    This alternative method provides a simple and faster procedure for preparing cross-sections of leaves and roots in herbaceous plants, especially for living specimens of orchids (Orchidaceae). This method used a clamp-on hand sliding microtome to make cross-sections of leaves and roots, with sections preserved inside the microtubes containing preservation liquid. This preservation technique allowed the sections to be restained and to be used for further usage in future. This method was more practical than the paraffin embedding method because it does not need the additional steps of paraffin embedding and deparaffinization. It may also provide better cross-section results than free-hand sectioning method. The procedure is very feasible and is recommended for use in plant anatomy observation.

  17. A simple method for the preparation of activated carbon fibers coated with graphite nanofibers.

    PubMed

    Kim, Byung-Joo; Park, Soo-Jin

    2007-11-15

    A simple method is described for the preparation of activated carbon fibers (ACFs) coated with graphite nanofibers (GNFs). Low-pressure-plasma mixed-gas (Ar/O2) treatment of the ACFs led to the growth of GNFs on their surface. The growth was greater at higher power inputs, and from TEM observations the GNFs were seen to be of herringbone type. It was found that the N2 adsorption capacity of the ACFs did not sharply decrease, and that volume resistivity of the ACFs enhanced as a result of this treatment.

  18. Preparation of a porous Sn@C nanocomposite as a high-performance anode material for lithium-ion batteries

    NASA Astrophysics Data System (ADS)

    Zhang, Yanjun; Jiang, Li; Wang, Chunru

    2015-07-01

    A porous Sn@C nanocomposite was prepared via a facile hydrothermal method combined with a simple post-calcination process, using stannous octoate as the Sn source and glucose as the C source. The as-prepared Sn@C nanocomposite exhibited excellent electrochemical behavior with a high reversible capacity, long cycle life and good rate capability when used as an anode material for lithium ion batteries.A porous Sn@C nanocomposite was prepared via a facile hydrothermal method combined with a simple post-calcination process, using stannous octoate as the Sn source and glucose as the C source. The as-prepared Sn@C nanocomposite exhibited excellent electrochemical behavior with a high reversible capacity, long cycle life and good rate capability when used as an anode material for lithium ion batteries. Electronic supplementary information (ESI) available: Detailed experimental procedure and additional characterization, including a Raman spectrum, TGA curve, N2 adsorption-desorption isotherm, TEM images and SEM images. See DOI: 10.1039/c5nr03093e

  19. Large-scale preparation of strawberry-like, AgNP-doped SiO2 microspheres using the electrospraying method

    NASA Astrophysics Data System (ADS)

    Ma, Zhijun; Ji, Huijiao; Tan, Dezhi; Dong, Guoping; Teng, Yu; Zhou, Jiajia; Guan, Miaojia; Qiu, Jianrong; Zhang, Ming

    2011-07-01

    In this paper, we report on a novel strategy for the preparation of silver nanoparticle-doped SiO2 microspheres (Ag-SMSs) with an interesting strawberry-like morphology using a simple and efficient electrospraying method. SEM (scanning electron microscopy), TEM (transmission electron microscopy), XRD (x-ray diffraction), EDS (energy-dispersive spectroscopy) and UV-vis spectra (ultraviolet-visible spectra) were applied to investigate the morphology, structure, composition and optical properties of the hybrid microspheres, and E. coli (Escherichia coli) was used as a model microbe to evaluate their antibacterial ability. The results showed that the Ag-SMSs were environmentally stable and washing resistant. The Ag-SMSs exhibited effective inhibition against proliferation of E. coli, and their antibacterial ability could be well preserved for a long time. The environmental stability, washing resistance, efficient antibacterial ability and simple but productive preparation method endowed the Ag-SMSs with great potential for practical biomedical applications.

  20. A simple method to prepare magnetic modified beer yeast and its application for cationic dye adsorption.

    PubMed

    Yu, Jun-Xia; Wang, Li-Yan; Chi, Ru-An; Zhang, Yue-Fei; Xu, Zhi-Gao; Guo, Jia

    2013-01-01

    The purpose of this research is to use a simple method to prepare magnetic modified biomass with good adsorption performances for cationic ions. The magnetic modified biomass was prepared by two steps: (1) preparation of pyromellitic dianhydride (PMDA) modified biomass in N, N-dimethylacetamide solution and (2) preparation of magnetic PMDA modified biomass by a situ co-precipitation method under the assistance of ultrasound irradiation in ammonia water. The adsorption potential of the as-prepared magnetic modified biomass was analyzed by using cationic dyes: methylene blue and basic magenta as model dyes. Optical micrograph and x-ray diffraction analyses showed that Fe(3)O(4) particles were precipitated on the modified biomass surface. The as-prepared biosorbent could be recycled easily by using an applied magnetic field. Titration analysis showed that the total concentration of the functional groups on the magnetic PMDA modified biomass was calculated to be 0.75 mmol g(-1) by using the first derivative method. The adsorption capacities (q(m)) of the magnetic PMDA modified biomass for methylene blue and basic magenta were 609.0 and 520.9 mg g(-1), respectively, according to the Langmuir equation. Kinetics experiment showed that adsorption could be completed within 150 min for both dyes. The desorption experiment showed that the magnetic sorbent could be used repeatedly after regeneration. The as-prepared magnetic modified sorbent had a potential in the dyeing industry wastewater treatment.

  1. Simple synthesis of graphene nanocomposites MgO-rGO and Fe2O3-rGO for multifunctional applications

    NASA Astrophysics Data System (ADS)

    Abdel-Aal, Seham K.; Ionov, Andrey; Mozhchil, R. N.; Naqvi, Alim H.

    2018-05-01

    Hummer's method was used to prepare graphene oxide (GO) by chemical exfoliation of graphite. Simple precipitation method was used for the preparation of hybrid nanocomposites MgO-rGO and Fe2O3-rGO. A 0.3 Molar of corresponding metal nitrate solution and GO solution are used for the preparation process. XRD, FT-IR, and XPS were used to characterize the prepared nanocomposites. The reduction of GO into reduced rGO in the formed nanocomposites was confirmed. Morphological characterization showed the formation of needle-shaped nanocrystals of MgO successfully grown on graphene nanosheet with average crystallite size 8.4 nm. Hematite nanocomposite Fe2O3-rGO forms rod-shaped crystals with average crystallite size 27.5 nm. The saturation magnetization observed for Fe2O3-rGO is less than reported value for the pure Fe2O3 nanoparticles. Thermal properties of as-prepared hybrid nanocomposites MgO-rGO and Fe2O3-rGO showed thermal stability of the prepared nanocomposite over long range of temperature.

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

    PubMed

    Piotrowska, N; Goslar, T

    2002-12-01

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

  3. A simple method for multiday imaging of slice cultures.

    PubMed

    Seidl, Armin H; Rubel, Edwin W

    2010-01-01

    The organotypic slice culture (Stoppini et al. A simple method for organotypic cultures of nervous tissue. 1991;37:173-182) has become the method of choice to answer a variety of questions in neuroscience. For many experiments, however, it would be beneficial to image or manipulate a slice culture repeatedly, for example, over the course of many days. We prepared organotypic slice cultures of the auditory brainstem of P3 and P4 mice and kept them in vitro for up to 4 weeks. Single cells in the auditory brainstem were transfected with plasmids expressing fluorescent proteins by way of electroporation (Haas et al. Single-cell electroporation for gene transfer in vivo. 2001;29:583-591). The culture was then placed in a chamber perfused with oxygenated ACSF and the labeled cell imaged with an inverted wide-field microscope repeatedly for multiple days, recording several time-points per day, before returning the slice to the incubator. We describe a simple method to image a slice culture preparation during the course of multiple days and over many continuous hours, without noticeable damage to the tissue or photobleaching. Our method uses a simple, inexpensive custom-built insulator constructed around the microscope to maintain controlled temperature and uses a perfusion chamber as used for in vitro slice recordings. (c) 2009 Wiley-Liss, Inc.

  4. Preparation of carbon nanoparticles and carbon nitride from high nitrogen compound

    DOEpatents

    Huynh, My Hang V [Los Alamos, NM; Hiskey, Michael A [Los Alamos, NM

    2009-09-01

    The high-nitrogen compound 3,6-di(azido)-1,2,4,5-tetrazine (DiAT) was synthesized by a relatively simple method and used as a precursor for the preparation of carbon nanospheres and nanopolygons, and nitrogen-rich carbon nitrides.

  5. Preparation and Characterization of a Small Library of Thermally-Labile End-Caps for Variable-Temperature Triggering of Self-Immolative Polymers.

    PubMed

    Taimoory, S Maryamdokht; Sadraei, S Iraj; Fayoumi, Rose Anne; Nasri, Sarah; Revington, Matthew; Trant, John F

    2018-04-20

    The reaction between furans and maleimides has increasingly become a method of interest as its reversibility makes it a useful tool for applications ranging from self-healing materials, to self-immolative polymers, to hydrogels for cell culture and for the preparation of bone repair. However, most of these applications have relied on simple monosubstituted furans and simple maleimides and have not extensively evaluated the potential thermal variability inherent in the process that is achievable through simple substrate modification. A small library of cycloadducts suitable for the above applications was prepared, and the temperature dependence of the retro-Diels-Alder processes was determined through in situ 1 H NMR analyses complemented by computational calculations. The practical range of the reported systems ranges from 40 to >110 °C. The cycloreversion reactions are more complex than would be expected based on simple trends expected based on frontier molecular orbital analyses of the materials.

  6. Technical Advances in Intracellular Detection Using Immuno-Gold Particles: Simple Cryofixation with Metal Contact Quick Freezing.

    PubMed

    Song, Chihong; Lee, Ju Huck; Jun, Sangmi; Chung, Jeong Min; Hyun, Jaekyung; Jung, Hyun Suk

    2016-05-01

    The preparation of biological specimens using cryofixation techniques ensures excellent visibility of intracellular structures and preserves the antigenic sites of subcellular molecules. Hence, cryofixation is an effective method of preparing samples for analyses using antibodies conjugated to gold nanoparticles that are designed to detect the localization of specific target molecules within cells. However, cryofixation cannot be utilized easily because it requires expensive equipment and skilled technologists, resulting in a high level of expense for researchers. Here, we describe a simple technical approach to cryofixation that uses metal contact quick freezing followed by a modified freeze substitution technique and immuno-gold labeling electron microscopy. Micrograph images of cells prepared using this modified cryofixation method demonstrated its superiority over chemical fixation for high contrast visualization of the morphologies of cellular components and preservation of antigenicity for immuno-gold labeling. This report provides valuable technical information related to the advancement of metal contact quick freezing techniques, which can be used to visualize biomedical events of interest in an easy, simple, and rapid manner.

  7. In-situ polymerization PLOT columns I: divinylbenzene

    NASA Technical Reports Server (NTRS)

    Shen, T. C.

    1992-01-01

    A novel method for preparation of porous-layer open-tubular (PLOT) columns is described. The method involves a simple and reproducible, straight-forward in-situ polymerization of monomer directly on the metal tube.

  8. Efficient solar-assisted O2 reduction by a cofacial iron porphyrin dimer integrated to a p-CuBi2O4 photocathode prepared by a simple novel method.

    PubMed

    Zahran, Zaki N; Mohamed, Eman A; Naruta, Yoshinori; Haleem, Ashraf

    2017-10-04

    A cofacial iron porphyrin hetero-dimer, Fe2TPFPP-TMP showed high electro-catalytic activity, selectivity, and stability for the O2 reduction to H2O both in homogeneous non-aqueous and heterogeneous neutral aqueous solutions. Moreover, when it is integrated to FTO/p-CuBi2O4 (FTO = fluorine doped tin oxide) photocathode prepared by a simple novel method, a remarkable efficient solar-assisted O2 reduction is achieved in neutral potassium phosphate (KPi) or basic NaOH solutions saturated with O2. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Sonicated Diagnostic Immunoblot for Bartonellosis

    PubMed Central

    Mallqui, Vania; Speelmon, Emily C.; Verástegui, Manuela; Maguiña-Vargas, Ciro; Pinell-Salles, Paula; Lavarello, Rosa; Delgado, Jose; Kosek, Margaret; Romero, Sofia; Arana, Yanina; Gilman, Robert H.

    2000-01-01

    Two simple Bartonella bacilliformis immunoblot preparation methods were developed. Antigen was prepared by two different methods: sonication of whole organisms or glycine extraction. Both methods were then tested for sensitivity and specificity. Well-defined control sera were utilized in the development of these diagnostic immunoblots, and possible cross-reactions were thoroughly examined. Sera investigated for cross-reaction with these diagnostic antigens were drawn from patients with brucellosis, chlamydiosis, Q fever, and cat scratch disease, all of whom were from regions where bartonellosis is not endemic. While both immunoblots yielded reasonable sensitivity and high specificity, we recommend the use of the sonicated immunoblot, which has a higher sensitivity when used to detect acute disease and produces fewer cross-reactions. The sonicated immunoblot reported here is 94% sensitive to chronic bartonellosis and 70% sensitive to acute bartonellosis. In a healthy group, it is 100% specific. This immunoblot preparation requires a simple sonication protocol for the harvesting of B. bacilliformis antigens and is well suited for use in regions of endemicity. PMID:10618267

  10. A validated high performance thin layer chromatography method for determination of yohimbine hydrochloride in pharmaceutical preparations

    PubMed Central

    Badr, Jihan M.

    2013-01-01

    Background: Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations. Materials and Method: In the present work, a simple and sensitive high performance thin layer chromatographic method is developed for determination of yohimbine (occurring as yohimbine hydrochloride) in pharmaceutical preparations and validated according to International Conference of Harmonization (ICH) guidelines. The method employed thin layer chromatography aluminum sheets precoated with silica gel as the stationary phase and the mobile phase consisted of chloroform:methanol:ammonia (97:3:0.2), which gave compact bands of yohimbine hydrochloride. Results: Linear regression data for the calibration curves of standard yohimbine hydrochloride showed a good linear relationship over a concentration range of 80–1000 ng/spot with respect to the area and correlation coefficient (R2) was 0.9965. The method was evaluated regarding accuracy, precision, selectivity, and robustness. Limits of detection and quantitation were recorded as 5 and 40 ng/spot, respectively. The proposed method efficiently separated yohimbine hydrochloride from other components even in complex mixture containing powdered plants. The amount of yohimbine hydrochloride ranged from 2.3 to 5.2 mg/tablet or capsule in preparations containing the pure alkaloid, while it varied from zero (0) to 1.5–1.8 mg/capsule in dietary supplements containing powdered yohimbe bark. Conclusion: We concluded that this method employing high performance thin layer chromatography (HPTLC) in quantitative determination of yohimbine hydrochloride in pharmaceutical preparations is efficient, simple, accurate, and validated. PMID:23661986

  11. A simple and selective resonance Rayleigh scattering-energy transfer spectral method for determination of trace neomycin sulfate using Cu2O particle as probe

    NASA Astrophysics Data System (ADS)

    Ouyang, Huixiang; Liang, Aihui; Jiang, Zhiliang

    2018-02-01

    The stable Cu2O nanocubic (Cu2ONC) sol was prepared, based on graphene oxide (GO) catalysis of glucose-Fehling's reagent reaction, and its absorption and resonance Rayleigh scattering (RRS) spectra, transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) were examined. Using the as-prepared Cu2ONC as RRS probe, and coupling with the neomycin sulfate (NEO) complex reaction, a new, simple, sensitive and selective RRS-energy transfer (RRS-ET) method was established for detection of neomycin sulfate, with a linear range of 1.4-112 μM and a detection limit of 0.4 μM. The method has been applied to the detection of neomycin sulfate in samples with satisfactory results.

  12. Determination of the Effect of Various Modes of Cooking on the Vitamin C Content of a Common Food, Green Pepper: An Introductory Biochemistry Experiment.

    ERIC Educational Resources Information Center

    Johnson, Eric R.

    1988-01-01

    Describes a laboratory experiment that measures the amount of ascorbic acid destroyed by food preparation methods (boiling and steaming). Points out that aqueous extracts of cooked green pepper samples can be analyzed for ascorbic acid by a relatively simple redox titration. Lists experimental procedure for four methods of preparation. (MVL)

  13. Structure and magnetic/electrochemical properties of Cu-doped BiFeO3 nanoparticles prepared by a simple solution method

    NASA Astrophysics Data System (ADS)

    Khajonrit, Jessada; Phumying, Santi; Maensiri, Santi

    2016-06-01

    BiFe1- x Cu x O3 (x = 0, 0.05, 0.1, 0.2, and 0.3) nanoparticles were prepared by a simple solution method. The prepared nanoparticles were characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), Brunauer-Emmett-Teller (BET) method analysis using the Barret-Joyner-Halenda (BJH) model, and X-ray absorption spectroscopy (XAS). Magnetization properties were obtained using a vibrating sample magnetometer (VSM) at room temperature. Magnetization was clearly enhanced by increasing Cu content and decreasing particle size. Zero-field-cooled (ZFC) and field-cooled (FC) temperature-dependent magnetization measurements showed that blocking temperature increased with increasing Cu content. Electrochemical properties were investigated by cyclic voltammetry (CV) and the galvanostatic charge-discharge (GCD) method. The performance of the fabricated supercapacitor was improved for the BiFe0.95Cu0.05O3 electrode. The highest specific capacitance was 568.13 F g-1 at 1 A g-1 and the capacity retention was 77.13% after 500 cycles.

  14. Studies on wettability of polypropylene/methyl-silicone composite film and polypropylene monolithic material.

    PubMed

    Hou, Weixin; Mu, Bo; Wang, Qihua

    2008-11-01

    A polypropylene/methyl-silicone superhydrophobic surface was prepared using a simple casting method. Varying the ratio of polypropylene and methyl-silicone results in different surface microstructure. The wetting behavior of the as-prepared surface was investigated. A polypropylene monolithic material was also prepared. Its superhydrophobicity still retains when the material was cut or abraded. The as-prepared material can also be used to separate some organic solvents from water.

  15. A novel inorganic precipitation-peptization method for VO2 sol and VO2 nanoparticles preparation: Synthesis, characterization and mechanism.

    PubMed

    Li, Yao; Jiang, Peng; Xiang, Wei; Ran, Fanyong; Cao, Wenbin

    2016-01-15

    In this paper, a simple, safe and cost-saving precipitation-peptization method was proposed to prepare VO2 sol by using inorganic VOSO4-NH3⋅H2O-H2O2 reactants system in air under room temperature. In this process, VOSO4 was firstly precipitated to form VO(OH)2, then monometallic species of VO(O2)(OH)(-) were formed through the coordination between VO(OH)2 and H2O2. The rearrangement of VO(O2)(OH)(-) in a nonplanar pattern and intermolecular condensation reactions result in multinuclear species. Finally, VO2 sol is prepared through the condensation reactions between the multinuclear species. After drying the obtained sol at 40°C, VO2 xerogel exhibiting monoclinic crystal structure with the space group of C2/m was prepared. The crystal structure of VO2 nanoparticles was transferred to monoclinic crystal structure with the space group of P21/c (VO2(M)) by annealing the xerogel at 550°C. Both XRD and TEM analysis indicated that the nanoparticles possess good crystallinity with crystallite size of 34.5nm as estimated by Scherrer's method. These results suggest that the VO2 sol has been prepared successfully through the proposed simple method. Copyright © 2015 Elsevier Inc. All rights reserved.

  16. Preparation and Evaluation of Solid Dispersion Tablets by a Simple and Manufacturable Wet Granulation Method Using Porous Calcium Silicate.

    PubMed

    Fujimoto, Yumi; Hirai, Nobuaki; Takatani-Nakase, Tomoka; Takahashi, Koichi

    2016-01-01

    The aim of this study was to prepare and evaluate solid dispersion tablets containing a poorly water-soluble drug using porous calcium silicate (PCS) by a wet granulation method. Nifedipine (NIF) was used as the model poorly water-soluble drug. Solid dispersion tablets were prepared with the wet granulation method using ethanol and water by a high-speed mixer granulator. The binder and disintegrant were selected from 7 and 4 candidates, respectively. The dissolution test was conducted using the JP 16 paddle method. The oral absorption of NIF was studied in fasted rats. Xylitol and crospovidone were selected as the binder and disintegrant, respectively. The dissolution rates of NIF from solid dispersion formulations were markedly enhanced compared with NIF powder and physical mixtures. Powder X-ray diffraction (PXRD) confirmed the reduced crystallinity of NIF in the solid dispersion formulations. Fourier transform infrared (FT-IR) showed the physical interaction between NIF and PCS in the solid dispersion formulations. NIF is present in an amorphous state in granules prepared by the wet granulation method using water. The area under the plasma concentration-time curve (AUC) and peak concentration (C(max)) values of NIF after dosing rats with the solid dispersion granules were significantly greater than those after dosing with NIF powder. The solid dispersion formulations of NIF prepared with PCS using the wet granulation method exhibited accelerated dissolution rates and superior oral bioavailability. This method is very simple, and may be applicable to the development of other poorly water-soluble drugs.

  17. A validated high performance thin layer chromatography method for determination of yohimbine hydrochloride in pharmaceutical preparations.

    PubMed

    Badr, Jihan M

    2013-01-01

    Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations. In the present work, a simple and sensitive high performance thin layer chromatographic method is developed for determination of yohimbine (occurring as yohimbine hydrochloride) in pharmaceutical preparations and validated according to International Conference of Harmonization (ICH) guidelines. The method employed thin layer chromatography aluminum sheets precoated with silica gel as the stationary phase and the mobile phase consisted of chloroform:methanol:ammonia (97:3:0.2), which gave compact bands of yohimbine hydrochloride. Linear regression data for the calibration curves of standard yohimbine hydrochloride showed a good linear relationship over a concentration range of 80-1000 ng/spot with respect to the area and correlation coefficient (R(2)) was 0.9965. The method was evaluated regarding accuracy, precision, selectivity, and robustness. Limits of detection and quantitation were recorded as 5 and 40 ng/spot, respectively. The proposed method efficiently separated yohimbine hydrochloride from other components even in complex mixture containing powdered plants. The amount of yohimbine hydrochloride ranged from 2.3 to 5.2 mg/tablet or capsule in preparations containing the pure alkaloid, while it varied from zero (0) to 1.5-1.8 mg/capsule in dietary supplements containing powdered yohimbe bark. We concluded that this method employing high performance thin layer chromatography (HPTLC) in quantitative determination of yohimbine hydrochloride in pharmaceutical preparations is efficient, simple, accurate, and validated.

  18. 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.

  19. A Guide to Job Analysis for the Preparation of Job Training Programmes.

    ERIC Educational Resources Information Center

    Ceramics, Glass, and Mineral Products Industry Training Board, Harrow (England).

    The paper deals with job analysis for the preparation of job training programs. The analytical approach involves five steps: enlisting support, examining the job, describing the job, analyzing training requirements, and planning the programs. Appendixes include methods of producing training schemes--the simple job breakdown, straightforward…

  20. A Ricin Forensic Profiling Approach Based on a Complex Set of Biomarkers

    DOE PAGES

    Fredriksson, Sten-Ake; Wunschel, David S.; Lindstrom, Susanne Wiklund; ...

    2018-03-28

    A forensic method for the retrospective determination of preparation methods used for illicit ricin toxin production was developed. The method was based on a complex set of biomarkers, including carbohydrates, fatty acids, seed storage proteins, in combination with data on ricin and Ricinus communis agglutinin. The analyses were performed on samples prepared from four castor bean plant (R. communis) cultivars by four different sample preparation methods (PM1 – PM4) ranging from simple disintegration of the castor beans to multi-step preparation methods including different protein precipitation methods. Comprehensive analytical data was collected by use of a range of analytical methods andmore » robust orthogonal partial least squares-discriminant analysis- models (OPLS-DA) were constructed based on the calibration set. By the use of a decision tree and two OPLS-DA models, the sample preparation methods of test set samples were determined. The model statistics of the two models were good and a 100% rate of correct predictions of the test set was achieved.« less

  1. A Ricin Forensic Profiling Approach Based on a Complex Set of Biomarkers

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

    Fredriksson, Sten-Ake; Wunschel, David S.; Lindstrom, Susanne Wiklund

    A forensic method for the retrospective determination of preparation methods used for illicit ricin toxin production was developed. The method was based on a complex set of biomarkers, including carbohydrates, fatty acids, seed storage proteins, in combination with data on ricin and Ricinus communis agglutinin. The analyses were performed on samples prepared from four castor bean plant (R. communis) cultivars by four different sample preparation methods (PM1 – PM4) ranging from simple disintegration of the castor beans to multi-step preparation methods including different protein precipitation methods. Comprehensive analytical data was collected by use of a range of analytical methods andmore » robust orthogonal partial least squares-discriminant analysis- models (OPLS-DA) were constructed based on the calibration set. By the use of a decision tree and two OPLS-DA models, the sample preparation methods of test set samples were determined. The model statistics of the two models were good and a 100% rate of correct predictions of the test set was achieved.« less

  2. Simple room-temperature preparation of high-yield large-area graphene oxide

    PubMed Central

    Huang, NM; Lim, HN; Chia, CH; Yarmo, MA; Muhamad, MR

    2011-01-01

    Graphene has attracted much attention from researchers due to its interesting mechanical, electrochemical, and electronic properties. It has many potential applications such as polymer filler, sensor, energy conversion, and energy storage devices. Graphene-based nanocomposites are under an intense spotlight amongst researchers. A large amount of graphene is required for preparation of such samples. Lately, graphene-based materials have been the target for fundamental life science investigations. Despite graphene being a much sought-after raw material, the drawbacks in the preparation of graphene are that it is a challenge amongst researchers to produce this material in a scalable quantity and that there is a concern about its safety. Thus, a simple and efficient method for the preparation of graphene oxide (GO) is greatly desired to address these problems. In this work, one-pot chemical oxidation of graphite was carried out at room temperature for the preparation of large-area GO with ~100% conversion. This high-conversion preparation of large-area GO was achieved using a simplified Hummer’s method from large graphite flakes (an average flake size of 500 μm). It was found that a high degree of oxidation of graphite could be realized by stirring graphite in a mixture of acids and potassium permanganate, resulting in GO with large lateral dimension and area, which could reach up to 120 μm and ~8000 μm2, respectively. The simplified Hummer’s method provides a facile approach for the preparation of large-area GO. PMID:22267928

  3. Quantitation & Case-Study-Driven Inquiry to Enhance Yeast Fermentation Studies

    ERIC Educational Resources Information Center

    Grammer, Robert T.

    2012-01-01

    We propose a procedure for the assay of fermentation in yeast in microcentrifuge tubes that is simple and rapid, permitting assay replicates, descriptive statistics, and the preparation of line graphs that indicate reproducibility. Using regression and simple derivatives to determine initial velocities, we suggest methods to compare the effects of…

  4. Graphene oxide caged in cellulose microbeads for removal of malachite green dye from aqueous solution.

    PubMed

    Zhang, Xiaomei; Yu, Hongwen; Yang, Hongjun; Wan, Yuchun; Hu, Hong; Zhai, Zhuang; Qin, Jieming

    2015-01-01

    A simple sol-gel method using non-toxic and cost-effective precursors has been developed to prepare graphene oxide (GO)/cellulose bead (GOCB) composites for removal of dye pollutants. Taking advantage of the combined benefits of GO and cellulose, the prepared GOCB composites exhibit excellent removal efficiency towards malachite green (>96%) and can be reused for over 5 times through simple filtration method. The high-decontamination performance of the GOCB system is strongly dependent on encapsulation amount of GO, temperature and pH value. In addition, the adsorption behavior of this new adsorbent fits well with the Langmuir isotherm and pseudo-second-order kinetic model. Copyright © 2014 Elsevier Inc. All rights reserved.

  5. Microwave Synthesis of BCNO/SiO2 Nanocomposite Material

    NASA Astrophysics Data System (ADS)

    Faryuni, I. D.; Ramdhani, F.; Sampurno, J.; Nuryadin, B. W.; Noor, F. A.; Iskandar, F.

    2017-07-01

    In the present work, we report the preparation of BCNO/SiO2 phosphor synthesized using a microwave-assisted method. This method allows a lower temperature and a shorter reaction time than simple heating (furnace). The phosphors were prepared from precursors containing, boric acid, urea, citric acid and SiO2 nanoparticles. To These precursors, silica nanoparticles were added at various concentrations from 0 to 5 %wt. The emission wavelength produced by the phosphor was varied by varying the fraction mass of the silica that were added to the precursors. The results showed that higher photoluminescence (PL) intensity was produced by the BCNO/SiO2 with 3 %wt silica addition. The novelty of this research is using microwave heating for BCNO/SiO2 synthesis, which is usually conducted using a simple heating method.

  6. Application of a Permethrin Immunosorbent Assay Method to Residential Soil and Dust Samples

    EPA Science Inventory

    A low-cost, high throughput bioanalytical screening method was developed for monitoring cis/trans-permethrin in dust and soil samples. The method consisted of a simple sample preparation procedure [sonication with dichloromethane followed by a solvent exchange into methanol:wate...

  7. Preparation of colloidal gold for staining proteins electrotransferred onto nitrocellulose membranes.

    PubMed

    Yamaguchi, K; Asakawa, H

    1988-07-01

    This paper describes a simple method of preparing colloidal gold for staining protein blots. Colloidal gold was prepared from 0.005 or 0.01% HAuCl4 by the addition of formalin as a reductant and potassium hydroxide. Staining of small cell carcinoma tissue extract blotted onto nitrocellulose membranes with this colloidal gold solution resulted in the appearance of a large number of clear wine-red bands. The sensitivity of gold staining was 60 times higher than that of Coomassie brilliant blue staining and almost comparable to that of silver staining of proteins in polyacrylamide gel. The sensitivity of this method was also satisfactory in comparison with that of enzyme immunoblotting. The colloidal gold prepared by this method is usable for routine work.

  8. Preparation of Electrically Conductive Polystyrene/Carbon Nanofiber Nanocomposite Films

    ERIC Educational Resources Information Center

    Sun, Luyi; O'Reilly, Jonathan Y.; Tien, Chi-Wei; Sue, Hung-Jue

    2008-01-01

    A simple and effective approach to prepare conductive polystyrene/carbon nanofiber (PS/CNF) nanocomposite films via a solution dispersion method is presented. Inexpensive CNF, which has a structure similar to multi-walled carbon nanotubes, is chosen as a nanofiller in this experiment to achieve conductivity in PS films. A good dispersion is…

  9. Preparation of ZnO nanoparticles showing upconversion luminescence through simple chemical method

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

    Anjana, R.; Subha, P. P.; Markose, Kurias K.

    2016-05-23

    Upconversion luminescence is an interesting area while considering its applications in a vast variety of fields. Rare earth ions like erbium is the most studied and efficient candidate for achieving upconversion. Erbium and ytterbium co-doped ZnO nanoparticles were prepared through co-precipitation method. A strong red emission has been obtained while exciting with 980 nm laser. Dependence of luminescence emission colour on ytterbium concentration has been studied.

  10. Self-assembly and hierarchical patterning of aligned organic nanowire arrays by solvent evaporation on substrates with patterned wettability.

    PubMed

    Bao, Rong-Rong; Zhang, Cheng-Yi; Zhang, Xiu-Juan; Ou, Xue-Mei; Lee, Chun-Sing; Jie, Jian-Sheng; Zhang, Xiao-Hong

    2013-06-26

    The controlled growth and alignment of one-dimensional organic nanostructures at well-defined locations considerably hinders the integration of nanostructures for electronic and optoelectronic applications. Here, we demonstrate a simple process to achieve the growth, alignment, and hierarchical patterning of organic nanowires on substrates with controlled patterns of surface wettability. The first-level pattern is confined by the substrate patterns of wettability. Organic nanostructures are preferentially grown on solvent wettable regions. The second-level pattern is the patterning of aligned organic nanowires deposited by controlling the shape and movement of the solution contact lines during evaporation on the wettable regions. This process is controlled by the cover-hat-controlled method or vertical evaportation method. Therefore, various new patterns of organic nanostructures can be obtained by combing these two levels of patterns. This simple method proves to be a general approach that can be applied to other organic nanostructure systems. Using the as-prepared patterned nanowire arrays, an optoelectronic device (photodetector) is easily fabricated. Hence, the proposed simple, large-scale, low-cost method of preparing patterns of highly ordered organic nanostructures has high potential applications in various electronic and optoelectronic devices.

  11. Simple method for preparation of nanostructurally organized spines of sand dollar Scaphechinus mirabilis (Agassiz, 1863).

    PubMed

    Ehrlich, Herman; Elkin, Yury N; Artoukov, Alexandr A; Stonik, Valentin A; Safronov, Peter P; Bazhenov, Vasily V; Kurek, Denis V; Varlamov, Valery P; Born, René; Meissner, Heike; Richter, Gert

    2011-06-01

    Unique skeletal formations of marine invertebrates, including representatives of Echinodermata, have the unique potential to serve as templates for bio-inspired materials chemistry, biomimetics, and materials science. The sand dollar Scaphechinus mirabilis (Agassiz, 1983) is widely distributed in the northwest of the Pacific Ocean from southern Japan to the Aleutian Islands. This animal is the main source of naphtochinone-based substances. These compounds have recently drawn medical attention for their use as cardiological and ophthalmological drugs. Unfortunately, after extraction of the naphtochinones, the residual skeletons and spines of the sand dollars were usually discarded. Here, we report the first method for the preparation of nanostructurally organized spines of S. mirabilis, using a simple enzymatic and hydrogen peroxide-based treatment. Application of this method opens the way for development of non-wasteful environmentally clean technology of sand dollars as well-known industrial marine invertebrates.

  12. A ricin forensic profiling approach based on a complex set of biomarkers.

    PubMed

    Fredriksson, Sten-Åke; Wunschel, David S; Lindström, Susanne Wiklund; Nilsson, Calle; Wahl, Karen; Åstot, Crister

    2018-08-15

    A forensic method for the retrospective determination of preparation methods used for illicit ricin toxin production was developed. The method was based on a complex set of biomarkers, including carbohydrates, fatty acids, seed storage proteins, in combination with data on ricin and Ricinus communis agglutinin. The analyses were performed on samples prepared from four castor bean plant (R. communis) cultivars by four different sample preparation methods (PM1-PM4) ranging from simple disintegration of the castor beans to multi-step preparation methods including different protein precipitation methods. Comprehensive analytical data was collected by use of a range of analytical methods and robust orthogonal partial least squares-discriminant analysis- models (OPLS-DA) were constructed based on the calibration set. By the use of a decision tree and two OPLS-DA models, the sample preparation methods of test set samples were determined. The model statistics of the two models were good and a 100% rate of correct predictions of the test set was achieved. Copyright © 2018 Elsevier B.V. All rights reserved.

  13. A Facile Preparation of Imidazolinium Chlorides

    PubMed Central

    Kuhn, Kevin M.; Grubbs, Robert H.

    2009-01-01

    A process for the preparation of symmetric and unsymmetric imidazolinium chlorides that involves reaction of a formamidine with dichloroethane and a base (a) is described. This method makes it possible to obtain numerous imidazolinium chlorides under solvent-free reaction conditions and in excellent yields with purification by simple filtration. Alternatively, symmetric imidazolinium chlorides can be prepared directly in moderate yields from substituted anilines by utilizing half of the formamidine intermediate as sacrificial base (b). PMID:18412354

  14. Fabrication of metal/semiconductor nanocomposites by selective laser nano-welding.

    PubMed

    Yu, Huiwu; Li, Xiangyou; Hao, Zhongqi; Xiong, Wei; Guo, Lianbo; Lu, Yongfeng; Yi, Rongxing; Li, Jiaming; Yang, Xinyan; Zeng, Xiaoyan

    2017-06-01

    A green and simple method to prepare metal/semiconductor nanocomposites by selective laser nano-welding metal and semiconductor nanoparticles was presented, in which the sizes, phases, and morphologies of the components can be maintained. Many types of nanocomposites (such as Ag/TiO 2 , Ag/SnO 2 , Ag/ZnO 2 , Pt/TiO 2 , Pt/SnO 2 , and Pt/ZnO) can be prepared by this method and their corresponding performances were enhanced.

  15. A simple and fast method for fixation of cultured cell lines that preserves cellular structures containing gamma-tubulin.

    PubMed

    Alvarado-Kristensson, Maria

    2018-01-01

    When using fluorescence microscope techniques to study cells, it is essential that the cell structure and contents are preserved after preparation of the samples, and that the preparation method employed does not create artefacts that can be perceived as cellular structure/components. γ-Tubulin forms filaments that in some cases are immunostained with an anti-γ-tubulin antibody, but this immunostaining is not reproducible [[1], [2

  16. Using Simple Educational Methods To Motivate Consumers To Prepare for Emergencies.

    ERIC Educational Resources Information Center

    Bowen, Cathy Faulcon; Faison, Nakesha

    2002-01-01

    Of 357 Pennsylvania residents who received booklets on Y2K preparedness, 187 attended workshops. Nearly 50% read all or most of the booklets; over 50% reported preparing for an emergency because of the booklet or workshop. Older and more educated consumers were more likely to take action. Short, visually appealing materials increased likelihood of…

  17. Evaluation of a Fast and Simple Sample Preparation Method for Polybrominated Diphenyl Ether (PBDE) Flame Retardants and Dichlorodiphenyltrichloroethane (DDT) Pesticides in Fish for Analysis by ELISA Compared with GC-MS/MS.

    PubMed

    Sapozhnikova, Yelena; Simons, Tawana; Lehotay, Steven J

    2015-05-13

    A simple, fast, and cost-effective sample preparation method, previously developed and validated for the analysis of organic contaminants in fish using low-pressure gas chromatography-tandem mass spectrometry (LPGC-MS/MS), was evaluated for the analysis of polybrominated diphenyl ethers (PBDEs) and dichlorodiphenyltrichloroethane (DDT) pesticides using enzyme-linked immunosorbent assay (ELISA). The sample preparation technique was based on the quick, easy, cheap, rugged, effective, and safe (QuEChERS) approach with filter-vial dispersive solid phase extraction (d-SPE). Incurred PBDEs and DDTs were analyzed in three types of fish with 3-10% lipid content: Pacific croaker, salmon, and National Institute of Standards and Technology (NIST) Standard Reference Material 1947 (Lake Michigan fish tissue). LPGC-MS/MS and ELISA results were in agreement: 108-111 and 65-82% accuracy ELISA versus LPGC-MS/MS results for PBDEs and DDTs, respectively. Similar detection limits were achieved for ELISA and LPGC-MS/MS. Matrix effects (MEs) were significant (e.g., -60%) for PBDE measurement in ELISA, but not a factor in the case of DDT pesticides. This study demonstrated that the sample preparation method can be adopted for semiquantitative screening analysis of fish samples by commercial kits for PBDEs and DDTs.

  18. 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.

  19. A simple one-step method to prepare fluorescent carbon dots and their potential application in non-invasive glioma imaging

    NASA Astrophysics Data System (ADS)

    Ruan, Shaobo; Qian, Jun; Shen, Shun; Zhu, Jianhua; Jiang, Xinguo; He, Qin; Gao, Huile

    2014-08-01

    Fluorescent carbon dots (CD) possess impressive potential in bioimaging because of their low photobleaching, absence of optical blinking and good biocompatibility. However, their relatively short excitation/emission wavelengths restrict their application in in vivo imaging. In the present study, a kind of CD was prepared by a simple heat treatment method using glycine as the only precursor. The diameter of CD was lower than 5 nm, and the highest emission wavelength was 500 nm. However, at 600 nm, there was still a relatively strong fluorescent emission, suggesting CD could be used for in vivo imaging. Additionally, several experiments demonstrated that CD possessed good serum stability and low cytotoxicity. In vitro, CD could be taken up into C6 glioma cells in a time- and concentration-dependent manner, with both endosomes and mitochondria involved. In vivo, CD could be used for non-invasive glioma imaging because of its high accumulation in the glioma site of the brain, which was demonstrated by both in vivo imaging and ex vivo tissue imaging. Furthermore, the fluorescent distribution in tissue slices also showed CD distributed in glioma with high intensity, while with a low intensity in normal brain tissue. In conclusion, CD were prepared using a simple method with relatively long excitation and emission wavelengths and could be used for non-invasive glioma imaging.Fluorescent carbon dots (CD) possess impressive potential in bioimaging because of their low photobleaching, absence of optical blinking and good biocompatibility. However, their relatively short excitation/emission wavelengths restrict their application in in vivo imaging. In the present study, a kind of CD was prepared by a simple heat treatment method using glycine as the only precursor. The diameter of CD was lower than 5 nm, and the highest emission wavelength was 500 nm. However, at 600 nm, there was still a relatively strong fluorescent emission, suggesting CD could be used for in vivo imaging. Additionally, several experiments demonstrated that CD possessed good serum stability and low cytotoxicity. In vitro, CD could be taken up into C6 glioma cells in a time- and concentration-dependent manner, with both endosomes and mitochondria involved. In vivo, CD could be used for non-invasive glioma imaging because of its high accumulation in the glioma site of the brain, which was demonstrated by both in vivo imaging and ex vivo tissue imaging. Furthermore, the fluorescent distribution in tissue slices also showed CD distributed in glioma with high intensity, while with a low intensity in normal brain tissue. In conclusion, CD were prepared using a simple method with relatively long excitation and emission wavelengths and could be used for non-invasive glioma imaging. Electronic supplementary information (ESI) available. See DOI: 10.1039/c4nr02657h

  20. Experimental preparation and characterization of four-dimensional quantum states using polarization and time-bin modes of a single photon

    NASA Astrophysics Data System (ADS)

    Yoo, Jinwon; Choi, Yujun; Cho, Young-Wook; Han, Sang-Wook; Lee, Sang-Yun; Moon, Sung; Oh, Kyunghwan; Kim, Yong-Su

    2018-07-01

    We present a detailed method to prepare and characterize four-dimensional pure quantum states or ququarts using polarization and time-bin modes of a single-photon. In particular, we provide a simple method to generate an arbitrary pure ququart and fully characterize the state with quantum state tomography. We also verify the reliability of the recipe by showing experimental preparation and characterization of 20 ququart states in mutually unbiased bases. As qudits provide superior properties over qubits in many fundamental tests of quantum physics and applications in quantum information processing, the presented method will be useful for photonic quantum information science.

  1. Method for the preparation of radon-211

    DOEpatents

    Meyer, Geerd-J.; Lambrecht, Richard M.

    1982-01-01

    A method for the production of .sup.211 Rn comprising bombarding .sup.209 Bi with .sup.7 Li particles utilizing the nuclear reaction .sup.209 Bi(.sup.7 Li,5n).sup.211 Rn. The method provides a simple spectrum from which .sup.211 Rn can be easily isolated in a highly pure condition.

  2. A green method of graphene preparation in an alkaline environment.

    PubMed

    Štengl, Václav; Henych, Jiří; Bludská, Jana; Ecorchard, Petra; Kormunda, Martin

    2015-05-01

    We present a new, simple, quick and ecologically friendly method of exfoliating graphite to produce graphene. The method is based on the intercalation of a permanganate M2MnO4 (M=K, Na, Li), which is formed by the reaction of a manganate MMnO4 with an alkali metal hydroxide MOH. The quality of exfoliation and the morphology were determined using X-ray photoelectron spectroscopy, X-ray diffraction and microscopic techniques, including transmission electron microscopy and atomic force microscopy. We observed that a stable graphene suspension could be prepared under strongly alkaline conditions in the presence of permanganate and ultrasound assistance. The use of only an alkaline environment for the direct preparation of graphene from graphite structures has not been previously described or applied. It was found that such a method of preparation leads to surprisingly high yields and a stable product for hydrophilic graphene applications. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. [Exploration of one-step preparation of Ganoderma lucidum multicomponent microemulsion].

    PubMed

    He, Jun-Jie; Chen, Yan; Du, Meng; Cao, Wei; Yuan, Ling; Zheng, Li-Yan

    2013-03-01

    To explore one-step method for the preparation of Ganoderma lucidum multicomponent microemulsion, according to the dissolution characteristics of triterpenes and polysaccharides in Ganoderma lucidum, formulation of the microemulsion was optimized. The optimal blank microemulsion was used as a solvent to sonicate the Ganoderma lucidum powder to prepare the multicomponent microemulsion, besides, its physicochemical properties were compared with the microemulsion made by conventional method. The results showed that the multicomponent microemulsion was characterized as (43.32 +/- 6.82) nm in size, 0.173 +/- 0.025 in polydispersity index (PDI) and -(3.98 +/- 0.82) mV in zeta potential. The contents of Ganoderma lucidum triterpenes and polysaccharides were (5.95 +/- 0.32) and (7.58 +/- 0.44) mg x mL(-1), respectively. Sonicating Ganoderma lucidum powder by blank microemulsion could prepare the multicomponent microemulsion. Compared with the conventional method, this method is simple and low cost, which is suitable for industrial production.

  4. Facile synthesis of hierarchical dendritic PtPd nanogarlands supported on reduced graphene oxide with enhanced electrocatalytic properties

    NASA Astrophysics Data System (ADS)

    Li, Shan-Shan; Zheng, Jie-Ning; Ma, Xiaohong; Hu, Yuan-Yuan; Wang, Ai-Jun; Chen, Jian-Rong; Feng, Jiu-Ju

    2014-05-01

    A simple and facile method is developed for one-pot preparation of hierarchical dendritic PtPd nanogarlands supported on reduced graphene oxide (PtPd/RGO) at room temperature, without using any seed, organic solvent, or complex apparatus. It is found that octylphenoxypolyethoxyethanol (NP-40) as a soft template and its amount are critical to the formation of PtPd garlands. The as-prepared nanocomposites are further applied to methanol and ethanol oxidation with significantly enhanced electrocatalytic activity and better stability in alkaline media.A simple and facile method is developed for one-pot preparation of hierarchical dendritic PtPd nanogarlands supported on reduced graphene oxide (PtPd/RGO) at room temperature, without using any seed, organic solvent, or complex apparatus. It is found that octylphenoxypolyethoxyethanol (NP-40) as a soft template and its amount are critical to the formation of PtPd garlands. The as-prepared nanocomposites are further applied to methanol and ethanol oxidation with significantly enhanced electrocatalytic activity and better stability in alkaline media. Electronic supplementary information (ESI) available: Experimental section, Fig. S1-S12 and Tables S1 and S2. See DOI: 10.1039/c3nr06808k

  5. A Simple and Rapid Method for Preparing a Cell-Free Bacterial Lysate for Protein Synthesis

    PubMed Central

    Kaduri, Maya; Shainsky-Roitman, Janna; Goldfeder, Mor; Ivanir, Eran; Benhar, Itai; Shoham, Yuval; Schroeder, Avi

    2016-01-01

    Cell-free protein synthesis (CFPS) systems are important laboratory tools that are used for various synthetic biology applications. Here, we present a simple and inexpensive laboratory-scale method for preparing a CFPS system from E. coli. The procedure uses basic lab equipment, a minimal set of reagents, and requires less than one hour to process the bacterial cell mass into a functional S30-T7 extract. BL21(DE3) and MRE600 E. coli strains were used to prepare the S30-T7 extract. The CFPS system was used to produce a set of fluorescent and therapeutic proteins of different molecular weights (up to 66 kDa). This system was able to produce 40–150 μg-protein/ml, with variations depending on the plasmid type, expressed protein and E. coli strain. Interestingly, the BL21-based CFPS exhibited stability and increased activity at 40 and 45°C. To the best of our knowledge, this is the most rapid and affordable lab-scale protocol for preparing a cell-free protein synthesis system, with high thermal stability and efficacy in producing therapeutic proteins. PMID:27768741

  6. The content of Ca, Cu, Fe, Mg and Mn and antioxidant activity of green coffee brews.

    PubMed

    Stelmach, Ewelina; Pohl, Pawel; Szymczycha-Madeja, Anna

    2015-09-01

    A simple and fast method of the analysis of green coffee infusions was developed to measure total concentrations of Ca, Cu, Fe, Mg and Mn by high resolution-continuum source flame atomic absorption spectrometry. The precision of the method was within 1-8%, while the accuracy was within -1% to 2%. The method was used to the analysis of infusions of twelve green coffees of different geographical origin. It was found that Ca and Mg were leached the easiest, i.e., on average 75% and 70%, respectively. As compared to the mug coffee preparation, the rate of the extraction of elements was increased when infusions were prepared using dripper or Turkish coffee preparation methods. Additionally, it was established that the antioxidant activity of green coffee infusions prepared using the mug coffee preparation was high, 75% on average, and positively correlated with the total content of phenolic compounds and the concentration of Ca in the brew. Copyright © 2015 Elsevier Ltd. All rights reserved.

  7. 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.

  8. High-throughput method for macrolides and lincosamides antibiotics residues analysis in milk and muscle using a simple liquid-liquid extraction technique and liquid chromatography-electrospray-tandem mass spectrometry analysis (LC-MS/MS).

    PubMed

    Jank, Louise; Martins, Magda Targa; Arsand, Juliana Bazzan; Campos Motta, Tanara Magalhães; Hoff, Rodrigo Barcellos; Barreto, Fabiano; Pizzolato, Tânia Mara

    2015-11-01

    A fast and simple method for residue analysis of the antibiotics classes of macrolides (erythromycin, azithromycin, tylosin, tilmicosin and spiramycin) and lincosamides (lincomycin and clindamycin) was developed and validated for cattle, swine and chicken muscle and for bovine milk. Sample preparation consists in a liquid-liquid extraction (LLE) with acetonitrile, followed by liquid chromatography-electrospray-tandem mass spectrometry analysis (LC-ESI-MS/MS), without the need of any additional clean-up steps. Chromatographic separation was achieved using a C18 column and a mobile phase composed by acidified acetonitrile and water. The method was fully validated according the criteria of the Commission Decision 2002/657/EC. Validation parameters such as limit of detection, limit of quantification, linearity, accuracy, repeatability, specificity, reproducibility, decision limit (CCα) and detection capability (CCβ) were evaluated. All calculated values met the established criteria. Reproducibility values, expressed as coefficient of variation, were all lower than 19.1%. Recoveries range from 60% to 107%. Limits of detection were from 5 to 25 µg kg(-1).The present method is able to be applied in routine analysis, with adequate time of analysis, low cost and a simple sample preparation protocol. Copyright © 2015. Published by Elsevier B.V.

  9. Construction of super - hydrophobic copper alloy surface by one - step mixed solution immersion method

    NASA Astrophysics Data System (ADS)

    Gu, Qiang; Chen, Ying; Chen, Dong; Zhang, Zeting

    2018-01-01

    This paper presents a method for preparing a super hydrophobic surface with a fast, simple, low-cost, one-step reaction by immersing copper alloy in an ethanol solution containing silver nitrate and myristic acid. The effects of reaction time, reaction temperature, reactant concentration and reaction time on the wettability of the material were studied. The surface wettability, appearance, chemical composition, durability and chemical stability of the prepared samples was measured by water contact angle (CA), scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The results show that when the reaction time is only 10min, the surface WCA of the prepared material can reach 154.9. This study provides an effective method for the rapid preparation of stable super hydrophobic surfaces.

  10. Infrared light-assisted preparation of Ag nanoparticles-reduced graphene oxide nanocomposites for non-enzymatic H{sub 2}O{sub 2} sensing

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

    Ji, Ye; State Key Laboratory of Transducer Technology, Chinese Academy of Sciences; Zhang, Yong

    2015-12-15

    Graphical abstract: An infrared light irradiation method has been developed for preparation of AgNPs/rGO nanocomposites for electrochemical detection of H{sub 2}O{sub 2}. - Highlights: • AgNPs/rGO nanocomposites have been prepared by photochemical method. • AgNPs/rGO nanocomposites exhibit good sensing performances for detection of H{sub 2}O{sub 2}. • The present work provides a simple and green method for preparation of rGO-based materials. - Abstract: A green method has been developed for preparation of Ag nanoparticles/reduced graphene oxide (AgNPs/rGO) nanocomposites by infrared light irradiation. The characterizations indicate the successful preparation of AgNPs/rGO nanocomposites. Most importantly, AgNPs/rGO nanocomposites exhibit excellent electrocatalytic activity formore » reduction of H{sub 2}O{sub 2}, leading to a high-performance non-enzymatic H{sub 2}O{sub 2} sensor with linear detection range and detection limit about 0.1 mM to 140 mM (r = 0.9896) and 3.0 μM, respectively.« less

  11. A novel method to prepare concentrated conidial biomass formulation of Trichoderma harzianum for seed application.

    PubMed

    Singh, P C; Nautiyal, C S

    2012-12-01

    To prepare concentrated formulation of Trichoderma harzianum MTCC-3841 (NBRI-1055) with high colony forming units (CFU), long shelf life and efficient in root colonization by a simple scrapping method. NBRI-1055 spores scrapped from potato dextrose agar plates were used to prepare a concentrated formulation after optimizing carrier material, moisture content and spore harvest time. The process provides an advantage of maintaining optimum moisture level by the addition of water rather than dehydration. The formulation had an initial 11-12 log(10) CFU g(-1). Its concentrated form reduces its application amount by 100 times (10 g 100 kg(-1) seed) and provides 3-4 log(10) CFU seed(-1). Shelf life of the product was experimentally determined at 30 and 40 °C and predicted at other temperatures following Arrhenius equation. The concentrated formulation as compared to similar products provides an extra advantage of smaller packaging for storage and transportation, cutting down product cost. Seed application of the formulation recorded significant increase in plant growth promotion. Stable and effective formulation of Trichoderma harzianum NBRI-1055 was obtained by a simple scrapping method. A new method for the production of concentrated, stable, effective and cost efficient formulation of T. harzianum has been validated for seed application. © 2012 The Society for Applied Microbiology.

  12. Spectrophotometric Method for the Determination of Two Coformulated Drugs with Highly Different Concentrations. Application on Vildagliptin and Metformin Hydrochloride

    NASA Astrophysics Data System (ADS)

    Zaazaa, H. E.; Elzanfaly, E. S.; Soudi, A. T.; Salem, M. Y.

    2016-03-01

    A new smart simple validated spectrophotometric method was developed for the determination of two drugs one of which is in a very low concentration compared to the other. The method is based on spiking and dilution then simple mathematical manipulation of the absorbance spectra. This method was applied for the determination of a binary mixture of vildagliptin and metformin hydrochloride in the ratio 50:850 in laboratory prepared mixtures containing both drugs in this ratio and in pharmaceutical dosage form with good recoveries. The developed method was validated according to ICH guidelines and can be used for routine quality control testing.

  13. Method of preparing pure fluorine gas

    DOEpatents

    Asprey, Larned B.

    1976-01-01

    A simple, inexpensive system for purifying and storing pure fluorine is described. The method utilizes alkali metal-nickel fluorides to absorb tank fluorine by forming nickel complex salts and leaving the gaseous impurities which are pumped away. The complex nickel fluoride is then heated to evolve back pure gaseous fluorine.

  14. Simple preparation of magnetic field-responsive structural colored Janus particles.

    PubMed

    Teshima, Midori; Seki, Takahiro; Takeoka, Yukikazu

    2018-03-08

    We established a simple method for preparing Janus particles displaying different structural colors using submicron-sized fine silica particles and magnetic nanoparticles composed of Fe 3 O 4 . A w/o emulsion is prepared by vortex-stirring a mixed aqueous solution of suspended fine silica particles and magnetic nanoparticles and of hexadecane containing an emulsifier. Subsequent drying of the emulsion on a hot plate using a magnetic stirrer provides a polydisperse particle aggregate displaying two different structural colors according to the ratio of the amount of fine silica particles to the amount of magnetic nanoparticles. This polydisperse particle aggregate can be converted into monodisperse particles simply by using a sieve made of stainless steel. In the presence of a magnet, the monodisperse Janus particles can change their orientation and can switch between two different structural colors.

  15. A simple, rapid and inexpensive method for localization of Tomato yellow leaf curl virus and Potato leafroll virus in plant and insect vectors.

    PubMed

    Ghanim, Murad; Brumin, Marina; Popovski, Smadar

    2009-08-01

    A simple, rapid, inexpensive method for the localization of virus transcripts in plant and insect vector tissues is reported here. The method based on fluorescent in situ hybridization using short DNA oligonucleotides complementary to an RNA segment representing a virus transcript in the infected plant or insect vector. The DNA probe harbors a fluorescent molecule at its 5' or 3' ends. The protocol: simple fixation, hybridization, minimal washing and confocal microscopy, provides a highly specific signal. The reliability of the protocol was tested by localizing two phloem-limited plant virus transcripts in infected plants and insect tissues: Tomato yellow leaf curl virus (TYLCV) (Begomovirus: Geminiviridae), exclusively transmitted by the whitefly Bemisia tabaci (Gennadius) in a circulative non-propagative manner, and Potato leafroll virus (Polerovirus: Luteoviridae), similarly transmitted by the aphid Myzus persicae (Sulzer). Transcripts for both viruses were localized specifically to the phloem sieve elements of infected plants, while negative controls showed no signal. TYLCV transcripts were also localized to the digestive tract of B. tabaci, confirming TYLCV route of transmission. Compared to previous methods for localizing virus transcripts in plant and insect tissues that include complex steps for in-vitro probe preparation or antibody raising, tissue fixation, block preparation, sectioning and hybridization, the method described below provides very reliable, convincing, background-free results with much less time, effort and cost.

  16. The formation of stable pH gradients with weak monovalent buffers for isoelectric focusing in free solution

    NASA Technical Reports Server (NTRS)

    Mosher, Richard A.; Thormann, Wolfgang; Graham, Aly; Bier, Milan

    1985-01-01

    Two methods which utilize simple buffers for the generation of stable pH gradients (useful for preparative isoelectric focusing) are compared and contrasted. The first employs preformed gradients comprised of two simple buffers in density-stabilized free solution. The second method utilizes neutral membranes to isolate electrolyte reservoirs of constant composition from the separation column. It is shown by computer simulation that steady-state gradients can be formed at any pH range with any number of components in such a system.

  17. A simple validated multi-analyte method for detecting drugs in oral fluid by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).

    PubMed

    Zheng, Yufang; Sparve, Erik; Bergström, Mats

    2018-06-01

    A UPLC-MS/MS method was developed to identify and quantitate 37 commonly abused drugs in oral fluid. Drugs of interest included amphetamines, benzodiazepines, cocaine, opiates, opioids, phencyclidine and tetrahydrocannabinol. Sample preparation and extraction are simple, and analysis times short. Validation showed satisfactory performance at relevant concentrations. The possibility of contaminated samples as well as the interpretation in relation to well-knows matrices, such as urine, will demand further study. Copyright © 2017 John Wiley & Sons, Ltd.

  18. Preparation of SmBCO layer for the surface optimization of GdYBCO film by MOCVD process based on a simple self-heating technology

    NASA Astrophysics Data System (ADS)

    Zhao, Ruipeng; Zhang, Fei; Liu, Qing; Xia, Yudong; Lu, Yuming; Cai, Chuanbing; Tao, Bowan; Li, Yanrong

    2018-07-01

    The MOCVD process was adopted to grow the REBa2Cu3O7-δ ((REBCO), RE = rare earth elements) films on the LaMnO3 (LMO) templates. Meanwhile, the LMO-template tapes are heated by the joule effect after applying a heating current through the Hastelloy metal substrates. The surface of GdYBCO films prepared by MOCVD method is prone to form outgrowths. So the surface morphology of GdYBCO film is optimized by depositing the SmBCO layer, which is an important process method for the preparation of high-quality multilayer REBCO films. At last, the GdYBCO/SmBCO/GdYBCO multilayer films were successfully prepared on the LMO templates based on the simple self-heating method. It is demonstrated that the GdYBCO surface was well improved by the characterization analysis of scanning electron microscope. And the Δω of REBCO (005) and Δφ of REBCO (103), which were performed by an X-ray diffraction system, are respectively 1.3° and 3.3° What's more, the critical current density (Jc) has been more than 3 MA/cm2 (77 K, 0 T) and the critical current (Ic) basically shows a trend of good linear increase with the increase of the number of REBCO layers.

  19. Modified release matrix prepared by compaction of spheres containing waxy material.

    PubMed

    Bado, L; Ghaly, E S

    1995-09-01

    In this study, chlorpheniramine maleate spheres were prepared by the extruder/marumerizer. A new waxy material, Gelucire 50/02 at three levels (10%, 30% and 50%) was added and Avicel PH-101 was used as spheronizing material. The drug was incorporated into the waxy material by two methods. The first was the direct method, in which the drug (10%), wax and Avicel PH-101 were mixed together. The second was the fusion method, in which the drug was dispersed in the melted wax and the solidified mass was milled and mixed with Avicel PH-101. The data obtained indicated that simple addition of waxy material into chlorpheniramine maleate-Avicel PH-101 spheres interrupted matrix formation and increased drug release. Also in this study, a multiparticulate delivery system was prepared successfully by compaction of spheres into tablets. Tablets compacted from spheres prepared by fusion method gave less drug release than those compacted from spheres of the same composition but prepared with direct method. As the level of wax was increased in tablet formulation, drug release was decreased.

  20. Pyocin-sensitivity testing as a method of typing Pseudomonas aeruginosa: use of "phage-free" preparations of pyocin.

    PubMed

    Rampling, A; Whitby, J L; Wildy, P

    1975-11-01

    A method for pyocin-sensitivity typing by means of "phage-free" preparations of pyocin is described. The method was tested on 227 isolates of P. aeruginosa, collected from 34 different foci of infection in hospitals in the British Isles and the results were compared with those for combined serological and phage typing of all strains and pyocin production of 105 of the isolates. It is concluded that pyocin-sensitivity typing is a simple and reliable method giving a high degree of discrimination, comparable to that of combined serological and phage typing, and it is suitable for use in routine hospital laboratories.

  1. Evaluation of the Illumigene Malaria LAMP: A Robust Molecular Diagnostic Tool for Malaria Parasites

    PubMed Central

    Lucchi, Naomi W.; Gaye, Marie; Diallo, Mammadou Alpha; Goldman, Ira F.; Ljolje, Dragan; Deme, Awa Bineta; Badiane, Aida; Ndiaye, Yaye Die; Barnwell, John W.; Udhayakumar, Venkatachalam; Ndiaye, Daouda

    2016-01-01

    Isothermal nucleic acid amplification assays such as the loop mediated isothermal amplification (LAMP), are well suited for field use as they do not require thermal cyclers to amplify the DNA. To further facilitate the use of LAMP assays in remote settings, simpler sample preparation methods and lyophilized reagents are required. The performance of a commercial malaria LAMP assay (Illumigene Malaria LAMP) was evaluated using two sample preparation workflows (simple filtration prep (SFP)) and gravity-driven filtration prep (GFP)) and pre-dispensed lyophilized reagents. Laboratory and clinical samples were tested in a field laboratory in Senegal and the results independently confirmed in a reference laboratory in the U.S.A. The Illumigene Malaria LAMP assay was easily implemented in the clinical laboratory and gave similar results to a real-time PCR reference test with limits of detection of ≤2.0 parasites/μl depending on the sample preparation method used. This assay reliably detected Plasmodium sp. parasites in a simple low-tech format, providing a much needed alternative to the more complex molecular tests for malaria diagnosis. PMID:27827432

  2. Simple preparation of plant epidermal tissue for laser microdissection and downstream quantitative proteome and carbohydrate analysis

    PubMed Central

    Falter, Christian; Ellinger, Dorothea; von Hülsen, Behrend; Heim, René; Voigt, Christian A.

    2015-01-01

    The outwardly directed cell wall and associated plasma membrane of epidermal cells represent the first layers of plant defense against intruding pathogens. Cell wall modifications and the formation of defense structures at sites of attempted pathogen penetration are decisive for plant defense. A precise isolation of these stress-induced structures would allow a specific analysis of regulatory mechanism and cell wall adaption. However, methods for large-scale epidermal tissue preparation from the model plant Arabidopsis thaliana, which would allow proteome and cell wall analysis of complete, laser-microdissected epidermal defense structures, have not been provided. We developed the adhesive tape – liquid cover glass technique (ACT) for simple leaf epidermis preparation from A. thaliana, which is also applicable on grass leaves. This method is compatible with subsequent staining techniques to visualize stress-related cell wall structures, which were precisely isolated from the epidermal tissue layer by laser microdissection (LM) coupled to laser pressure catapulting. We successfully demonstrated that these specific epidermal tissue samples could be used for quantitative downstream proteome and cell wall analysis. The development of the ACT for simple leaf epidermis preparation and the compatibility to LM and downstream quantitative analysis opens new possibilities in the precise examination of stress- and pathogen-related cell wall structures in epidermal cells. Because the developed tissue processing is also applicable on A. thaliana, well-established, model pathosystems that include the interaction with powdery mildews can be studied to determine principal regulatory mechanisms in plant–microbe interaction with their potential outreach into crop breeding. PMID:25870605

  3. Simple preparation of plant epidermal tissue for laser microdissection and downstream quantitative proteome and carbohydrate analysis.

    PubMed

    Falter, Christian; Ellinger, Dorothea; von Hülsen, Behrend; Heim, René; Voigt, Christian A

    2015-01-01

    The outwardly directed cell wall and associated plasma membrane of epidermal cells represent the first layers of plant defense against intruding pathogens. Cell wall modifications and the formation of defense structures at sites of attempted pathogen penetration are decisive for plant defense. A precise isolation of these stress-induced structures would allow a specific analysis of regulatory mechanism and cell wall adaption. However, methods for large-scale epidermal tissue preparation from the model plant Arabidopsis thaliana, which would allow proteome and cell wall analysis of complete, laser-microdissected epidermal defense structures, have not been provided. We developed the adhesive tape - liquid cover glass technique (ACT) for simple leaf epidermis preparation from A. thaliana, which is also applicable on grass leaves. This method is compatible with subsequent staining techniques to visualize stress-related cell wall structures, which were precisely isolated from the epidermal tissue layer by laser microdissection (LM) coupled to laser pressure catapulting. We successfully demonstrated that these specific epidermal tissue samples could be used for quantitative downstream proteome and cell wall analysis. The development of the ACT for simple leaf epidermis preparation and the compatibility to LM and downstream quantitative analysis opens new possibilities in the precise examination of stress- and pathogen-related cell wall structures in epidermal cells. Because the developed tissue processing is also applicable on A. thaliana, well-established, model pathosystems that include the interaction with powdery mildews can be studied to determine principal regulatory mechanisms in plant-microbe interaction with their potential outreach into crop breeding.

  4. Detection of Cucurbit chlorotic yellows virus from Bemisia tabaci captured on sticky traps using reverse transcription loop-mediated isothermal amplification (RT-LAMP) and simple template preparation.

    PubMed

    Okuda, Mitsuru; Okuda, Shiori; Iwai, Hisashi

    2015-09-01

    Cucurbit chlorotic yellows virus (CCYV) of the genus Crinivirus within the family Closteroviridae is an emerging infectious agent of cucurbits leading to severe disease and significant economic losses. Effective detection and identification methods for this virus are urgently required. In this study, a reverse transcription loop-mediated isothermal amplification (RT-LAMP) assay was developed to detect CCYV from its vector Bemisia tabaci. LAMP primer sets to detect CCYV were evaluated for their sensitivity and specificity, and a primer set designed from the HSP70h gene with corresponding loop primers were selected. The RT-LAMP assay was applied to detect CCYV from viruliferous B. tabaci trapped on sticky traps. A simple extraction procedure using RNAsecure™ was developed for template preparation. CCYV was detected in all of the B. tabaci 0, 1, 7 and 14 days after they were trapped. Although the rise of turbidity was delayed in reactions using RNA from B. tabaci trapped for 7 and 14 days compared with those from 0 and 1 day, the DNA amplification was sufficient to detect CCYV in all of the samples. These findings therefore present a simple template preparation method and an effective RT-LAMP assay, which can be easily and rapidly performed to monitor CCYV-viruliferous B. tabaci in the field. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Effect of bath temperature on surface morphology and photocatalytic activity of ZnO nanorods

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

    Sriharan, N.; Senthil, T. S., E-mail: tssenthi@gmail.com; Muthukumarasamy, N.

    2016-05-06

    ZnO nanorods were prepared by using simple hydrothermal method using four different bath temperatures. All the prepared ZnO nanorods are annealed at 450°C and are characterized by using various techniques such as X-ray diffraction, UV spectra and scanning electron microscopy. Photocatalytic activity of the prepared ZnO nanorods is analyzed. A novel photocatalytic reactor designed with ZnO nanorods prepared at 90°C shows enhanced catalytic efficiency. The role of light irradiation time, bath temperature and surface morphology of the ZnO nanorods on the performance of photocatalytic reaction is analyzed.

  6. A simple LC/MRM-MS-based method to quantify free linker-payload in antibody-drug conjugate preparations.

    PubMed

    Zmolek, Wesley; Bañas, Stefanie; Barfield, Robyn M; Rabuka, David; Drake, Penelope M

    2016-10-01

    Antibody-drug conjugates represent a growing class of biologic drugs that use the targeted specificity of an antibody to direct the localization of a small molecule drug, often a cytotoxic payload. After conjugation, antibody-drug conjugate preparations typically retain a residual amount of free (unconjugated) linker-payload. Monitoring this free small molecule drug component is important due to the potential for free payload to mediate unintended (off-target) toxicity. We developed a simple RP-HPLC/MRM-MS-based assay that can be rapidly employed to quantify free linker-payload. The method uses low sample volumes and offers an LLOQ of 10nM with 370pg on column. This analytical approach was used to monitor free linker-payload removal during optimization of the tangential flow filtration manufacturing step. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Synthesis of ZnO decorated graphene nanocomposite for enhanced photocatalytic properties

    NASA Astrophysics Data System (ADS)

    Gayathri, S.; Jayabal, P.; Kottaisamy, M.; Ramakrishnan, V.

    2014-05-01

    Zinc oxide/Graphene (GZ) composites with different concentrations of ZnO were successfully synthesized through simple chemical precipitation method. The X-ray diffraction pattern and the micro-Raman spectroscopic technique revealed the formation of GZ composite, and the energy dispersive X-ray spectrometry analysis showed the purity of the prepared samples. The ZnO nanoparticles decorated graphene sheets were clearly visible in the field emission scanning electron micrograph. Raman mapping was employed to analyze the homogeneity of the prepared samples. The diffuse-reflectance spectra clearly indicated that the formation of GZ composites promoted the absorption in the visible region also. The photocatalytic activity of ZnO and GZ composites was studied by the photodegradation of Methylene blue dye. The results revealed that the GZ composites exhibited a higher photocatalytic activity than pristine ZnO. Hence, we proposed a simple wet chemical method to synthesize GZ composite and its application on photocatalysis was demonstrated.

  8. A facile solvothermal method to produce graphene-ZnS composites for superior photoelectric applications

    NASA Astrophysics Data System (ADS)

    Lei, Yun; Chen, Feifei; Li, Rong; Xu, Jun

    2014-07-01

    In this experiment, flake graphite (<30 μm) was prepared as raw materials. Graphite oxide is prepared with Hummers method by low temperature, middle temperature and high temperature, and further treated with super-sonic oscillation to get graphene oxide. Graphene-zinc sulfide composites were synthesized through a simple solvothermal method using thiourea or sodium sulfide as sulfur source in the ethylene glycol or ethylenediamine, respectively. The products were characterized by X-ray and SEM, and analyzed by the transient photocurrent response and electrochemical impedance spectra. The results indicate that the properties of graphene-zinc sulfide composites prepared with thiourea in ethylene glycol are superior to those of blank-ZnS and composites prepared with sodium sulfide and ethylenediamine, which is attributed to electron capture and transfer ability of graphene resulting in a more efficient separation of the photoexcited charge carriers from ZnS-graphene composites.

  9. Patterned forests of vertically-aligned multiwalled carbon nanotubes using metal salt catalyst solutions.

    PubMed

    Garrett, David J; Flavel, Benjamin S; Baronian, Keith H R; Downard, Alison J

    2013-01-01

    A simple method for producing patterned forests of multiwalled carbon nanotubes (MWCNTs) is described. An aqueous metal salt solution is spin-coated onto a substrate patterned with photoresist by standard methods. The photoresist is removed by acetone washing leaving the acetone-insoluble catalyst pattern on the substrate. Dense forests of vertically aligned (VA) MWCNTs are grown on the patterned catalyst layers by chemical vapour deposition. The procedures have been demonstrated by growing MWCNT forests on two substrates: silicon and conducting graphitic carbon films. The forests adhere strongly to the substrates and when grown directly on carbon film, offer a simple method of preparing MWCNT electrodes.

  10. Facile generation of cell microarrays using vacuum degassing and coverslip sweeping.

    PubMed

    Wang, Min S; Luo, Zhen; Cherukuri, Sundar; Nitin, Nitin

    2014-07-15

    A simple method to generate cell microarrays with high-percentage well occupancy and well-defined cell confinement is presented. This method uses a synergistic combination of vacuum degassing and coverslip sweeping. The vacuum degassing step dislodges air bubbles from the microwells, which in turn enables the cells to enter the microwells, while the physical sweeping step using a glass coverslip removes the excess cells outside the microwells. This low-cost preparation method provides a simple solution to generating cell microarrays that can be performed in basic research laboratories and point-of-care settings for routine cell-based screening assays. Copyright © 2014 Elsevier Inc. All rights reserved.

  11. Determination of Gentamicin Sulphate Composition and Related Substances in Pharmaceutical Preparations by LC with Charged Aerosol Detection

    PubMed Central

    Stypulkowska, Karolina; Fijalek, Zbigniew; Sarna, Katarzyna

    2010-01-01

    A new, simple and repeatable liquid chromatography method with charged aerosol detection (LC-CAD) for the determination of gentamicin sulphate composition and related substances has been developed. Gentamicin lacks of chromophores, therefore its determination is quite problematic. Using a universal CAD enables to achieve good separation without sample derivatization. Mass spectrometry was employed to confirm the LC-CAD peak profile. The proposed method was validated and applied for the determination of gentamicin sulphate composition and related substances in pharmaceutical preparations. PMID:21212825

  12. A combined simple bubbling method with high performance liquid chromatography purification strategy, higher radiochemical yield and purity and faster preparation of carbon-11-raclopride.

    PubMed

    Huang, Huacheng; Ning, Yanli; Zhang, Bucheng; Lou, Cen

    2015-01-01

    Carbon-11-raclopride (¹¹C-R) is a positron-emitting radiotracer successfully used for the study of cognitive control and widely applied in PET imaging. A simple automated preparation of ¹¹C-R by using the reaction of carbon-(11)-methyl triflate (¹¹C-MeOTF) or ¹¹C-methyl iodide (¹¹C-MeI) with demethylraclopride is described. Specifically we used a simple setup applied an additional "U" reaction vessel for ¹¹C-MeOTf compared with ¹¹C-MeI and assessed the influence of several solvents and of the amount of the percussor for ¹¹C-methylation of demethylraclopride by the bubbling method. The reversal of retention order between product and its precursor has been achieved for ¹¹C-R, enabling collection of the purified ¹¹C-R by using the HPLC column after shorter retention time. By the improved radiosynthesis and purification strategy, ¹¹C-R could be prepared with higher radiochemical yield than that of the previous studies. The yield for ¹¹C-MeOTf was 76% and for ¹¹C-CH3I >26% and with better radiochemical purity (>99% based on both ¹¹C-MeOTf and ¹¹C-MeI) as compared to the previously obtained purity of ¹¹C-R using HPLC method with acetonitrile as a part of mobile phase. Furthermore, by using ethanol as the organic modifier, residual solvent analysis prior to human injection could be avoided and ¹¹C-R could be injected directly following simple dilution and sterile filtration. Improved radiosynthesis and HPLC purification in combination with ethanol containing eluent, extremely shortened the time for preparation of ¹¹C-R, gave a higher radiochemical yield and purity for ¹¹C-R and can be used for multiple and faster synthesis of ¹¹C-R and probably for other ¹¹C-labeled radiopharmaceuticals.

  13. Synthesis of silica aerogel monoliths with controlled specific surface areas and pore sizes

    NASA Astrophysics Data System (ADS)

    Gao, Bingying; Lu, Shaoxiang; Kalulu, Mulenga; Oderinde, Olayinka; Ren, Lili

    2017-07-01

    To replace traditional preparation methods of silica aerogels, a small-molecule 1,2-epoxypropane (PO) has been introduced into the preparation process instead of using ammonia as the cross-linking agent, thus generating a lightweight, high porosity, and large surface area silica aerogel monolithic. We put forward a simple solution route for the chemical synthesis of silica aerogels, which was characterized by scanning electron microscopy (SEM), TEM, XRD, FTIR, thermogravimetric analysis (TGA) and the Brunauer-Emmett-Teller (BET) method In this paper, the effect of the amount of PO on the microstructure of silica aerogels is discussed. The BET surface areas and pore sizes of the resulting silica aerogels can be freely adjusted by changing the amount of PO, which will be helpful in promoting the development of silica aerogels to fabricate other porous materials with similar requirements. We also adopted a new organic solvent sublimation drying (OSSD) method to replace traditional expensive and dangerous drying methods such as critical point drying and freeze drying. This simple approach is easy to operate and has good repeatability, which will further facilitate actual applications of silica aerogels.

  14. Nano-sized crystalline drug production by milling technology.

    PubMed

    Moribe, Kunikazu; Ueda, Keisuke; Limwikrant, Waree; Higashi, Kenjirou; Yamamoto, Keiji

    2013-01-01

    Nano-formulation of poorly water-soluble drugs has been developed to enhance drug dissolution. In this review, we introduce nano-milling technology described in recently published papers. Factors affecting the size of drug crystals are compared based on the preparation methods and drug and excipient types. A top-down approach using the comminution process is a method conventionally used to prepare crystalline drug nanoparticles. Wet milling using media is well studied and several wet-milled drug formulations are now on the market. Several trials on drug nanosuspension preparation using different apparatuses, materials, and conditions have been reported. Wet milling using a high-pressure homogenizer is another alternative to preparing production-scale drug nanosuspensions. Dry milling is a simple method of preparing a solid-state drug nano-formulation. The effect of size on the dissolution of a drug from nanoparticles is an area of fundamental research, but it is sometimes incorrectly evaluated. Here, we discuss evaluation procedures and the associated problems. Lastly, the importance of quality control, process optimization, and physicochemical characterization are briefly discussed.

  15. Comparative study of six sequential spectrophotometric methods for quantification and separation of ribavirin, sofosbuvir and daclatasvir: An application on Laboratory prepared mixture, pharmaceutical preparations, spiked human urine, spiked human plasma, and dissolution test.

    PubMed

    Hassan, Wafaa S; Elmasry, Manal S; Elsayed, Heba M; Zidan, Dalia W

    2018-09-05

    In accordance with International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH) guidelines, six novel, simple and precise sequential spectrophotometric methods were developed and validated for the simultaneous analysis of Ribavirin (RIB), Sofosbuvir (SOF), and Daclatasvir (DAC) in their mixture without prior separation steps. These drugs are described as co-administered for treatment of Hepatitis C virus (HCV). HCV is the cause of hepatitis C and some cancers such as liver cancer (hepatocellular carcinoma) and lymphomas in humans. These techniques consisted of several sequential steps using zero, ratio and/or derivative spectra. DAC was first determined through direct spectrophotometry at 313.7 nm without any interference of the other two drugs while RIB and SOF can be determined after ratio subtraction through five methods; Ratio difference spectrophotometric method, successive derivative ratio method, constant center, isoabsorptive method at 238.8 nm, and mean centering of the ratio spectra (MCR) at 224 nm and 258 nm for RIB and SOF, respectively. The calibration curve is linear over the concentration ranges of (6-42), (10-70) and (4-16) μg/mL for RIB, SOF, and DAC, respectively. This method was successfully applied to commercial pharmaceutical preparation of the drugs, spiked human urine, and spiked human plasma. The above methods are very simple methods that were developed for the simultaneous determination of binary and ternary mixtures and so enhance signal-to-noise ratio. The method has been successfully applied to the simultaneous analysis of RIB, SOF, and DAC in laboratory prepared mixtures. The obtained results are statistically compared with those obtained by the official or reported methods, showing no significant difference with respect to accuracy and precision at p = 0.05. Copyright © 2018 Elsevier B.V. All rights reserved.

  16. Monodispersed ZIF-8 particles with enhanced performance for CO2 adsorption and heterogeneous catalysis

    NASA Astrophysics Data System (ADS)

    Guan, Yebin; Shi, Juanjuan; Xia, Ming; Zhang, Jun; Pang, Zhenfeng; Marchetti, Alessandro; Wang, Xiaohong; Cai, Jingsong; Kong, Xueqian

    2017-11-01

    Monodispersed zeolitic imidazolate frameworks (ZIFs) were prepared with a simple method using dimethylsulfoxide (DMSO) as solvent. This method yields ZIF-8 nanoparticles with a narrow particle size distribution of 90-110 nm and the dispersion is highly stable against agglomeration. These particles have larger nanosized porosity and enhanced CO2 adsorption capability compared to ZIF-8 prepared with different solvents such as methanol or N, N-dimethyl formamide. Their uniform size and surface chemistry also lead to superior performance in the Knoevenagel condensation reactions. The ZIF-8 nanoparticles possess high thermal stability up to 550 °C and the preparation steps are easy for scaling up which are favorable for industrial applications.

  17. A simple way to achieve bioinspired hybrid wettability surface with micro/nanopatterns for efficient fog collection.

    PubMed

    Yin, Kai; Du, Haifeng; Dong, Xinran; Wang, Cong; Duan, Ji-An; He, Jun

    2017-10-05

    Fog collection is receiving increasing attention for providing water in semi-arid deserts and inland areas. Inspired by the fog harvesting ability of the hydrophobic-hydrophilic surface of Namib desert beetles, we present a simple, low-cost method to prepare a hybrid superhydrophobic-hydrophilic surface. The surface contains micro/nanopatterns, and is prepared by incorporating femtosecond-laser fabricated polytetrafluoroethylene nanoparticles deposited on superhydrophobic copper mesh with a pristine hydrophilic copper sheet. The as-prepared surface exhibits enhanced fog collection efficiency compared with uniform (super)hydrophobic or (super)hydrophilic surfaces. This enhancement can be tuned by controlling the mesh number, inclination angle, and fabrication structure. Moreover, the surface shows excellent anti-corrosion ability after immersing in 1 M HCl, 1 M NaOH, and 10 wt% NaCl solutions for 2 hours. This work may provide insight into fabricating hybrid superhydrophobic-hydrophilic surfaces for efficient atmospheric water collection.

  18. A Simple and Rapid Protocol for Producing Yeast Extract from Saccharomyces cerevisiae Suitable for Preparing Bacterial Culture Media

    PubMed Central

    Zarei, Omid; Dastmalchi, Siavoush; Hamzeh-Mivehroud, Maryam

    2016-01-01

    Yeasts, especially Saccharomyces cerevisiae, are one of the oldest organisms with broad spectrum of applications, owing to their unique genetics and physiology. Yeast extract, i.e. the product of yeast cells, is extensively used as nutritional resource in bacterial culture media. The aim of this study was to develop a simple, rapid and cost benefit process to produce the yeast extract. In this procedure mechanical methods such as high temperature and pressure were utilized to produce the yeast extract. The growth of the bacteria feed with the produced yeast extract was monitored in order to assess the quality of the product. The results showed that the quality of the produced yeast extract was very promising concluded from the growth pattern of bacterial cells in media prepared from this product and was comparable with that of the three commercial yeast extracts in terms of bacterial growth properties. One of the main advantages of the current method was that no chemicals and enzymes were used, leading to the reduced production cost. The method is very simple and cost effective, and can be performed in a reasonable time making it suitable for being adopted by research laboratories. Furthermore, it can be scaled up to produce large quantities for industrial applications. PMID:28243289

  19. Fast and accurate preparation fatty acid methyl esters by microwave-assisted derivatization in the yeast Saccharomyces cerevisiae.

    PubMed

    Khoomrung, Sakda; Chumnanpuen, Pramote; Jansa-ard, Suwanee; Nookaew, Intawat; Nielsen, Jens

    2012-06-01

    We present a fast and accurate method for preparation of fatty acid methyl esters (FAMEs) using microwave-assisted derivatization of fatty acids present in yeast samples. The esterification of free/bound fatty acids to FAMEs was completed within 5 min, which is 24 times faster than with conventional heating methods. The developed method was validated in two ways: (1) through comparison with a conventional method (hot plate) and (2) through validation with the standard reference material (SRM) 3275-2 omega-3 and omega-6 fatty acids in fish oil (from the Nation Institute of Standards and Technology, USA). There were no significant differences (P>0.05) in yields of FAMEs with both validations. By performing a simple modification of closed-vessel microwave heating, it was possible to carry out the esterification in Pyrex glass tubes kept inside the closed vessel. Hereby, we are able to increase the number of sample preparations to several hundred samples per day as the time for preparation of reused vessels was eliminated. Pretreated cell disruption steps are not required, since the direct FAME preparation provides equally quantitative results. The new microwave-assisted derivatization method facilitates the preparation of FAMEs directly from yeast cells, but the method is likely to also be applicable for other biological samples.

  20. Automated digital image analysis of islet cell mass using Nikon's inverted eclipse Ti microscope and software to improve engraftment may help to advance the therapeutic efficacy and accessibility of islet transplantation across centers.

    PubMed

    Gmyr, Valery; Bonner, Caroline; Lukowiak, Bruno; Pawlowski, Valerie; Dellaleau, Nathalie; Belaich, Sandrine; Aluka, Isanga; Moermann, Ericka; Thevenet, Julien; Ezzouaoui, Rimed; Queniat, Gurvan; Pattou, Francois; Kerr-Conte, Julie

    2015-01-01

    Reliable assessment of islet viability, mass, and purity must be met prior to transplanting an islet preparation into patients with type 1 diabetes. The standard method for quantifying human islet preparations is by direct microscopic analysis of dithizone-stained islet samples, but this technique may be susceptible to inter-/intraobserver variability, which may induce false positive/negative islet counts. Here we describe a simple, reliable, automated digital image analysis (ADIA) technique for accurately quantifying islets into total islet number, islet equivalent number (IEQ), and islet purity before islet transplantation. Islets were isolated and purified from n = 42 human pancreata according to the automated method of Ricordi et al. For each preparation, three islet samples were stained with dithizone and expressed as IEQ number. Islets were analyzed manually by microscopy or automatically quantified using Nikon's inverted Eclipse Ti microscope with built-in NIS-Elements Advanced Research (AR) software. The AIDA method significantly enhanced the number of islet preparations eligible for engraftment compared to the standard manual method (p < 0.001). Comparisons of individual methods showed good correlations between mean values of IEQ number (r(2) = 0.91) and total islet number (r(2) = 0.88) and thus increased to r(2) = 0.93 when islet surface area was estimated comparatively with IEQ number. The ADIA method showed very high intraobserver reproducibility compared to the standard manual method (p < 0.001). However, islet purity was routinely estimated as significantly higher with the manual method versus the ADIA method (p < 0.001). The ADIA method also detected small islets between 10 and 50 µm in size. Automated digital image analysis utilizing the Nikon Instruments software is an unbiased, simple, and reliable teaching tool to comprehensively assess the individual size of each islet cell preparation prior to transplantation. Implementation of this technology to improve engraftment may help to advance the therapeutic efficacy and accessibility of islet transplantation across centers.

  1. Chemistry Notes

    ERIC Educational Resources Information Center

    School Science Review, 1972

    1972-01-01

    Short articles describe preparation of clean iron sheet for corrosion experiments, models of crystalline structures using glass marbles, photographic production of diffraction grids for producing analogies of X-ray diffraction patterns, and a simple method of determining a reactivity series for the common metals. (AL)

  2. Going Beyond, Going Further: The Preparation of Acid-Base Titration Curves.

    ERIC Educational Resources Information Center

    McClendon, Michael

    1984-01-01

    Background information, list of materials needed, and procedures used are provided for a simple technique for generating mechanically plotted acid-base titration curves. The method is suitable for second-year high school chemistry students. (JN)

  3. Evaluating the efficiency of spectral resolution of univariate methods manipulating ratio spectra and comparing to multivariate methods: An application to ternary mixture in common cold preparation

    NASA Astrophysics Data System (ADS)

    Moustafa, Azza Aziz; Salem, Hesham; Hegazy, Maha; Ali, Omnia

    2015-02-01

    Simple, accurate, and selective methods have been developed and validated for simultaneous determination of a ternary mixture of Chlorpheniramine maleate (CPM), Pseudoephedrine HCl (PSE) and Ibuprofen (IBF), in tablet dosage form. Four univariate methods manipulating ratio spectra were applied, method A is the double divisor-ratio difference spectrophotometric method (DD-RD). Method B is double divisor-derivative ratio spectrophotometric method (DD-RD). Method C is derivative ratio spectrum-zero crossing method (DRZC), while method D is mean centering of ratio spectra (MCR). Two multivariate methods were also developed and validated, methods E and F are Principal Component Regression (PCR) and Partial Least Squares (PLSs). The proposed methods have the advantage of simultaneous determination of the mentioned drugs without prior separation steps. They were successfully applied to laboratory-prepared mixtures and to commercial pharmaceutical preparation without any interference from additives. The proposed methods were validated according to the ICH guidelines. The obtained results were statistically compared with the official methods where no significant difference was observed regarding both accuracy and precision.

  4. Magnesium oxide prepared via metal-chitosan complexation method: Application as catalyst for transesterification of soybean oil and catalyst deactivation studies

    NASA Astrophysics Data System (ADS)

    Almerindo, Gizelle I.; Probst, Luiz F. D.; Campos, Carlos E. M.; de Almeida, Rusiene M.; Meneghetti, Simoni M. P.; Meneghetti, Mario R.; Clacens, Jean-Marc; Fajardo, Humberto V.

    2011-10-01

    A simple method to prepare magnesium oxide catalysts for biodiesel production by transesterification reaction of soybean oil with ethanol is proposed. The method was developed using a metal-chitosan complex. Compared to the commercial oxide, the proposed catalysts displayed higher surface area and basicity values, leading to higher yield in terms of fatty acid ethyl esters (biodiesel). The deactivation of the catalyst due to contact with CO2 and H2O present in the ambient air was verified. It was confirmed that the active catalytic site is a hydrogenocarbonate adsorption site.

  5. An efficient and cost-effective method for preparing transmission electron microscopy samples from powders

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

    Wen, Haiming; Lin, Yaojun; Seidman, David N.

    The preparation of transmission electron microcopy (TEM) samples from powders with particle sizes larger than ~100 nm poses a challenge. The existing methods are complicated and expensive, or have a low probability of success. Herein, we report a modified methodology for preparation of TEM samples from powders, which is efficient, cost-effective, and easy to perform. This method involves mixing powders with an epoxy on a piece of weighing paper, curing the powder–epoxy mixture to form a bulk material, grinding the bulk to obtain a thin foil, punching TEM discs from the foil, dimpling the discs, and ion milling the dimpledmore » discs to electron transparency. Compared with the well established and robust grinding–dimpling–ion-milling method for TEM sample preparation for bulk materials, our modified approach for preparing TEM samples from powders only requires two additional simple steps. In this article, step-by-step procedures for our methodology are described in detail, and important strategies to ensure success are elucidated. Furthermore, our methodology has been applied successfully for preparing TEM samples with large thin areas and high quality for many different mechanically milled metallic powders.« less

  6. An efficient and cost-effective method for preparing transmission electron microscopy samples from powders

    DOE PAGES

    Wen, Haiming; Lin, Yaojun; Seidman, David N.; ...

    2015-09-09

    The preparation of transmission electron microcopy (TEM) samples from powders with particle sizes larger than ~100 nm poses a challenge. The existing methods are complicated and expensive, or have a low probability of success. Herein, we report a modified methodology for preparation of TEM samples from powders, which is efficient, cost-effective, and easy to perform. This method involves mixing powders with an epoxy on a piece of weighing paper, curing the powder–epoxy mixture to form a bulk material, grinding the bulk to obtain a thin foil, punching TEM discs from the foil, dimpling the discs, and ion milling the dimpledmore » discs to electron transparency. Compared with the well established and robust grinding–dimpling–ion-milling method for TEM sample preparation for bulk materials, our modified approach for preparing TEM samples from powders only requires two additional simple steps. In this article, step-by-step procedures for our methodology are described in detail, and important strategies to ensure success are elucidated. Furthermore, our methodology has been applied successfully for preparing TEM samples with large thin areas and high quality for many different mechanically milled metallic powders.« less

  7. A Simple and Selective Fluorescent Sensor Chip for Indole-3-Butyric Acid in Mung Bean Sprouts Based on Molecularly Imprinted Polymer Coatings

    PubMed Central

    Chang, Jiahua; Bahethan, Bota; Muhammad, Turghun; Yakup, Burabiye; Abbas, Mamatimin

    2017-01-01

    In this paper, we report the preparation of molecularly imprinted polymer coatings on quartz chips for selective solid-phase microextraction and fluorescence sensing of the auxin, indole-3-butyric acid. The multiple copolymerization method was used to prepare polymer coatings on silylated quartz chips. The polymer preparation conditions (e.g., the solvent, monomer, and cross-linker) were investigated systemically to enhance the binding performance of the imprinted coatings. Direct solid-phase fluorescence measurements on the chips facilitated monitoring changes in coating performance. The average binding capacity of an imprinted polymer coated chip was approximately 152.9 µg, which was higher than that of a non-imprinted polymer coated chip (60.8 µg); the imprinted coatings showed the highest binding to IBA among the structural analogues, indicating that the coatings possess high selectivity toward the template molecule. The developed method was used for the determination of the auxin in mung bean extraction, and the recovery was found to be in the range of 91.5% to 97.5%, with an RSD (n = 3) of less than 7.4%. Thus, the present study provides a simple method for fabricating a fluorescent sensor chip for selective analysis. PMID:28837081

  8. Simple morphological control over functional diversity of SERS materials

    NASA Astrophysics Data System (ADS)

    Semenova, A. A.; Goodilin, E. A.

    2018-03-01

    Nowadays, surface-enhanced Raman spectroscopy (SERS) becomes a promising universal low-cost and real-time tool in biomedical applications, medical screening or forensic analysis allowing for detection of different molecules below nanomolar concentrations. Silver nanoparticles and nanostructures have proven to be a common choice for SERS measurements due to a tunable plasmon resonance, high stability and facile fabrication methods. However, a proper design of silver-based nanomaterials for highly sensitive SERS applications still remains a challenge. In this work, effective and simple preparation methods of various silver nanostructures are proposed and systematically developed using aqueous diamminesilver (I) hydroxide as a precursor.

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

    PubMed

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

    2018-02-01

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

  10. Electrochemistry at Nanometer-Scaled Electrodes

    ERIC Educational Resources Information Center

    Watkins, John J.; Bo Zhang; White, Henry S.

    2005-01-01

    Electrochemical studies using nanometer-scaled electrodes are leading to better insights into electrochemical kinetics, interfacial structure, and chemical analysis. Various methods of preparing electrodes of nanometer dimensions are discussed and a few examples of their behavior and applications in relatively simple electrochemical experiments…

  11. Vertical Patellar Dislocation: Reduction by the Push Up and Rotate Method, A Case Report and Literature Review.

    PubMed

    Ahmad Khan, Hayat; Bashir Shah, Adil; Kamal, Younis

    2016-11-01

    Patellar dislocation is an emergency. Vertical patellar dislocation is rare, often seen in adolescents and mostly due to sports injuries or high-velocity trauma. Few cases have been reported in the literature. Closed or open reduction under general anesthesia is often needed. We report a case of vertical locked patellar dislocation in a 26-year-old male, which was reduced by a simple closed method under spinal anaesthesia. A literature review regarding the various methods of treatment is also discussed. A 26-year-old male experienced a trivial accident while descending stairs, sustaining patellar dislocation. The closed method of reduction was attempted, using a simple technique. Reduction was confirmed and postoperative rehabilitation was started. Follow-up was uneventful. Vertical patellar dislocations are encountered rarely in the emergency department. Adolescents are not the only victims, and high-velocity trauma is not the essential cause. Unnecessary manipulation should be avoided. The closed reduction method is simple, but the surgeon should be prepared for open reduction.

  12. Efficient method for preparation of highly purified lipopolysaccharides by hydrophobic interaction chromatography.

    PubMed

    Muck, A; Ramm, M; Hamburger, M

    1999-09-10

    A method for the efficient preparation of highly purified lipopolysaccharides (LPSs) by hydrophobic interaction chromatography (HIC) has been developed. The procedure can be used for the purification of cell wall bound LPSs after hot phenol-water extraction and for the isolation of extracellular LPSs from the supernatant, respectively. The method described has been tested with artificial mixtures containing LPSs, polysaccharide, protein and RNA and subsequently employed for the preparative purification of two LPSs of different origin, namely the extracellular LPS secreted by Escherichia coli E49 into the culture medium, and the cell wall bound LPS from Pseudomonas aeruginosa VA11465/1. Compared to currently used methods for LPS purification such as enzymatic digestion and ultracentrifugation, the chromatographic separation reported here combines superior purity with minimal loss of LPS, high reproducibility and simple handling. The removal of contaminants such as protein, RNA and polysaccharides and the recovery of LPSs were monitored by appropriate assays.

  13. [Preparation and antimicrobial effect of aromatic, natural and bacteriostatic foot wash with skin care].

    PubMed

    Gao, Su-Hua; Zhao, Guo-Xiang; Yang, Xiao-Dong; Xu, Ling-Ling

    2013-06-01

    To prepare the aromatic, natural and bacteriostatic foot wash with skin care and research the inhibition effect on the different bacteria and pathogenic fungus which cause dermatophytosis. It was prepared by using Sophoraflavescens and Dictamnus dasycarpus as materials with the addition of Aloe extract, essential oil, surfactant, etc. The antifungal and antibacterial activity was researched by the levitation liquid quantitative method. The foot wash smelled faintly scent. The use of this product can produce a rich foam. The inhibitory rate were all more than 90%. The preparation process of the foot wash was simple. It has obviously bacteriostatic and fungistatic effect.

  14. Preparation and Tribological Study of Biodegradable Lubrication Films on Si Substrate

    PubMed Central

    Shi, Shih-Chen; Huang, Teng-Feng; Wu, Jhen-Yu

    2015-01-01

    A novel method for preparing eco-biodegradable lubricant based on hydroxypropyl methylcellulose (HPMC) via hydration process is demonstrated. The smooth and homogeneous HPMC coating has a uniform thickness (~35 μm). It has been demonstrated that the preparation parameters play a critical role in controlling the lubricating behavior of the coating; in addition, excess HPMC and water concentration suppress the tribology properties. Nevertheless, a remarkable friction-reduction and anti-wear performance has been obtained. Impressively, the preparation parameter of 5% HPMC + 30 mL water significantly improves lubricant performance and durability. A simple approach for the water-degradability evaluation of HPMC is proposed. PMID:28788029

  15. Determination of Bosentan in Pharmaceutical Preparations by Linear Sweep, Square Wave and Differential Pulse Voltammetry Methods

    PubMed Central

    Atila, Alptug; Yilmaz, Bilal

    2015-01-01

    In this study, simple, fast and reliable cyclic voltammetry (CV), linear sweep voltammetry (LSV), square wave voltammetry (SWV) and differential pulse voltammetry (DPV) methods were developed and validated for determination of bosentan in pharmaceutical preparations. The proposed methods were based on electrochemical oxidation of bosentan at platinum electrode in acetonitrile solution containing 0.1 M TBACIO4. The well-defined oxidation peak was observed at 1.21 V. The calibration curves were linear for bosentan at the concentration range of 5-40 µg/mL for LSV and 5-35 µg/mL for SWV and DPV methods, respectively. Intra- and inter-day precision values for bosentan were less than 4.92, and accuracy (relative error) was better than 6.29%. The mean recovery of bosentan was 100.7% for pharmaceutical preparations. No interference was found from two tablet excipients at the selected assay conditions. Developed methods in this study are accurate, precise and can be easily applied to Tracleer and Diamond tablets as pharmaceutical preparation. PMID:25901151

  16. Determination of bosentan in pharmaceutical preparations by linear sweep, square wave and differential pulse voltammetry methods.

    PubMed

    Atila, Alptug; Yilmaz, Bilal

    2015-01-01

    In this study, simple, fast and reliable cyclic voltammetry (CV), linear sweep voltammetry (LSV), square wave voltammetry (SWV) and differential pulse voltammetry (DPV) methods were developed and validated for determination of bosentan in pharmaceutical preparations. The proposed methods were based on electrochemical oxidation of bosentan at platinum electrode in acetonitrile solution containing 0.1 M TBACIO4. The well-defined oxidation peak was observed at 1.21 V. The calibration curves were linear for bosentan at the concentration range of 5-40 µg/mL for LSV and 5-35 µg/mL for SWV and DPV methods, respectively. Intra- and inter-day precision values for bosentan were less than 4.92, and accuracy (relative error) was better than 6.29%. The mean recovery of bosentan was 100.7% for pharmaceutical preparations. No interference was found from two tablet excipients at the selected assay conditions. Developed methods in this study are accurate, precise and can be easily applied to Tracleer and Diamond tablets as pharmaceutical preparation.

  17. Assessment of cell concentration and viability of isolated hepatocytes using flow cytometry.

    PubMed

    Wigg, Alan J; Phillips, John W; Wheatland, Loretta; Berry, Michael N

    2003-06-01

    The assessment of cell concentration and viability of freshly isolated hepatocyte preparations has been traditionally performed using manual counting with a Neubauer counting chamber and staining for trypan blue exclusion. Despite the simple and rapid nature of this assessment, concerns about the accuracy of these methods exist. Simple flow cytometry techniques which determine cell concentration and viability are available yet surprisingly have not been extensively used or validated with isolated hepatocyte preparations. We therefore investigated the use of flow cytometry using TRUCOUNT Tubes and propidium iodide staining to measure cell concentration and viability of isolated rat hepatocytes in suspension. Analysis using TRUCOUNT Tubes provided more accurate and reproducible measurement of cell concentration than manual cell counting. Hepatocyte viability, assessed using propidium iodide, correlated more closely than did trypan blue exclusion with all indicators of hepatocyte integrity and function measured (lactate dehydrogenase leakage, cytochrome p450 content, cellular ATP concentration, ammonia and lactate removal, urea and albumin synthesis). We conclude that flow cytometry techniques can be used to measure cell concentration and viability of isolated hepatocyte preparations. The techniques are simple, rapid, and more accurate than manual cell counting and trypan blue staining and the results are not affected by protein-containing media.

  18. Preparation of magnetic and pH-responsive chitosan microcapsules via sonochemical method.

    PubMed

    Xu, Fengzhi; Zhao, Tianqi; Wang, Shurong; Liu, Songfeng; Yang, Ting; Li, Zhanfeng; Wang, Hongyan; Cui, Xuejun

    2016-01-01

    Magnetic and pH-responsive chitosan microcapsules (MPRCMCs) were prepared by a simple sonochemical method. Superparamagnetic oleic acid modified Fe3O4 nanoparticles (OA-Fe3O4 NPs) and hydrophobic drugs could be directly loaded into MPRCMCs during sonication. The obtained microcapsules had a well-defined spherical morphology with the average size of 2 μm. The microcapsules showed an excellent magnetic property. In addition, the pH-responsive controlled release of coumarin 6 (C6) from MPRCMCs indicated that the developed microcapsules could be a promising candidate for drugs carriers.

  19. Phenolate constrained geometry polymerization catalyst and method for preparing

    DOEpatents

    Marks, Tobin J.; Chen, You-Xian

    1999-01-01

    The subject invention involves a method of preparing and the constrained geometry catalyst thereby prepared of the general formula Ar'R4(O)Ar"R'.sub.4 M(CH.sub.2 Ph).sub.2 where Ar' is a phenyl or naphthyl group; Ar" is a cyclopentadienyl or indenyl group, R and R' are H or alkyl substituents (C.ltoreq.10) and M is Ti, Zr or Hf. The synthetic method involves a simple alkane elimination approach which permits a "one-pot" procedure. The catalyst, when combined with a cocatalyst such as Pb.sub.3 C.sup.+ B(Ar.sub.3.sup.F).sub.4 BAr.sub.3.sup.F or methyl alumoxane where Ar.sup.F is a fluoroaryl group, is an effective catalyst for the polymerization of .alpha.-olefins such as ethylene, propylene and styrene.

  20. Stability of sotalol hydrochloride in extemporaneously prepared oral suspension formulations.

    PubMed

    Sidhom, Madiha B; Rivera, Nadya; Almoazen, Hassan; Taft, David R; Kirschenbaum, Harold L

    2005-01-01

    The physical, chemical, and microbial stabilities of extemporaneously compounded oral liquid formulations of sotalol hydrochloride were studied. Sotalol hydrochloride oral liquid suspensions (5mg/mL) were prepared from commercially available tablets (Betapace) in a 1:1 mixture of Ora-Plus: Ora-Sweet, a 1:1 mixture of Ora-Plus:Ora-Sweet SF, and a 1:2.4 mixture of simple syrup:methylcellulose vehicle. Six batches of each formulation were prepared; three were stored at refrigerated temperature (2 deg to 8 deg C) and three at room temperature (20 deg to 25 deg C). Samples were collected from each batch weekly for 6 weeks, and again at 12 weeks. Samples were analyzed by means of a high-performance liquid chromatographic method, and the concentrations obtained were compared to the theoretical time zero value. Samples were examined for pH, odor, color, and consistency changes. The suspensions also were evaluated for their microbial stability. Sotalol hydrochloride oral liquid suspensions (5mg/mL) were chemically stable for 12 weeks regardless of storage conditions (room temperature or refrigerated). Bacterial growth was not supported by any of the formulations. Suspensions stored at refrigerated temperature retained better physical quality (e.g., odor, color, and consistency) than suspensions stored at room temperature. Overall, this study demonstrates that oral formulations of sotalol hydrochloride can be readily prepared with commercially available vehicles. The method of preparation is relatively simple, the materials are relatively inexpensive, and the products have a shelf-life of at least 12 weeks.

  1. Integrity of chromatin and replicating DNA in nuclei released from fission yeast by semi-automated grinding in liquid nitrogen

    PubMed Central

    2011-01-01

    Background Studies of nuclear function in many organisms, especially those with tough cell walls, are limited by lack of availability of simple, economical methods for large-scale preparation of clean, undamaged nuclei. Findings Here we present a useful method for nuclear isolation from the important model organism, the fission yeast, Schizosaccharomyces pombe. To preserve in vivo molecular configurations, we flash-froze the yeast cells in liquid nitrogen. Then we broke their tough cell walls, without damaging their nuclei, by grinding in a precision-controlled motorized mortar-and-pestle apparatus. The cryo-ground cells were resuspended and thawed in a buffer designed to preserve nuclear morphology, and the nuclei were enriched by differential centrifugation. The washed nuclei were free from contaminating nucleases and have proven well-suited as starting material for genome-wide chromatin analysis and for preparation of fragile DNA replication intermediates. Conclusions We have developed a simple, reproducible, economical procedure for large-scale preparation of endogenous-nuclease-free, morphologically intact nuclei from fission yeast. With appropriate modifications, this procedure may well prove useful for isolation of nuclei from other organisms with, or without, tough cell walls. PMID:22088094

  2. Facile Synthesis of Carbon Nanosphere/NiCo2O4 Core-shell Sub-microspheres for High Performance Supercapacitor

    PubMed Central

    Li, Delong; Gong, Youning; Zhang, Yupeng; Luo, Chengzhi; Li, Weiping; Fu, Qiang; Pan, Chunxu

    2015-01-01

    This paper introduced a process to prepare the carbon nanosphere (CNS)/NiCo2O4 core-shell sub-microspheres. That is: 1) CNSs were firstly prepared via a simple hydrothermal method; 2) a layer of NiCo2O4 precursor was coated on the CNS surface; 3) finally the composite was annealed at 350 °C for 2 hours in the air, and the CNS/NiCo2O4 core-shell sub-microspheres were obtained. This core-shell sub-microsphere was prepared with a simple, economical and environmental-friendly hydrothermal method, and was suitable for large-scale production, which expects a promising electrode candidate for high performance energy storage applications. Electrochemical experiments revealed that the composite exhibited remarkable electrochemical performances with high capacitance and desirable cycle life at high rates, such as: 1) the maximum specific capacitance was up to 1420 F/g at 1 A/g; 2) about 98.5% of the capacitance retained after 3000 charge-discharge cycles; 3) the capacitance retention was about 72% as the current density increase from 1 A/g to 10 A/g. PMID:26245982

  3. Integrity of chromatin and replicating DNA in nuclei released from fission yeast by semi-automated grinding in liquid nitrogen.

    PubMed

    Givens, Robert M; Mesner, Larry D; Hamlin, Joyce L; Buck, Michael J; Huberman, Joel A

    2011-11-16

    Studies of nuclear function in many organisms, especially those with tough cell walls, are limited by lack of availability of simple, economical methods for large-scale preparation of clean, undamaged nuclei. Here we present a useful method for nuclear isolation from the important model organism, the fission yeast, Schizosaccharomyces pombe. To preserve in vivo molecular configurations, we flash-froze the yeast cells in liquid nitrogen. Then we broke their tough cell walls, without damaging their nuclei, by grinding in a precision-controlled motorized mortar-and-pestle apparatus. The cryo-ground cells were resuspended and thawed in a buffer designed to preserve nuclear morphology, and the nuclei were enriched by differential centrifugation. The washed nuclei were free from contaminating nucleases and have proven well-suited as starting material for genome-wide chromatin analysis and for preparation of fragile DNA replication intermediates. We have developed a simple, reproducible, economical procedure for large-scale preparation of endogenous-nuclease-free, morphologically intact nuclei from fission yeast. With appropriate modifications, this procedure may well prove useful for isolation of nuclei from other organisms with, or without, tough cell walls.

  4. Determination of Caffeine in Beverages by High Performance Liquid Chromatography.

    ERIC Educational Resources Information Center

    DiNunzio, James E.

    1985-01-01

    Describes the equipment, procedures, and results for the determination of caffeine in beverages by high performance liquid chromatography. The method is simple, fast, accurate, and, because sample preparation is minimal, it is well suited for use in a teaching laboratory. (JN)

  5. Preparation, structural characterization, and catalytic performance of Pd(II) and Pt(II) complexes derived from cellulose Schiff base

    NASA Astrophysics Data System (ADS)

    Baran, Talat; Yılmaz Baran, Nuray; Menteş, Ayfer

    2018-05-01

    In this study, we reported production, characterization, and catalytic behavior of two novel heterogeneous palladium(II) and platinum(II) catalysts derived from cellulose biopolymer. In order to eliminate the use of toxic organic or inorganic solvents and to reduce the use of excess energy in the coupling reactions, we have developed a very simple, rapid, and eco-friendly microwave irradiation protocol. The developed microwave-assisted method of Suzuki cross coupling reactions produced excellent reaction yields in the presence of cellulose supported palladium and platinum (II) catalysts. Moreover, the catalysts easily regenerated after simple filtration, and they gave good reusability. This study revealed that the designed catalysts and method provide clean, simple, rapid, and impressive catalytic performance for Suzuki coupling reactions.

  6. Facile preparation of super durable superhydrophobic materials.

    PubMed

    Wu, Lei; Zhang, Junping; Li, Bucheng; Fan, Ling; Li, Lingxiao; Wang, Aiqin

    2014-10-15

    The low stability, complicated and expensive fabrication procedures seriously hinder practical applications of superhydrophobic materials. Here we report an extremely simple method for preparing super durable superhydrophobic materials, e.g., textiles and sponges, by dip coating in fluoropolymers (FPs). The morphology, surface chemical composition, mechanical, chemical and environmental stabilities of the superhydrophobic textiles were investigated. The results show how simple the preparation of super durable superhydrophobic textiles can be! The superhydrophobic textiles outperform their natural counterparts and most of the state-of-the-art synthetic superhydrophobic materials in stability. The intensive mechanical abrasion, long time immersion in various liquids and repeated washing have no obvious influence on the superhydrophobicity. Water drops are spherical in shape on the samples and could easily roll off after these harsh stability tests. In addition, this simple dip coating approach is applicable to various synthetic and natural textiles and can be easily scaled up. Furthermore, the results prove that a two-tier roughness is helpful but not essential with regard to the creation of super durable superhydrophobic textiles. The combination of microscale roughness of textiles and materials with very low surface tension is enough to form super durable superhydrophobic textiles. According to the same procedure, superhydrophobic polyurethane sponges can be prepared, which show high oil absorbency, oil/water separation efficiency and stability. Copyright © 2014 Elsevier Inc. All rights reserved.

  7. A simple and rapid method for the reversible removal of lipids from a membrane-bound enzyme.

    PubMed Central

    Goodman, S L; Isern de Caldentey, M; Wheeler, K P

    1978-01-01

    A simple, rapid and reproducible method for the reversible removal of lipids from a membrane-bound enzyme is described. Essentially, a membrane preparation containing (Na+ + K+)-dependent adenosine triphosphatase was extracted with the non-ionic detergent Lubrol WX in the presence of glycerol, and partial separation of protein from lipid was achieved with the use of only two centrifugations. About 74% of the endogenous phospholipid and 79% of the cholesterol were removed, concomitant with a virtually complete loss of ouabain-sensitive adenosine triphosphatase activity, but with retention of 60-100% of the K+-dependent phosphatase activity. The addition of pure phosphatidylserine re-activated the enzyme to more than 80% of the initial activity, and up to 30% of the protein was recovered. Excess of phosphatidylserine could be washed off the enzyme to give a stable 'reconstituted' preparation. The effects of variation in the experimental conditions were examined, and the results are discussed with respect to the possibility of adapting the method to the study of other lipid-dependent enzymes bound to membranes. PMID:147078

  8. A Simple and Reproducible Method to Prepare Membrane Samples from Freshly Isolated Rat Brain Microvessels.

    PubMed

    Brzica, Hrvoje; Abdullahi, Wazir; Reilly, Bianca G; Ronaldson, Patrick T

    2018-05-07

    The blood-brain barrier (BBB) is a dynamic barrier tissue that responds to various pathophysiological and pharmacological stimuli. Such changes resulting from these stimuli can greatly modulate drug delivery to the brain and, by extension, cause considerable challenges in the treatment of central nervous system (CNS) diseases. Many BBB changes that affect pharmacotherapy, involve proteins that are localized and expressed at the level of endothelial cells. Indeed, such knowledge on BBB physiology in health and disease has sparked considerable interest in the study of these membrane proteins. From a basic science research standpoint, this implies a requirement for a simple but robust and reproducible method for isolation of microvessels from brain tissue harvested from experimental animals. In order to prepare membrane samples from freshly isolated microvessels, it is essential that sample preparations be enriched in endothelial cells but limited in the presence of other cell types of the neurovascular unit (i.e., astrocytes, microglia, neurons, pericytes). An added benefit is the ability to prepare samples from individual animals in order to capture the true variability of protein expression in an experimental population. In this manuscript, details regarding a method that is utilized for isolation of rat brain microvessels and preparation of membrane samples are provided. Microvessel enrichment, from samples derived, is achieved by using four centrifugation steps where dextran is included in the sample buffer. This protocol can easily be adapted by other laboratories for their own specific applications. Samples generated from this protocol have been shown to yield robust experimental data from protein analysis experiments that can greatly aid the understanding of BBB responses to physiological, pathophysiological, and pharmacological stimuli.

  9. A simple chromatographic method for purification of egg lecithin.

    PubMed

    Nielsen, J R

    1980-06-01

    Egg lecithin was purified from the CdCl2-lecithin complex by column chromatography on Alumina. The yield from 5 eggs was 2.8 g. The purified lecithin had correct chemical values for pure lecithin and a fatty acid composition similar to lecithin prepared by other methods. The method probably can be adapted for purification of other lipids containing the phosphocholine moiety and for purification of synthetic lecithin.

  10. The simple determination method for anthocyanidin aglycones in fruits using ultra-high-performance liquid chromatography.

    PubMed

    Shim, You-Shin; Yoon, Won-Jin; Kim, Dong-Man; Watanabe, Masaki; Park, Hyun-Jin; Jang, Hae Won; Lee, Jangho; Ha, Jaeho

    2015-01-01

    The simple determination method for anthocyanidin aglycones in fruits using ultra-high-performance liquid chromatography (UHPLC) coupled with the heating-block acidic hydrolysis method was validated through the precision, accuracy and linearity. The UHPLC separation was performed on a reversed-phase C18 column (particle size 2 μm, i.d. 2 mm, length 100 mm) with a photodiode-array detector. The limits of detection and quantification of the UHPLC analyses were 0.09 and 0.29 mg/kg for delphinidin, 0.08 and 0.24 mg/kg for cyanidin, 0.09 and 0.26 mg/kg for petunidin, 0.14 and 0.42 mg/kg for pelargonidin, 0.16 and 0.48 mg/kg for peonidin and 0.30 and 0.91 mg/kg for malvidin, respectively. The intra- and inter-day precisions of individual anthocyanidin aglycones were <10.3%. All calibration curves exhibited good linearity (r = 0.999) within the tested ranges. The total run time of UHPLC was 8 min. The simple preparation method with UHPLC detection in this study presented herein significantly improved the speed and the simplicity for preparation step of delphinidin, cyanidin, petunidin, pelargonidin, peonidin and malvidin in fruits. Especially, the UHPLC detection exhibited good resolution in spite of shorter run time about four times than conventional HPLC detection. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  11. Indirect enantioseparation of fluoxetine in mouse serum by derivatization with 1R-(-)-menthyl chloroformate followed by ultra high performance liquid chromatography and quadrupole time-of-flight mass spectrometry.

    PubMed

    Zhao, Jing; Jin, Yan; Shin, Yujin; Jeong, Kyung Min; Lee, Jeongmi

    2016-03-01

    Here we describe a simple and sensitive analytical method for the enantioselective quantification of fluoxetine in mouse serum using ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry. The sample preparation method included a simple deproteinization with acetonitrile in 50 μL of serum, followed by derivatization of the extracts in 50 μL of 2 mM 1R-(-)-menthyl chloroformate at 45ºC for 55 min. These conditions were statistically optimized through response surface methodology using a central composite design. Under the optimized conditions, neither racemization nor kinetic resolution occurred. The derivatized diastereomers were readily resolved on a conventional sub-2 μm C18 column under a simple gradient elution of aqueous methanol containing 0.1% formic acid. The established method was validated and found to be linear, precise, and accurate over the concentration range of 5.0-1000.0 ng/mL for both R and S enantiomers (r(2) > 0.993). Stability tests of the prepared samples at three different concentration levels showed that the R- and S-fluoxetine derivatives were relatively stable for 48 h. No significant matrix effects were observed. Last, the developed method was successfully used for enantiomeric analysis of real serum samples collected at a number of time points from mice administered with racemic fluoxetine. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. CuIn(S,Se)(2) thin films prepared from a novel thioacetic acid-based solution and their photovoltaic application.

    PubMed

    Xie, Yian; Liu, Yufeng; Wang, Yaoming; Zhu, Xiaolong; Li, Aimin; Zhang, Lei; Qin, Mingsheng; Lü, Xujie; Huang, Fuqiang

    2014-04-28

    Low-cost and high-yield preparation of CuInSe2 films is the bottleneck for promising CuInSe2-based thin film solar cells. Here, we developed a simple, safe and cost-effective method using thioacetic acid to fabricate the absorber films of CuIn(S,Se)2 (CISSe). Dissolution of Cu2O and In(OH)3 in thioacetic acid was attributed to the strong coordination ability of S. The adhesive precursor solution can be prepared without any heating, centrifugation and inert gas protection, superior to the previously reported methods. The precursor CISSe layer was easily deposited in air by spin coating to ensure low cost. Uniform and compact CISSe thin films with well-crystallized and pure-phased CISSe grains were obtained after one step annealing. The as-prepared CISSe thin films were successfully applied to solar cells and a energy conversion efficiency of 6.75% was achieved. This facile preparation provides a low-cost and easy method to fabricate Cu-based thin film solar cells.

  13. Spectrophotometric determination of dopaminergic drugs used for Parkinson's disease, cabergoline and ropinirole, in pharmaceutical preparations.

    PubMed

    Onal, Armağan; Cağlar, Sena

    2007-04-01

    Simple and reproducible spectrophotometric methods have been developed for determination of dopaminergic drugs used for Parkinson's disease, cabergoline (CAB) and ropinirole hydrochloride (ROP), in pharmaceutical preparations. The methods are based on the reactions between the studied drug substances and ion-pair agents [methyl orange (MO), bromocresol green (BCG) and bromophenol blue (BPB)] producing yellow colored ion-pair complexes in acidic buffers, after extracting in dichloromethane, which are spectrophotometrically determined at the appropriate wavelength of ion-pair complexes. Beer's law was obeyed within the concentration range from 1.0 to 35 microg ml(-1). The developed methods were applied successfully for the determination of these drugs in tablets.

  14. A simple, cheap, one-minute method to mount insect pins for use as sharp-tipped probes in plant dissection.

    PubMed

    Frohlich, Michael W

    2005-08-01

    A new method is presented for twist mounting insect pins onto standard dissecting (teasing) needles. Insect pins, with their sharp points, are ideal for fine dissection of plants, especially of shoot tips and early developing flower buds. Twist mounting makes them convenient and effective dissecting tools to prepare specimens for SEM.

  15. Preparation of sterile xenon-133 in saline for tissue perfusion studies

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

    DiPiazza, H.J.; Harbert, J.C.

    1983-11-01

    A simple, inexpensive method of obtaining Xe-133 in sterile saline is presented. The method uses commercial xenon ampules supplied for pulmonary ventilation studies. As much as 10% of the gas activity can be recovered per aliquot by cooling the saline to 4/sup 0/C. The specific activities obtained are adequate for most tissue perfusion studies.

  16. Rapid microwave assisted synthesis of graphene nanosheets/polyethyleneimine/gold nanoparticle composite and its application to the selective electrochemical determination of dopamine.

    PubMed

    Ponnusamy, Vinoth Kumar; Mani, Veerappan; Chen, Shen-Ming; Huang, Wan-Tran; Jen, Jen-Fon

    2014-03-01

    In this study, a simple and fast microwave assisted chemical reduction method for the preparation of graphene nanosheet/polyethyleneimine/gold nanoparticle (GNS/PEI/AuNP) composite was developed. PEI, a cationic polymer, was used both as a non-covalent functionalizing agent for the graphene oxide nanosheets (GONSs) through electrostatic interactions in the aqueous medium and also as a stabilizing agent for the formation of AuNPs on PEI wrapped GNSs. This preparation method involves a simple mixing step followed by a simultaneous microwave assisted chemical reduction of the GONSs and gold ions. The prepared composite exhibits the dispersion of high density AuNPs which were densely decorated on the large surface area of the PEI wrapped GNS. X-ray photoelectron spectroscopy, powder X-ray diffraction, high-resolution transmission electron microscopy, field-emission scanning electron microscopy with energy dispersive X-ray spectroscopy, and thermo-gravimetric analysis, were used to characterize the properties of the resultant composite. The prepared GNS/PEI/AuNP composite film exhibited excellent electrocatalytical activity towards the selective determination of dopamine in the presence of ascorbic acid, which showed potential application in electrochemical sensors. The applicability of the presented sensor was also demonstrated for the determination of dopamine in human urine samples. © 2013 Elsevier B.V. All rights reserved.

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

    Gu, Lina; He, Xiaomei; Wu, Zhenyu, E-mail: zhenyuwuhn@sina.com

    Highlights: • Mesoporous Fe{sub 3}O{sub 4}/hydroxyapatite composite was synthesized by a simple, efficient and environmental friendly method. • The prepared material had a large surface area, high pore volume, and good magnetic separability. • DOX-loaded Fe{sub 3}O{sub 4}/hydroxyapatite composite exhibited surprising slow drug release behavior and pH-dependent behavior. - Abstract: In this contribution, we introduced a simple, efficient, and green method of preparing a mesoporous Fe{sub 3}O{sub 4}/hydroxyapatite (HA) composite. The as-prepared material had a large surface area, high pore volume, and good magnetic separability, which made it suitable for targeted drug delivery systems. The chemotherapeutic agent doxorubicin (DOX) wasmore » used to investigate the drug release behavior of Fe{sub 3}O{sub 4}/HA composite. The drug release profiles displayed a little burst effect and pH-dependent behavior. The release rate of DOX at pH 5.8 was larger than that at pH 7.4, which could be attributed to DOX protonation in acid medium. In addition, the released DOX concentrations remained at 0.83 and 1.39 μg/ml at pH 7.4 and 5.8, respectively, which indicated slow, steady, and safe release rates. Therefore, the as-prepared Fe{sub 3}O{sub 4}/hydroxyapatite composite could be an efficient platform for targeted anticancer drug delivery.« less

  18. Continuous flow hydrogenation of nitroarenes, azides and alkenes using maghemite-Pd nanocomposites

    EPA Science Inventory

    Maghemite-supported ultra-fine Pd (1-2 nm) nanoparticles, prepared by a simple co-precipitation method, find application in the catalytic continuous flow hydrogenation of nitroarenes, azides, and alkenes wherein they play an important role in reduction of various functional group...

  19. Evaluate the contribution of the mixture components on the longevity and performance of FC-5 : [summary].

    DOT National Transportation Integrated Search

    2014-05-01

    At its most basic, an asphalt mixture is asphalt : binder and crushed stone aggregate. This : seemingly simple mixture is very complex; method : of preparation and application, additives, and : aggregate type all influence the quality and : durabilit...

  20. Determination of lansoprazole in human plasma by rapid resolution liquid chromatography-electrospray tandem mass spectrometry: application to a bioequivalence study on Chinese volunteers.

    PubMed

    Wu, Guo-Lan; Zhou, Hui-Li; Shentu, Jian-Zhong; He, Qiao-Jun; Yang, Bo

    2008-12-15

    A simple, sensitive and rapid LC/MS/MS method was developed for the quantification of lansoprazole in human plasma. After a simple sample preparation procedure by one-step protein precipitation with acetonitrile, lansoprazole and the internal standard bicalutamide were chromatographed on a Zorbax SB-C(18) (3.0 mm x 150 mm, 3.5 microm, Agilent) column with the mobile phase consisted of methanol-water (70:30, v/v, containing 5 mM ammonium formate, pH was adjusted to 7.85 by 1% ammonia solution). Detection was performed on a triple quadrupole tandem mass spectrometry by multiple reaction monitoring (MRM) mode via negative eletrospray ionization source (ESI(-)). The lower limit of quantification was 5.5 ng/mL, and the assay exhibited a linear range of 5.5-2200.0 ng/mL. The validated method was successfully applied to investigate the bioequivalence between two kinds of preparation (test vs. reference product) in twenty-eight healthy male Chinese volunteers.

  1. Development and validation of spectrophotometric methods for estimating amisulpride in pharmaceutical preparations.

    PubMed

    Sharma, Sangita; Neog, Madhurjya; Prajapati, Vipul; Patel, Hiren; Dabhi, Dipti

    2010-01-01

    Five simple, sensitive, accurate and rapid visible spectrophotometric methods (A, B, C, D and E) have been developed for estimating Amisulpride in pharmaceutical preparations. These are based on the diazotization of Amisulpride with sodium nitrite and hydrochloric acid, followed by coupling with N-(1-naphthyl)ethylenediamine dihydrochloride (Method A), diphenylamine (Method B), beta-naphthol in an alkaline medium (Method C), resorcinol in an alkaline medium (Method D) and chromotropic acid in an alkaline medium (Method E) to form a colored chromogen. The absorption maxima, lambda(max), are at 523 nm for Method A, 382 and 490 nm for Method B, 527 nm for Method C, 521 nm for Method D and 486 nm for Method E. Beer's law was obeyed in the concentration range of 2.5-12.5 microg mL(-1) in Method A, 5-25 and 10-50 microg mL(-1) in Method B, 4-20 microg mL(-1) in Method C, 2.5-12.5 microg mL(-1) in Method D and 5-15 microg mL(-1) in Method E. The results obtained for the proposed methods are in good agreement with labeled amounts, when marketed pharmaceutical preparations were analyzed.

  2. [A New Simple Technique for Producing Labeled Monoclonal Antibodies for Antibody Pair Screening in Sandwich-ELISA].

    PubMed

    Zaripov, M M; Afanasieva, G V; Glukhova, X A; Trizna, Y A; Glukhov, A S; Beletsky, I P; Prusakova, O V

    2015-01-01

    A simple and fast method for obtaining biotin-labeled monoclonal antibodies was developed usingcontent of hybridoma culture supernatant sufficient to select antibody pairs in sandwich ELISA. The method consists in chemical biotinylation of antigen-bound antibodies in a well of ELISA plate. Using as an example target Vaccinia virus A27L protein it was shown that the yield of biotinylated reactant is enough to set comprehensive sandwich ELISA for a moderate size panel of up to 25 monoclonal antibodies with an aim to determine candidate pairs. The technique is a cheap and effective solution since it avoids obtaining preparative amounts of antibodies.

  3. Simple and rapid quantification of brominated vegetable oil in commercial soft drinks by LC–MS

    PubMed Central

    Chitranshi, Priyanka; da Costa, Gonçalo Gamboa

    2016-01-01

    We report here a simple and rapid method for the quantification of brominated vegetable oil (BVO) in soft drinks based upon liquid chromatography–electrospray ionization mass spectrometry. Unlike previously reported methods, this novel method does not require hydrolysis, extraction or derivatization steps, but rather a simple “dilute and shoot” sample preparation. The quantification is conducted by mass spectrometry in selected ion recording mode and a single point standard addition procedure. The method was validated in the range of 5–25 μg/mL BVO, encompassing the legal limit of 15 μg/mL established by the US FDA for fruit-flavored beverages in the US market. The method was characterized by excellent intra- and inter-assay accuracy (97.3–103.4%) and very low imprecision [0.5–3.6% (RSD)]. The direct nature of the quantification, simplicity, and excellent statistical performance of this methodology constitute clear advantages in relation to previously published methods for the analysis of BVO in soft drinks. PMID:27451219

  4. C18-coated stir bar sorptive extraction combined with high performance liquid chromatography-electrospray tandem mass spectrometry for the analysis of sulfonamides in milk and milk powder.

    PubMed

    Yu, Chunhe; Hu, Bin

    2012-02-15

    A simple, rapid, sensitive, inexpensive and less sample consuming method of C(18)-stir bar sorptive extraction (SBSE)-high performance liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) was proposed for the determination of six sulfonamides in milk and milk powder samples. C(18) silica particles coated stir bar was prepared by adhesion method, and two kinds of adhesive glue, polydimethylsiloxane (PDMS) sol and epoxy glue were tried. It was found that the C(18)-coated stir bar prepared by PDMS sol as adhesive glue is more robust than that prepared by epoxy glue when liquid desorption was employed, in terms of both lifetime and organic solvent tolerance. The preparation of C(18) stir bar was simple with good mechanic strength and the stir bar could be reused for more than 20 times. Granular coating has relatively high specific surface area and is propitious to sorptive extraction based process. Compared to conventional PDMS SBSE coating, C(18) coating shows good affinity to the target polar/weak polar sulfonamides. To achieve optimum SBSE extraction performance, several parameters including extraction and desorption time, ionic strength, sample pH and stirring speed were investigated. The detection limits of the proposed method for six sulfonamides were in the range of 0.9-10.5 μg/L for milk and 2.7-31.5 μg/kg for milk powder. Good linearities were obtained for sulfonamides with the correlation coefficients (R) above 0.9922. Finally, the proposed method was successfully applied to the determination of sulfonamides in milk and milk powder samples and satisfied recoveries of spiked target compounds in real samples were obtained. Copyright © 2012 Elsevier B.V. All rights reserved.

  5. Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

    PubMed

    Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

    2014-12-01

    Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ((1)H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Simple, rapid method for the preparation of isotopically labeled formaldehyde

    DOEpatents

    Hooker, Jacob Matthew [Port Jefferson, NY; Schonberger, Matthias [Mains, DE; Schieferstein, Hanno [Aabergen, DE; Fowler, Joanna S [Bellport, NY

    2011-10-04

    Isotopically labeled formaldehyde (*C.sup..sctn.H.sub.2O) is prepared from labeled methyl iodide (*C.sup..sctn.H.sub.3I) by reaction with an oxygen nucleophile having a pendant leaving group. The mild and efficient reaction conditions result in good yields of *C.sup..sctn.H.sub.2O with little or no *C isotopic dilution. The simple, efficient production of .sup.11CH.sub.2O is described. The use of the .sup.11CH.sub.2O for the formation of positron emission tomography tracer compounds is described. The reaction can be incorporated into automated equipment available to radiochemistry laboratories. The isotopically labeled formaldehyde can be used in a variety of reactions to provide radiotracer compounds for imaging studies as well as for scintillation counting and autoradiography.

  7. Influence of pH on optoelectronic properties of zinc sulphide thin films prepared using hydrothermal and spin coating method

    NASA Astrophysics Data System (ADS)

    Choudapur, V. H.; Bennal, A. S.; Raju, A. B.

    2018-04-01

    The ZnS nanomaterial is synthesized by hydrothermal method under optimized conditions using Zinc acetate and sodium sulphide as precursors. The Zinc Sulphide thin films are obtained by simple spin coating method with high optical transmittance. The prepared thin films are adhesive and uniform. The x-ray diffraction analysis showed that the films are polycrystalline in cubic phase with the preferred orientation along (111) direction. Current-voltage curves were recorded at room temperature using Keithley 617 programmable electrometer and conductivity is calculated for the film coated on ITO by two probe method. The pH of the solution is varied by using ammonia and hydrochloric acid. The comparative studies of effect of pH on the morphology, crystallanity and optoelectronic properties of the films are studied. It is observed that the pH of the solution has large influence on optoelectronic properties. The thin film prepared with neutral pH has higher crystallanity, bandgap and conductivity as compared to the samples prepared in acidic or basic solutions.

  8. Protein detection by Simple Western™ analysis.

    PubMed

    Harris, Valerie M

    2015-01-01

    Protein Simple© has taken a well-known protein detection method, the western blot, and revolutionized it. The Simple Western™ system uses capillary electrophoresis to identify and quantitate a protein of interest. Protein Simple© provides multiple detection apparatuses (Wes, Sally Sue, or Peggy Sue) that are suggested to save scientists valuable time by allowing the researcher to prepare the protein sample, load it along with necessary antibodies and substrates, and walk away. Within 3-5 h the protein will be separated by size, or charge, immuno-detection of target protein will be accurately quantitated, and results will be immediately made available. Using the Peggy Sue instrument, one study recently examined changes in MAPK signaling proteins in the sex-determining stage of gonadal development. Here the methodology is described.

  9. Preparation of superhydrophobic titanium surfaces via electrochemical etching and fluorosilane modification

    NASA Astrophysics Data System (ADS)

    Lu, Yao; Xu, Wenji; Song, Jinlong; Liu, Xin; Xing, Yingjie; Sun, Jing

    2012-12-01

    The preparation of superhydrophobic surfaces on hydrophilic metal substrates depends on both surface microstructures and low surface energy modification. In this study, a simple and inexpensive electrochemical method for preparing robust superhydrophobic titanium surfaces is reported. The neutral sodium chloride solution is used as electrolyte. Fluoroalkylsilane (FAS) was used to reduce the surface energy of the electrochemically etched surface. Scanning electron microscopy (SEM) images, energy-dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR) spectra, and contact angle measurement are performed to characterize the morphological features, chemical composition, and wettability of the titanium surfaces. Stability and friction tests indicate that the prepared titanium surfaces are robust. The analysis of electrolyte, reaction process, and products demonstrates that the electrochemical processing is very inexpensive and environment-friendly. This method is believed to be easily adaptable for use in large-scale industry productions to promote the application of superhydrophobic titanium surfaces in aviation, aerospace, shipbuilding, and the military industry.

  10. Single molecule targeted sequencing for cancer gene mutation detection.

    PubMed

    Gao, Yan; Deng, Liwei; Yan, Qin; Gao, Yongqian; Wu, Zengding; Cai, Jinsen; Ji, Daorui; Li, Gailing; Wu, Ping; Jin, Huan; Zhao, Luyang; Liu, Song; Ge, Liangjin; Deem, Michael W; He, Jiankui

    2016-05-19

    With the rapid decline in cost of sequencing, it is now affordable to examine multiple genes in a single disease-targeted clinical test using next generation sequencing. Current targeted sequencing methods require a separate step of targeted capture enrichment during sample preparation before sequencing. Although there are fast sample preparation methods available in market, the library preparation process is still relatively complicated for physicians to use routinely. Here, we introduced an amplification-free Single Molecule Targeted Sequencing (SMTS) technology, which combined targeted capture and sequencing in one step. We demonstrated that this technology can detect low-frequency mutations using artificially synthesized DNA sample. SMTS has several potential advantages, including simple sample preparation thus no biases and errors are introduced by PCR reaction. SMTS has the potential to be an easy and quick sequencing technology for clinical diagnosis such as cancer gene mutation detection, infectious disease detection, inherited condition screening and noninvasive prenatal diagnosis.

  11. Environment dependent enhanced photoluminescence and Boolean logic gates like behavior of Bi2O3 and Ag:Bi2O3 nanostructures

    NASA Astrophysics Data System (ADS)

    Hariharan, S.; Karthikeyan, B.

    2018-03-01

    In the evolution of nanotechnology research for smart and precise sensor fabrication, here we report the implementation of simple logic gate operations performing by luminescent nanostructures in biomolecule environment based on photoluminescence (PL) technique. This present work deals with the luminescence property of α-Bi2O3 and Ag modified α-Bi2O3 nanostructures for D-glucose and Bovine serum albumin (BSA) sensing applications. These nanostructures are prepared by simple co-precipitation method and their morphology are examined using transmission electron microscope (TEM). We explore the PL characteristics of the prepared nanostructures and observe their change in PL intensity in the presence of D-glucose and BSA molecules. Enhancement in PL intensity is observed in the presence of D-glucose and BSA. Based on the PL response of prepared nanostructures in the biomolecule environment, we demonstrate biophotonic logic gates including YES, PASS 0, OR and INHIBIT gates.

  12. Facile synthesis of biocompatible gold nanoparticles with organosilicone-coated surface properties

    NASA Astrophysics Data System (ADS)

    Xia, Lijin; Yi, Sijia; Lenaghan, Scott C.; Zhang, Mingjun

    2012-07-01

    In this study, a simple method for one-step synthesis of gold nanoparticles has been developed using an organosilicone surfactant, Silwet L-77, as both a reducing and capping agent. Synthesis of gold nanoparticles using this method is rapid and can be conducted conveniently at ambient temperature. Further refinement of the method, through the addition of sodium hydroxide and/or silver nitrate, allowed fine control over the size of spherical nanoparticles produced. Coated on the surface with organosilicone, the as-prepared gold nanoparticles were biocompatible and stable over the pH range from 5 to 12, and have been proven effective at transportation into MC3T3 osteoblast cells. The proposed method is simple, fast, and can produce size-controlled gold nanoparticles with unique surface properties for biomedical applications.

  13. Combination of saponification and dispersive liquid-liquid microextraction for the determination of tocopherols and tocotrienols in cereals by reversed-phase high-performance liquid chromatography.

    PubMed

    Shammugasamy, Balakrishnan; Ramakrishnan, Yogeshini; Ghazali, Hasanah M; Muhammad, Kharidah

    2013-07-26

    A simple sample preparation technique coupled with reversed-phase high-performance liquid chromatography was developed for the determination of tocopherols and tocotrienols in cereals. The sample preparation procedure involved a small-scale hydrolysis of 0.5g cereal sample by saponification, followed by the extraction and concentration of tocopherols and tocotrienols from saponified extract using dispersive liquid-liquid microextraction (DLLME). Parameters affecting the DLLME performance were optimized to achieve the highest extraction efficiency and the performance of the developed DLLME method was evaluated. Good linearity was observed over the range assayed (0.031-4.0μg/mL) with regression coefficients greater than 0.9989 for all tocopherols and tocotrienols. Limits of detection and enrichment factors ranged from 0.01 to 0.11μg/mL and 50 to 73, respectively. Intra- and inter-day precision were lower than 8.9% and the recoveries were around 85.5-116.6% for all tocopherols and tocotrienols. The developed DLLME method was successfully applied to cereals: rice, barley, oat, wheat, corn and millet. This new sample preparation approach represents an inexpensive, rapid, simple and precise sample cleanup and concentration method for the determination of tocopherols and tocotrienols in cereals. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Preparative separation and purification of steroidal saponins in Paris polyphylla var. yunnanensis by macroporous adsorption resins.

    PubMed

    Liu, Zhen; Wang, Jieyin; Gao, Wenyuan; Man, Shuli; Wang, Ying; Liu, Changxiao

    2013-07-01

    Saponins are active compounds in natural products. Many researchers have tried to find the method for knowing their concentration in herbs. Some methods, such as solid-liquid extraction and solvent extraction, have been developed. However, the extraction methods of the steroidal saponins from Paris polyphylla Smith var. yunnanensis (Liliaceae) are not fully researched. To establish a simple extraction method for the separation of steroidal saponins from the rhizomes of P. polyphylla Smith var. yunnanensis. Macroporous adsorption resins were used for the separation of steroidal saponins. To select the most suitable resins, seven kinds of macroporous resins were selected in this study. The static adsorption and desorption tests on macroporous resins were determined. Also, we optimized the temperature and the ethanol concentration in the extraction method by the contents of five kinds of saponins. Then, we compared the extraction method with two other methods. D101 resin demonstrated the best adsorption and desorption properties for steroidal saponins. Its adsorption data fits best to the Freundlich adsorption model. The contents of steroidal saponins in the product were 4.83-fold increased with recovery yields of 85.47%. The process achieved simple and effective enrichment and separation for steroidal saponins. The method provides a scientific basis for large-scale preparation of steroidal saponins from the Rhizoma Paridis and other plants.

  15. Phenolate constrained geometry polymerization catalyst and method for preparing

    DOEpatents

    Marks, T.J.; Chen, Y.X.

    1999-01-05

    The subject invention involves a method of preparing and the constrained geometry catalyst thereby prepared of the general formula Ar{prime}R4(O)Ar{double_prime}R{prime}{sub 4}M(CH{sub 2}Ph){sub 2} where Ar{prime} is a phenyl or naphthyl group; Ar{double_prime} is a cyclopentadienyl or indenyl group, R and R{prime} are H or alkyl substituents (C{<=}10) and M is Ti, Zr or Hf. The synthetic method involves a simple alkane elimination approach which permits a ``one-pot`` procedure. The catalyst, when combined with a cocatalyst such as Pb{sub 3}C{sup +}B(Ar{sub 3}{sup F}){sub 4}BAr{sub 3}{sup F} or methyl alumoxane where Ar{sup F} is a fluoroaryl group, is an effective catalyst for the polymerization of {alpha}-olefins such as ethylene, propylene and styrene. 1 fig.

  16. Improvements in soft gelatin capsule sample preparation for USP-based simethicone FTIR analysis.

    PubMed

    Hargis, Amy D; Whittall, Linda B

    2013-02-23

    Due to the absence of a significant chromophore, Simethicone raw material and finished product analysis is achieved using a FTIR-based method that quantifies the polydimethylsiloxane (PDMS) component of the active ingredient. The method can be found in the USP monographs for several dosage forms of Simethicone-containing pharmaceutical products. For soft gelatin capsules, the PDMS assay values determined using the procedure described in the USP method were variable (%RSDs from 2 to 9%) and often lower than expected based on raw material values. After investigation, it was determined that the extraction procedure used for sample preparation was causing loss of material to the container walls due to the hydrophobic nature of PDMS. Evaluation revealed that a simple dissolution of the gelatin capsule fill in toluene provided improved assay results (%RSDs≤0.5%) as well as a simplified and rapid sample preparation. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. A simple method for semi-random DNA amplicon fragmentation using the methylation-dependent restriction enzyme MspJI.

    PubMed

    Shinozuka, Hiroshi; Cogan, Noel O I; Shinozuka, Maiko; Marshall, Alexis; Kay, Pippa; Lin, Yi-Han; Spangenberg, German C; Forster, John W

    2015-04-11

    Fragmentation at random nucleotide locations is an essential process for preparation of DNA libraries to be used on massively parallel short-read DNA sequencing platforms. Although instruments for physical shearing, such as the Covaris S2 focused-ultrasonicator system, and products for enzymatic shearing, such as the Nextera technology and NEBNext dsDNA Fragmentase kit, are commercially available, a simple and inexpensive method is desirable for high-throughput sequencing library preparation. MspJI is a recently characterised restriction enzyme which recognises the sequence motif CNNR (where R = G or A) when the first base is modified to 5-methylcytosine or 5-hydroxymethylcytosine. A semi-random enzymatic DNA amplicon fragmentation method was developed based on the unique cleavage properties of MspJI. In this method, random incorporation of 5-methyl-2'-deoxycytidine-5'-triphosphate is achieved through DNA amplification with DNA polymerase, followed by DNA digestion with MspJI. Due to the recognition sequence of the enzyme, DNA amplicons are fragmented in a relatively sequence-independent manner. The size range of the resulting fragments was capable of control through optimisation of 5-methyl-2'-deoxycytidine-5'-triphosphate concentration in the reaction mixture. A library suitable for sequencing using the Illumina MiSeq platform was prepared and processed using the proposed method. Alignment of generated short reads to a reference sequence demonstrated a relatively high level of random fragmentation. The proposed method may be performed with standard laboratory equipment. Although the uniformity of coverage was slightly inferior to the Covaris physical shearing procedure, due to efficiencies of cost and labour, the method may be more suitable than existing approaches for implementation in large-scale sequencing activities, such as bacterial artificial chromosome (BAC)-based genome sequence assembly, pan-genomic studies and locus-targeted genotyping-by-sequencing.

  18. Magnetic Fields: Visible and Permanent.

    ERIC Educational Resources Information Center

    Winkeljohn, Dorothy R.; Earl, Robert D.

    1983-01-01

    Children will be able to see the concept of a magnetic field translated into a visible reality using the simple method outlined. Standard shelf paper, magnets, iron filings, and paint in a spray can are used to prepare a permanent and well-detailed picture of the magnetic field. (Author/JN)

  19. Counting Tree Growth Rings Moderately Difficult to Distinguish

    Treesearch

    C. B. Briscoe; M. Chudnoff

    1964-01-01

    There is an extensive literature dealing with techniques and gadgets to facilitate counting tree growth rings. A relatively simple method is described below, satisfactory for species too difficult to count in the field, but not sufficiently difficult to require the preparation of microscope slides nor staining techniques.

  20. Comparative study between derivative spectrophotometry and multivariate calibration as analytical tools applied for the simultaneous quantitation of Amlodipine, Valsartan and Hydrochlorothiazide

    NASA Astrophysics Data System (ADS)

    Darwish, Hany W.; Hassan, Said A.; Salem, Maissa Y.; El-Zeany, Badr A.

    2013-09-01

    Four simple, accurate and specific methods were developed and validated for the simultaneous estimation of Amlodipine (AML), Valsartan (VAL) and Hydrochlorothiazide (HCT) in commercial tablets. The derivative spectrophotometric methods include Derivative Ratio Zero Crossing (DRZC) and Double Divisor Ratio Spectra-Derivative Spectrophotometry (DDRS-DS) methods, while the multivariate calibrations used are Principal Component Regression (PCR) and Partial Least Squares (PLSs). The proposed methods were applied successfully in the determination of the drugs in laboratory-prepared mixtures and in commercial pharmaceutical preparations. The validity of the proposed methods was assessed using the standard addition technique. The linearity of the proposed methods is investigated in the range of 2-32, 4-44 and 2-20 μg/mL for AML, VAL and HCT, respectively.

  1. 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.

  2. Structural mechanical and antibacterial properties of HPMC/SF-AgNPs nanocomposite films

    NASA Astrophysics Data System (ADS)

    Harish, K. V.; Rao, B. Lakshmeesha; Asha, S.; Vipin, C.; Sangappa, Y.

    2018-04-01

    In the present study, Hydroxypropyl Methylcellulose (HPMC) pure and HPMC/SF-AgNPs biopolymer nanocomposite films were prepared by simple solution casting method. The prepared nanocomposite films were characterized using UV-Visible spectroscopy(UV-Vis), X-ray diffraction (XRD) measurements. The mechanical properties of HPMC/SF-AgNPs nanocomposites were found to be decrease with increase in the AgNP's concentrations. The HPMC/SF-AgNPs nanocomposites showed very good antibacterial activity against human pathogens P. aeruginosa, E.coli, and S.aureus.

  3. Hierarchically ordered carbon tubes

    NASA Astrophysics Data System (ADS)

    Pan, Zheng-Wei; Zhu, Hao-Guo; Zhang, Zong-Tao; Im, Hee-Jung; Dai, Sheng; Beach, David B.; Lowndes, Douglas H.

    2003-04-01

    Micropatterns of hierarchically ordered carbon tubes (i.e., ordered carbon microtubes composed of aligned carbon nanotubes) were grown on a film-like iron/silica substrate consisting of ring-like catalyst patterns. The substrates were prepared by a combined technique, in which the sol-gel method was used to prepare catalyst film and transmission electron microscope grids were used as a shadow mask. In comparison with other techniques that involve sophisticated lithography, this approach represents a simple and low-cost way to the micropatterning of aligned carbon nanotubes.

  4. Search for Polarization Effects in the Antiproton Production Process

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

    Grzonka, D.; Kilian, K.; Ritman, J.

    For the production of a polarized antiproton beam, various methods have been suggested including the possibility that antiprotons may be produced polarized which will be checked experimentally. The polarization of antiprotons produced under typical conditions for antiproton beam preparation will be measured at the CERN/PS. If the production process creates some polarization, a polarized antiproton beam could be prepared by a rather simple modification of the antiproton beam facility. The detection setup and the expected experimental conditions are described.

  5. Research and preparation of ultra purity silicon tetrachloride

    NASA Astrophysics Data System (ADS)

    Wan, Ye; Zhao, Xiong; Yan, Dazhou; Yang, Dian; Li, Yunhao; Guo, Shuhu

    2017-10-01

    This article demonstrated a technology for producing ultra-purity silicon tetrachloride, which using the high purity SiCl4 as raw material through the method of combination ray reaction with purification. This technology could remove metal impurities and compounds impurities contained hydrogen effectively. The purity of product prepared by this technology can reach at 99.9999%, content of metal impurities can be low at 0.3PPb, meeting the requirement of industry easily. This technology has the advantages of simple process, continuous operation, and stable performance.

  6. Large scale preparation and crystallization of neuron-specific enolase.

    PubMed

    Ishioka, N; Isobe, T; Kadoya, T; Okuyama, T; Nakajima, T

    1984-03-01

    A simple method has been developed for the large scale purification of neuron-specific enolase [EC 4.2.1.11]. The method consists of ammonium sulfate fractionation of brain extract, and two subsequent column chromatography steps on DEAE Sephadex A-50. The chromatography was performed on a short (25 cm height) and thick (8.5 cm inside diameter) column unit that was specially devised for the large scale preparation. The purified enolase was crystallized in 0.05 M imidazole-HCl buffer containing 1.6 M ammonium sulfate (pH 6.39), with a yield of 0.9 g/kg of bovine brain tissue.

  7. A novel pretreatment method combining sealing technique with direct injection technique applied for improving biosafety.

    PubMed

    Wang, Xinyu; Gao, Jing-Lin; Du, Chaohui; An, Jing; Li, MengJiao; Ma, Haiyan; Zhang, Lina; Jiang, Ye

    2017-01-01

    People today have a stronger interest in the risk of biosafety in clinical bioanalysis. A safe, simple, effective method of preparation is needed urgently. To improve biosafety of clinical analysis, we used antiviral drugs of adefovir and tenofovir as model drugs and developed a safe pretreatment method combining sealing technique with direct injection technique. The inter- and intraday precision (RSD %) of the method were <4%, and the extraction recoveries ranged from 99.4 to 100.7%. Meanwhile, the results showed that standard solution could be used to prepare calibration curve instead of spiking plasma, acquiring more accuracy result. Compared with traditional methods, the novel method not only improved biosecurity of the pretreatment method significantly, but also achieved several advantages including higher precision, favorable sensitivity and satisfactory recovery. With these highly practical and desirable characteristics, the novel method may become a feasible platform in bioanalysis.

  8. Magnetically recyclable magnetite-ceria (Nanocat-Fe-Ce) nanocatalysts - applications in multicomponent reactions under benign conditions

    EPA Science Inventory

    A novel magnetite nanoparticle-supported ceria catalyst (Nanocat-Fe-Ce) has been successfully prepared by simple impregnation method and was well characterized by XRD, SIMS, FEG-SEM-EDS, and TEM. The exact nature of Nanocat-Fe-Ce was confirmed by X-ray photoelectron spectroscopy ...

  9. Kitchen Microbiology: It's Easier Than You Think!

    ERIC Educational Resources Information Center

    Wilcoxson, Catherine; Shand, Stacey M.; Shand, Richard F.

    1999-01-01

    Offers a simple experiment that tests the effectiveness of cleaners that inhibit bacterial growth. Outlines a step-by-step method for preparing culture media that can be used for isolation and propagation of microorganisms. Concludes that kitchen medium is as efficient as the professionally-made medium in supporting colony growth. (CCM)

  10. Preparation of CdS Nanoparticles by First-Year Undergraduates

    ERIC Educational Resources Information Center

    Winkelmann, Kurt; Noviello, Thomas; Brooks, Stephen

    2007-01-01

    The first year undergraduates use a simple method to synthesize 5-nm CdS nanoparticles in a water-in-oil microemulsion. The quantum size effect, the relationship between colors, optical absorbance, band-gap energy and the CdS particles affected by the formation of micelles are observed.

  11. The Pedagogy of Flipped Instruction in Oman

    ERIC Educational Resources Information Center

    Lane-Kelso, Mary

    2015-01-01

    "Flipping the classroom", or reverse instruction has been hailed the new pedagogical approach for preparing students for the 21st century. The idea behind this method is relatively simple. Instead of structuring class work to deliver direct instruction from the teacher in class and giving homework to students to practice outside of…

  12. Attitude Surveys Document Sampler.

    ERIC Educational Resources Information Center

    Walker, Albert, Comp.

    This packet presents results of a series of attitude surveys representing a variety of purposes, methods and defined publics. They range from a simple questionnaire prepared and mailed to a small group of key individuals by a public relations staff to scientifically derived surveys purchased from Louis Harris and Associates and other research…

  13. Nano-sized particles, processes of making, compositions and uses thereof

    DOEpatents

    O'Brien, Stephen [New York, NY; Yin, Ming [Los Alamos, NM

    2012-05-22

    The present invention describes methods for preparing high quality nanoparticles, i.e., metal oxide based nanoparticles of uniform size and monodispersity. The nanoparticles advantageously comprise organic alkyl chain capping groups and are stable in air and in nonpolar solvents. The methods of the invention provide a simple and reproducible procedure for forming transition metal oxide nanocrystals, with yields over 80%. The highly crystalline and monodisperse nanocrystals are obtained directly without further size selection; particle size can be easily and fractionally increased by the methods. The resulting nanoparticles can exhibit magnetic and/or optical properties. These properties result from the methods used to prepare them. Also advantageously, the nanoparticles of this invention are well suited for use in a variety of industrial applications, including cosmetic and pharmaceutical formulations and compositions.

  14. Anodic Oxidation of Etodolac and its Linear Sweep, Square Wave and Differential Pulse Voltammetric Determination in Pharmaceuticals

    PubMed Central

    Yilmaz, B.; Kaban, S.; Akcay, B. K.

    2015-01-01

    In this study, simple, fast and reliable cyclic voltammetry, linear sweep voltammetry, square wave voltammetry and differential pulse voltammetry methods were developed and validated for determination of etodolac in pharmaceutical preparations. The proposed methods were based on electrochemical oxidation of etodolac at platinum electrode in acetonitrile solution containing 0.1 M lithium perchlorate. The well-defined oxidation peak was observed at 1.03 V. The calibration curves were linear for etodolac at the concentration range of 2.5-50 μg/ml for linear sweep, square wave and differential pulse voltammetry methods, respectively. Intra- and inter-day precision values for etodolac were less than 4.69, and accuracy (relative error) was better than 2.00%. The mean recovery of etodolac was 100.6% for pharmaceutical preparations. No interference was found from three tablet excipients at the selected assay conditions. Developed methods in this study are accurate, precise and can be easily applied to Etol, Tadolak and Etodin tablets as pharmaceutical preparation. PMID:26664057

  15. Food adulteration analysis without laboratory prepared or determined reference food adulterant values.

    PubMed

    Kalivas, John H; Georgiou, Constantinos A; Moira, Marianna; Tsafaras, Ilias; Petrakis, Eleftherios A; Mousdis, George A

    2014-04-01

    Quantitative analysis of food adulterants is an important health and economic issue that needs to be fast and simple. Spectroscopy has significantly reduced analysis time. However, still needed are preparations of analyte calibration samples matrix matched to prediction samples which can be laborious and costly. Reported in this paper is the application of a newly developed pure component Tikhonov regularization (PCTR) process that does not require laboratory prepared or reference analysis methods, and hence, is a greener calibration method. The PCTR method requires an analyte pure component spectrum and non-analyte spectra. As a food analysis example, synchronous fluorescence spectra of extra virgin olive oil samples adulterated with sunflower oil is used. Results are shown to be better than those obtained using ridge regression with reference calibration samples. The flexibility of PCTR allows including reference samples and is generic for use with other instrumental methods and food products. Copyright © 2013 Elsevier Ltd. All rights reserved.

  16. Gravimetric method for the determination of diclofenac in pharmaceutical preparations.

    PubMed

    Tubino, Matthieu; De Souza, Rafael L

    2005-01-01

    A gravimetric method for the determination of diclofenac in pharmaceutical preparations was developed. Diclofenac is precipitated from aqueous solution with copper(II) acetate in pH 5.3 (acetic acid/acetate buffer). Sample aliquots had approximately the same quantity of the drug content in tablets (50 mg) or in ampules (75 mg). The observed standard deviation was about +/- 2 mg; therefore, the relative standard deviation (RSD) was approximately 4% for tablet and 3% for ampule preparations. The results were compared with those obtained with the liquid chromatography method recommended in the United States Pharmacopoeia using the statistical Student's t-test. Complete agreement was observed. It is possible to obtain more precise results using higher aliquots, for example 200 mg, in which case the RSD falls to 1%. This gravimetric method, contrary to what is expected for this kind of procedure, is relatively fast and simple to perform. The main advantage is the absolute character of the gravimetric analysis.

  17. Fabricated CeO2 nanopowders as a novel sensing platform for advanced forensic, electrochemical and photocatalytic applications

    NASA Astrophysics Data System (ADS)

    Rohini, B. S.; Nagabhushana, H.; Darshan, G. P.; Basavaraj, R. B.; Sharma, S. C.; Sudarmani, R.

    2017-11-01

    In Forensic investigation, identification of various types of ridge details are essential in order to fix the criminals associated in various crimes. Even though several methods and labeling agents are available to visualize latent finger prints (LFPs) there is still simple, accurate, cost-effective, and non-destructive tool is required. In the present work, CeO2 nanopowders (NPs) are prepared via simple solution combustion route using Tamarindus indica fruit extract as a fuel. The optimized NPs are utilized for visualization of LFPs on various surfaces by powder dusting method. Results revealed that visualized LFPs exhibit Level 3 features such as pores and ridge contours under normal light with high sensitivity and without background hindrance. The photometric characteristics of the prepared samples exhibit blue color emission and highly useful in warm light emitting diodes. The photocatalytic studies were carried out with different Methylene blue (MB) dye concentration and pH values. The obtained results reveal that the CeO2 NPs exhibits an excellent catalytic properties which can act as a good catalytic reagent. The findings demonstrate that the prepared NPs are quite useful as a labeling agent for visualization of LFPs, efficient catalysts for dye degradation as well as solid-state lighting applications.

  18. Synthesis and Characterization of AlCl3 Impregnated Molybdenum Oxide as Heterogeneous Nano-Catalyst for the Friedel-Crafts Acylation Reaction in Ambient Condition.

    PubMed

    Jadhav, Arvind H; Chinnappan, Amutha; Hiremath, Vishwanath; Seo, Jeong Gil

    2015-10-01

    Aluminum trichloride (AlCl3) impregnated molybdenum oxide heterogeneous nano-catalyst was prepared by using simple impregnation method. The prepared heterogeneous catalyst was characterized by powder X-ray diffraction, FT-IR spectroscopy, solid-state NMR spectroscopy, SEM imaging, and EDX mapping. The catalytic activity of this protocol was evaluated as heterogeneous catalyst for the Friedel-Crafts acylation reaction at room temperature. The impregnated MoO4(AlCl2)2 catalyst showed tremendous catalytic activity in Friedel-Crafts acylation reaction under solvent-free and mild reaction condition. As a result, 84.0% yield of acyl product with 100% consumption of reactants in 18 h reaction time at room temperature was achieved. The effects of different solvents system with MoO4(AlCl2)2 catalyst in acylation reaction was also investigated. By using optimized reaction condition various acylated derivatives were prepared. In addition, the catalyst was separated by simple filtration process after the reaction and reused several times. Therefore, heterogeneous MoO4(AlCl2)2 catalyst was found environmentally benign catalyst, very convenient, high yielding, and clean method for the Friedel-Crafts acylation reaction under solvent-free and ambient reaction condition.

  19. Spectrophotometric determination of meclizine hydrochloride and pyridoxine hydrochloride in laboratory prepared mixtures and in their pharmaceutical preparation

    NASA Astrophysics Data System (ADS)

    Ibrahim, Maha M.; Elzanfaly, Eman S.; El-Zeiny, Mohamed B.; Ramadan, Nesreen K.; Kelani, Khadiga M.

    2017-05-01

    In this paper, three rapid, simple, accurate and precise spectrophotometric methods were developed for the determination of meclizine hydrochloride in the presence of pyridoxine hydrochloride without previous separation. The methods under study are dual wavelength (DWL), ratio difference (RD) and continuous wavelet transform (CWT). On the other hand, pyridoxine hydrochloride (PYH) was determined directly at 291 nm. The methods obey Beer's law in the range of (5-50 μg/mL) for both compounds. All the methods were validated according to the ICH guidelines where the accuracy was found to be 98.29, 99.59, 100.42 and 100.62% for DWL, RD, CWT and PYH; respectively. Moreover the precision of the methods were calculated in terms of %RSD and it was found to be 0.545, 0.372, 1.287 and 0.759 for DWL, RD,CWT and PYH; respectively. The selectivity of the proposed methods was tested using laboratory prepared mixtures and assessed by applying the standard addition technique. So, they can be used for the routine analysis of pyridoxine hydrochloride and meclizine hydrochloride in quality-control laboratories.

  20. A series of spinel phase cathode materials prepared by a simple hydrothermal process for rechargeable lithium batteries

    NASA Astrophysics Data System (ADS)

    Liang, Yan-Yu; Bao, Shu-Juan; Li, Hu-Lin

    2006-07-01

    A series of spinel-structured materials have been prepared by a simple hydrothermal procedure in an aqueous medium. The new synthetic method is time and energy saving i.e., no further thermal treatment and extended grinding. The main experimental process involved the insertion of lithium into electrolytic manganese dioxide with glucose as a mild reductant in an autoclave. Both the hydrothermal temperature and the presence of glucose play the critical roles in determining the final spinel integrity. Particular electrochemical performance has also been systematically explored, and the results show that Al 3+, F - co-substituted spinels have the best combination of initial capacity and capacity retention among all these samples, exhibited the initial capacity of 115 mAh/g and maintained more than 90% of the initial value at the 50th cycle.

  1. One-step oxidation preparation of unfolded and good soluble graphene nanoribbons by longitudinal unzipping of carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Hu, Xiaolin; Hu, Yizhen; Huang, Jindan; Zhou, Ning; Liu, Yuhan; Wei, Lin; Chen, Xin; Zhuang, Naifeng

    2018-04-01

    A simple one-step method to prepare graphene nanoribbon (GNR) is reported in this paper. Compared with water steam etching, the oxidation and co-etching of dilute sulfuric acid can result in the more complete longitudinal unzipping of carbon nanotube, although there is no other strong oxidant. As-prepared GNRs are more flat and have more oxygenated functional groups along the edge. Moreover, they can steadily disperse in a water system. These make them suitable as a carrier for supporting palladium (Pd) nanoparticles. The Pd/GNR composite exhibits a superior electrocatalytic activity for ethanol oxidation.

  2. 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.

  3. Colloidal synthesis of silicon nanoparticles in molten salts.

    PubMed

    Shavel, A; Guerrini, L; Alvarez-Puebla, R A

    2017-06-22

    Silicon nanoparticles are unique materials with applications in a variety of fields, from electronics to catalysis and biomedical uses. Despite technological advancements in nanofabrication, the development of a simple and inexpensive route for the synthesis of homogeneous silicon nanoparticles remains highly challenging. Herein, we describe a new, simple and inexpensive colloidal synthetic method for the preparation, under normal pressure and mild temperature conditions, of relatively homogeneous spherical silicon nanoparticles of either ca. 4 or 6 nm diameter. The key features of this method are the selection of a eutectic salt mixture as a solvent, the identification of appropriate silicon alkoxide precursors, and the unconventional use of alkali earth metals as shape-controlling agents.

  4. 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.

  5. Novel sodium intercalated (NH4)2V6O16 platelets: High performance cathode materials for lithium-ion battery.

    PubMed

    Fei, Hailong; Wu, Xiaomin; Li, Huan; Wei, Mingdeng

    2014-02-01

    A simple and versatile method for preparation of novel sodium intercalated (NH4)2V6O16 is developed via a simple hydrothermal route. It is found that ammonium sodium vanadium bronze displays higher discharge capacity and better rate cyclic stability than ammonium vanadium bronze as lithium-ion battery cathode material because of smaller charge transfer resistance, which would favor superior discharge capacity and rate performance. Crown Copyright © 2013. Published by Elsevier Inc. All rights reserved.

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

    PubMed

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

    2016-05-30

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

  7. Non-invasive continuous imaging of drug release from soy-based skin equivalent using wide-field interferometry

    NASA Astrophysics Data System (ADS)

    Gabai, Haniel; Baranes-Zeevi, Maya; Zilberman, Meital; Shaked, Natan T.

    2013-04-01

    We propose an off-axis interferometric imaging system as a simple and unique modality for continuous, non-contact and non-invasive wide-field imaging and characterization of drug release from its polymeric device used in biomedicine. In contrast to the current gold-standard methods in this field, usually based on chromatographic and spectroscopic techniques, our method requires no user intervention during the experiment, and only one test-tube is prepared. We experimentally demonstrate imaging and characterization of drug release from soy-based protein matrix, used as skin equivalent for wound dressing with controlled anesthetic, Bupivacaine drug release. Our preliminary results demonstrate the high potential of our method as a simple and low-cost modality for wide-field imaging and characterization of drug release from drug delivery devices.

  8. Fast preparation of ultrafine monolayered transition-metal dichalcogenide quantum dots using electrochemical shock for explosive detection.

    PubMed

    Chen, Zhigang; Tao, Zhengxu; Cong, Shan; Hou, Junyu; Zhang, Dengsong; Geng, Fengxia; Zhao, Zhigang

    2016-09-15

    A simple, general and fast method called "electrochemical shock" is developed to prepare monolayered transition-metal dichalcogenide (TMD) QDs with an average size of 2-4 nm and an average thickness of 0.85 ± 0.5 nm with only about 10 min of ultrasonication. Just like nails hammered into a plate, the electrochemical shock with Al 3+ ions and the following extraction with the help of oleic acid can disintegrate bulk TMD crystals into ultrafine TMD QDs. The fast-prepared QDs are then applied to detect highly explosive molecules such as 2,4,6-trinitrophenol (TNP) with a low detection limit of 10 -6 M. Our versatile method could be broadly applicable for the fast production of ultrathin QDs of other materials with great promise for various applications.

  9. Synthesis of Hollow Sphere and 1D Structural Materials by Sol-Gel Process.

    PubMed

    Li, Fa-Liang; Zhang, Hai-Jun

    2017-08-25

    The sol-gel method is a simple and facile wet chemical process for fabricating advanced materials with high homogeneity, high purity, and excellent chemical reactivity at a relatively low temperature. By adjusting the processing parameters, the sol-gel technique can be used to prepare hollow sphere and 1D structural materials that exhibit a wide application in the fields of catalyst, drug or gene carriers, photoactive, sensors and Li-ion batteries. This feature article reviewed the development of the preparation of hollow sphere and 1D structural materials using the sol-gel method. The effects of calcination temperature, soaking time, pH value, surfactant, etc., on the preparation of hollow sphere and 1D structural materials were summarized, and their formation mechanisms were generalized. Finally, possible future research directions of the sol-gel technique were outlined.

  10. Synthesis of Hollow Sphere and 1D Structural Materials by Sol-Gel Process

    PubMed Central

    Li, Fa-Liang; Zhang, Hai-Jun

    2017-01-01

    The sol-gel method is a simple and facile wet chemical process for fabricating advanced materials with high homogeneity, high purity, and excellent chemical reactivity at a relatively low temperature. By adjusting the processing parameters, the sol-gel technique can be used to prepare hollow sphere and 1D structural materials that exhibit a wide application in the fields of catalyst, drug or gene carriers, photoactive, sensors and Li-ion batteries. This feature article reviewed the development of the preparation of hollow sphere and 1D structural materials using the sol-gel method. The effects of calcination temperature, soaking time, pH value, surfactant, etc., on the preparation of hollow sphere and 1D structural materials were summarized, and their formation mechanisms were generalized. Finally, possible future research directions of the sol-gel technique were outlined. PMID:28841188

  11. A comparative study of the novel spectrophotometric methods versus conventional ones for the simultaneous determination of Esomeprazole magnesium trihydrate and Naproxen in their binary mixture.

    PubMed

    Lotfy, Hayam M; Amer, Sawsan M; Zaazaa, Hala E; Mostafa, Noha S

    2015-01-01

    Two novel simple, specific, accurate and precise spectrophotometric methods manipulating ratio spectra are developed and validated for simultaneous determination of Esomeprazole magnesium trihydrate (ESO) and Naproxen (NAP) namely; absorbance subtraction and ratio difference. The results were compared to that of the conventional spectrophotometric methods namely; dual wavelength and isoabsorptive point coupled with first derivative of ratio spectra and derivative ratio. The suggested methods were validated in compliance with the ICH guidelines and were successfully applied for determination of ESO and NAP in their laboratory prepared mixtures and pharmaceutical preparation. No preliminary separation steps are required for the proposed spectrophotometeric procedures. The statistical comparison showed that there is no significant difference between the proposed methods and the reported method with respect to both accuracy and precision. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Comparative study between derivative spectrophotometry and multivariate calibration as analytical tools applied for the simultaneous quantitation of Amlodipine, Valsartan and Hydrochlorothiazide.

    PubMed

    Darwish, Hany W; Hassan, Said A; Salem, Maissa Y; El-Zeany, Badr A

    2013-09-01

    Four simple, accurate and specific methods were developed and validated for the simultaneous estimation of Amlodipine (AML), Valsartan (VAL) and Hydrochlorothiazide (HCT) in commercial tablets. The derivative spectrophotometric methods include Derivative Ratio Zero Crossing (DRZC) and Double Divisor Ratio Spectra-Derivative Spectrophotometry (DDRS-DS) methods, while the multivariate calibrations used are Principal Component Regression (PCR) and Partial Least Squares (PLSs). The proposed methods were applied successfully in the determination of the drugs in laboratory-prepared mixtures and in commercial pharmaceutical preparations. The validity of the proposed methods was assessed using the standard addition technique. The linearity of the proposed methods is investigated in the range of 2-32, 4-44 and 2-20 μg/mL for AML, VAL and HCT, respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. New method for the rapid extraction of natural products: efficient isolation of shikimic acid from star anise.

    PubMed

    Just, Jeremy; Deans, Bianca J; Olivier, Wesley J; Paull, Brett; Bissember, Alex C; Smith, Jason A

    2015-05-15

    A new, practical, rapid, and high-yielding process for the pressurized hot water extraction (PHWE) of multigram quantities of shikimic acid from star anise (Illicium verum) using an unmodified household espresso machine has been developed. This operationally simple and inexpensive method enables the efficient and straightforward isolation of shikimic acid and the facile preparation of a range of its synthetic derivatives.

  14. Application of PLE for the determination of essential oil components from Thymus vulgaris L.

    PubMed

    Dawidowicz, Andrzej L; Rado, Ewelina; Wianowska, Dorota; Mardarowicz, Marek; Gawdzik, Jan

    2008-08-15

    Essential plants, due to their long presence in human history, their status in culinary arts, their use in medicine and perfume manufacture, belong to frequently examined stock materials in scientific and industrial laboratories. Because of a large number of freshly cut, dried or frozen plant samples requiring the determination of essential oil amount and composition, a fast, safe, simple, efficient and highly automatic sample preparation method is needed. Five sample preparation methods (steam distillation, extraction in the Soxhlet apparatus, supercritical fluid extraction, solid phase microextraction and pressurized liquid extraction) used for the isolation of aroma-active components from Thymus vulgaris L. are compared in the paper. The methods are mainly discussed with regard to the recovery of components which typically exist in essential oil isolated by steam distillation. According to the obtained data, PLE is the most efficient sample preparation method in determining the essential oil from the thyme herb. Although co-extraction of non-volatile ingredients is the main drawback of this method, it is characterized by the highest yield of essential oil components and the shortest extraction time required. Moreover, the relative peak amounts of essential components revealed by PLE are comparable with those obtained by steam distillation, which is recognized as standard sample preparation method for the analysis of essential oils in aromatic plants.

  15. Fast quantification of endogenous carbohydrates in plasma using hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry.

    PubMed

    Zhu, Bangjie; Liu, Feng; Li, Xituo; Wang, Yan; Gu, Xue; Dai, Jieyu; Wang, Guiming; Cheng, Yu; Yan, Chao

    2015-01-01

    Endogenous carbohydrates in biosamples are frequently highlighted as the most differential metabolites in many metabolomics studies. A simple, fast, simultaneous quantitative method for 16 endogenous carbohydrates in plasma has been developed using hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry. In order to quantify 16 endogenous carbohydrates in plasma, various conditions, including columns, chromatographic conditions, mass spectrometry conditions, and plasma preparation methods, were investigated. Different conditions in this quantified analysis were performed and optimized. The reproducibility, precision, recovery, matrix effect, and stability of the method were verified. The results indicated that a methanol/acetonitrile (50:50, v/v) mixture could effectively and reproducibly precipitate rat plasma proteins. Cold organic solvents coupled with vortex for 1 min and incubated at -20°C for 20 min were the most optimal conditions for protein precipitation and extraction. The results, according to the linearity, recovery, precision, matrix effect, and stability, showed that the method was satisfactory in the quantification of endogenous carbohydrates in rat plasma. The quantified analysis of endogenous carbohydrates in rat plasma performed excellently in terms of sensitivity, high throughput, and simple sample preparation, which met the requirement of quantification in specific expanded metabolomic studies after the global metabolic profiling research. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Synthesis and electrochemical performance of Ti3C2Tx with hydrothermal process

    NASA Astrophysics Data System (ADS)

    Wang, Libo; Zhang, Heng; Wang, Bo; Shen, Changjie; Zhang, Chuanxiang; Hu, Qianku; Zhou, Aiguo; Liu, Baozhong

    2016-09-01

    In this study, a simple hydrothermal method has been developed to prepare Ti3C2Tx from Ti3AlC2 as a high-performance electrode material for supercapacitors. This method is environmentally friendly and has a low level of danger. The morphology and structure of the Ti3C2Tx can be controlled by hydrothermal reaction time, temperature and NH4F amounts. The prepared Ti3C2Tx was characterized by X-ray diffraction, field emission scanning electron microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy and Brunauer-Emmet-Teller. The results show that the prepared Ti3C2Tx is terminated by O, OH, and F groups. The electrochemical properties of the Ti3C2Tx sample exhibit specific capacitance up to 141 Fcm-3 in 3 M KOH aqueous electrolyte, and even after 1000 cycles, no significant degradation of the volumetric capacitance was observed. These results indicate that the Ti3C2Tx material prepared by this hydrothermal method can be used in high performance supercapacitors.

  17. A simple and novel method for RNA-seq library preparation of single cell cDNA analysis by hyperactive Tn5 transposase.

    PubMed

    Brouilette, Scott; Kuersten, Scott; Mein, Charles; Bozek, Monika; Terry, Anna; Dias, Kerith-Rae; Bhaw-Rosun, Leena; Shintani, Yasunori; Coppen, Steven; Ikebe, Chiho; Sawhney, Vinit; Campbell, Niall; Kaneko, Masahiro; Tano, Nobuko; Ishida, Hidekazu; Suzuki, Ken; Yashiro, Kenta

    2012-10-01

    Deep sequencing of single cell-derived cDNAs offers novel insights into oncogenesis and embryogenesis. However, traditional library preparation for RNA-seq analysis requires multiple steps with consequent sample loss and stochastic variation at each step significantly affecting output. Thus, a simpler and better protocol is desirable. The recently developed hyperactive Tn5-mediated library preparation, which brings high quality libraries, is likely one of the solutions. Here, we tested the applicability of hyperactive Tn5-mediated library preparation to deep sequencing of single cell cDNA, optimized the protocol, and compared it with the conventional method based on sonication. This new technique does not require any expensive or special equipment, which secures wider availability. A library was constructed from only 100 ng of cDNA, which enables the saving of precious specimens. Only a few steps of robust enzymatic reaction resulted in saved time, enabling more specimens to be prepared at once, and with a more reproducible size distribution among the different specimens. The obtained RNA-seq results were comparable to the conventional method. Thus, this Tn5-mediated preparation is applicable for anyone who aims to carry out deep sequencing for single cell cDNAs. Copyright © 2012 Wiley Periodicals, Inc.

  18. Miniaturized Sample Preparation and Rapid Detection of Arsenite in Contaminated Soil Using a Smartphone.

    PubMed

    Siddiqui, Mohd Farhan; Kim, Soocheol; Jeon, Hyoil; Kim, Taeho; Joo, Chulmin; Park, Seungkyung

    2018-03-04

    Conventional methods for analyzing heavy metal contamination in soil and water generally require laboratory equipped instruments, complex procedures, skilled personnel and a significant amount of time. With the advancement in computing and multitasking performances, smartphone-based sensors potentially allow the transition of the laboratory-based analytical processes to field applicable, simple methods. In the present work, we demonstrate the novel miniaturized setup for simultaneous sample preparation and smartphone-based optical sensing of arsenic As(III) in the contaminated soil. Colorimetric detection protocol utilizing aptamers, gold nanoparticles and NaCl have been optimized and tested on the PDMS-chip to obtain the high sensitivity with the limit of detection of 0.71 ppm (in the sample) and a correlation coefficient of 0.98. The performance of the device is further demonstrated through the comparative analysis of arsenic-spiked soil samples with standard laboratory method, and a good agreement with a correlation coefficient of 0.9917 and the average difference of 0.37 ppm, are experimentally achieved. With the android application on the device to run the experiment, the whole process from sample preparation to detection is completed within 3 hours without the necessity of skilled personnel. The approximate cost of setup is estimated around 1 USD, weight 55 g. Therefore, the presented method offers the simple, rapid, portable and cost-effective means for onsite sensing of arsenic in soil. Combined with the geometric information inside the smartphones, the system will allow the monitoring of the contamination status of soils in a nation-wide manner.

  19. Self-Sacrificial Salt Templating: Simple Auxiliary Control over the Nanoporous Structure of Porous Carbon Monoliths Prepared through the Solvothermal Route

    PubMed Central

    Feng, Junzong; Jiang, Yonggang; Liu, Ping; Zhang, Qiuhua; Wei, Ronghui; Chen, Xiang; Feng, Jian

    2018-01-01

    The conventional sol-gel method for preparing porous carbons is tedious and high-cost to prepare porous carbons and the control over the nanoporous architecture by solvents and carbonization is restricted. A simple and novel self-sacrificial salt templating method was first presented to adjust the microporous structure of porous carbon monoliths synthesized via the solvothermal method. Apart from good monolithic appearance, the solvothermal route allowed for ambient drying because it made sure that the polymerization reaction was completed quickly and thoroughly. The intact and crack-free porous carbon monoliths were investigated by scanning electron microscopy (SEM), thermogravimetric differential scanning calorimetry (TG-DSC), Fourier transform infrared (FT-IR), energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and nitrogen sorption measurements. It was proven that the self-sacrificial salts NH4SCN had been removed during pyrolyzing and so, porous carbon monoliths could be directly obtained after carbonization without the need of washing removal of salts. Most importantly, the microporous specific surface area of the resultant porous carbon monoliths was dramatically increased up to 770 m2/g and the Brunauer–Emmett–Teller (BET) specific surface area was up to 1131 m2/g. That was because the salts NH4SCN as self-sacrificial templating helped to form more around 0.6 nm, 0.72 nm and 1.1 nm micropores. The self-sacrificial salt templating is also a suitable and feasible method for controlling the nanoporous structure of other porous materials. PMID:29671818

  20. Simple and Fast Sample Preparation Followed by Gas Chromatography-Tandem Mass Spectrometry (GC-MS/MS) for the Analysis of 2- and 4-Methylimidazole in Cola and Dark Beer.

    PubMed

    Choi, Sol Ji; Jung, Mun Yhung

    2017-04-01

    We have developed a simple and fast sample preparation technique in combination with a gas chromatography-tandem mass spectrometry (GC-MS/MS) for the quantification of 2-methylimidazole (2-MeI) and 4-methylimidazole (4-MeI) in colas and dark beers. Conventional sample preparation technique for GC-MS requires laborious and time-consuming steps consisting of sample concentration, pH adjustment, ion pair extraction, centrifugation, back-extraction, centrifugation, derivatization, and extraction. Our sample preparation technique consists of only 2 steps (in situ derivation and extraction) which requires less than 3 min. This method provided high linearity, low limit of detection and limit of quantification, high recovery, and high intra- and interday repeatability. It was found that internal standard method with diluted stable isotope (4-MeI-d 6 ) and 2-ethylimidazole (2-EI) could not correctly compensate the matrix effects. Thus, standard addition technique was used for the quantification of 2- and 4-MeI. The established method was successfully applied to colas and dark beers for the determination of 2-MeI and 4-MeI. The 4-MeI contents in colas and dark beers ranged from 8 to 319 μg/L and from trace to 417 μg/L, respectively. Small quantity (0 to 8 μg/L) of 2-MeI was found only in dark beers. The contents of 4-MeI (22 μg/L) in colas obtained from fast food restaurants were significantly lower than those (177 μg/L) in canned or bottled colas. © 2017 Institute of Food Technologists®.

  1. Robust Polypropylene Fabrics Super-Repelling Various Liquids: A Simple, Rapid and Scalable Fabrication Method by Solvent Swelling.

    PubMed

    Zhu, Tang; Cai, Chao; Duan, Chunting; Zhai, Shuai; Liang, Songmiao; Jin, Yan; Zhao, Ning; Xu, Jian

    2015-07-01

    A simple, rapid (10 s) and scalable method to fabricate superhydrophobic polypropylene (PP) fabrics is developed by swelling the fabrics in cyclohexane/heptane mixture at 80 °C. The recrystallization of the swollen macromolecules on the fiber surface contributes to the formation of submicron protuberances, which increase the surface roughness dramatically and result in superhydrophobic behavior. The superhydrophobic PP fabrics possess excellent repellency to blood, urine, milk, coffee, and other common liquids, and show good durability and robustness, such as remarkable resistances to water penetration, abrasion, acidic/alkaline solution, and boiling water. The excellent comprehensive performance of the superhydrophobic PP fabrics indicates their potential applications as oil/water separation materials, protective garments, diaper pads, or other medical and health supplies. This simple, fast and low cost method operating at a relatively low temperature is superior to other reported techniques for fabricating superhydrophobic PP materials as far as large scale manufacturing is considered. Moreover, the proposed method is applicable for preparing superhydrophobic PP films and sheets as well.

  2. A validated spectrofluorimetric method for the determination of citalopram in bulk and pharmaceutical preparations based on the measurement of the silver nanoparticles-enhanced fluorescence of citalopram/terbium complexes.

    PubMed

    Khan, Muhammad Naeem; Shah, Jasmin; Jan, Muhammad Rasul; Lee, Sang Hak

    2013-01-01

    A simple, sensitive, and accurate spectrofluorimetric method was developed for the determination of citalopram in bulk and pharmaceutical preparations. The method is based on the enhancement of the weak fluorescence signal (FL) of the Tb (III)-citalopram system in the presence of silver nanoparticles. Fluorescence intensities were measured at 555 nm after excitation at 281 nm. Prepared silver nanoparticles (AgNPs) were characterized by UV-Visible spectra and transmission electron microscopy (TEM). Various factors affecting the formation of citalopram-Tb (III)-AgNPs complexes were studied and optimized. The fluorescence intensity versus concentration plot was linear over the range 0.02-14 μg mL(-1), with an excellent correlation coefficient of 0.9978. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 7.15 × 10(-6) μg mL(-1) and 2.38 × 10(-5) μg mL(-1) respectively. The proposed method was found to have good reproducibility with a relative standard deviation of 3.66% (n = 6). The interference effects of common excipients found in pharmaceutical preparations were studied. The developed method was validated statistically by performing recoveries studies and successfully applied for the assay of citalopram in bulk powder and pharmaceutical preparations. Percent recoveries were found to range from 98.98% to 100.97% for bulk powder and from 96.57% to 101.77% for pharmaceutical preparations.

  3. Preparation of regenerable granular carbon nanotubes by a simple heating-filtration method for efficient removal of typical pharmaceuticals

    NASA Astrophysics Data System (ADS)

    Shan, Danna; Deng, Shubo; Zhao, Tianning; Yu, Gang; Winglee, Judith; Wiesner, Mark R.

    2017-04-01

    A simple and convenient method was used to prepare novel granular carbon nanotubes (CNTs) for enhanced adsorption of pharmaceuticals. By heating CNTs powder at 450 degree centigrade in air, followed by filtration, the obtained granular adsorbent exhibited high surface area and pore volume since the heating process produced some oxygen-containing functional groups on CNT surface, making CNTs more dispersible in the formation of granular cake. The porous granular CNTs not only had more available surfaces for adsorption but also were more easily separated from solution than pristine CNTs (p-CNTs) powder. This adsorbent exhibited relatively fast adsorption for carbamazepine (CBZ), tetracycline (TC) and diclofe- nac sodium (DS), and the maximum adsorption capacity on the granular CNTs was 369.5 μmol/g for CBZ, 284.2 μmol/g for TC and 203.1 μmol/g for DS according to the Langmuir fitting, increasing by 42.4%, 37.8% and 38.0% in comparison with the pristine CNTs powder. Moreover, the spent granular CNTs were successfully regenerated at 400 degree centigrade in air without decreasing the adsorption capacity in five regeneration cycles. The adsorbed CBZ and DS were completely degraded, while the adsorbed TC was partially oxidized and the residual was favorable for the subsequent adsorption. This research develops an easy method to prepare and regenerate granular CNT adsorbent for the enhanced removal of organic pollutants from water or wastewater.

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

    PubMed

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

    2015-01-01

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

  5. Development and Validation of Spectrofluorimetric Method for Determination of Biotin in Bulk and Pharmaceutical Preparations via its Oxidation with Cerium (IV)

    PubMed Central

    Walash, M. I.; Rizk, M.; Sheribah, Z. A.; Salim, M. M.

    2010-01-01

    A simple and sensitive spectrofluorimetric method was developed for the determination of biotin in pure form and in pharmaceutical preparations. The proposed method is based on the oxidation of the drug with cerium (IV) ammonium sulfate in acidic medium. The fluorescence of the produced Cerium (III) was measured at 365 nm after excitation at 255 nm. The different experimental parameters affecting the development and stability of the reaction were carefully studied and optimized. The method is applicable over the concentration range of 30-120 ng/mL with correlation coefficient of 0.9998. The detection limit (LOD) of biotin was 2.41 ng/mL while quantitation limit (LOQ) was 7.29 ng/mL. The proposed procedure was successfully applied for the determination of biotin in pharmaceutical preparations with mean recoveries of 99.55 ± 0.83 and 101.67 ± 1.53 for biotin ampoules and capsules, respectively. The results obtained were in good agreement with those obtained using the official method. PMID:23675202

  6. Direct amination of γ-halo-β-ketoesters with anilines

    PubMed Central

    Zhang, Yinan; Silverman, Richard B.

    2012-01-01

    The direct amination of α-haloacetoacetates with anilines is described. Compared to existing methods, this simple protocol provides an attractive strategy to prepare diverse γ-anilino-β-ketoesters in one step. Good to excellent yields of the amination products were obtained under robust conditions, providing versatile and useful scaffolds. PMID:22390154

  7. Preparation of 152Gd targets from a small quantity of gadolinium oxide in a pyrochemical reaction

    NASA Astrophysics Data System (ADS)

    Lipski, A. R.

    1995-02-01

    A simple method utilizing small amounts (< 5 mg) of isotopically enriched material for the production of gadolinium targets is discussed. An electrostatically focused e-gun is used in the procedure in which 152Gd 2O 3 powder undergoes reduction-distillation and deposition onto an Fe foil.

  8. Preparation of isotopic molybdenum foils utilizing small quantities of material

    NASA Astrophysics Data System (ADS)

    Lipski, A. R.; Lee, L. L.; Liang, J. F.; Mahon, J. C.

    1993-09-01

    A simple method utilizing a small amount of isotopic material for production of molybdenum foils is discussed. An e-gun is used in the procedure. The Mo powder undergoes reduction-sintering and melting-solidifying steps leading to the creation of a metallic droplet suitable for further cold rolling or vacuum deposition.

  9. Key Mites Commonly Associated With the Southern Pine Beetle

    Treesearch

    D.N. Kinn

    1976-01-01

    This paper outlines a method of preparing mites for microscopic examination and contains a simple key to the 15 species of mites commonly associated with the southern pine bark beetle. Research workers wanting to identify these mites and others curious about them, but untrained in acarology, should find little difficulty in making identifications.

  10. GREENER SYNTHESIS OF NANOMETALS AND NANOCOMPOSITES AND THEIR APPLICATION IN ORGANIC SYNTHESES

    EPA Science Inventory

    A brief account of a greener preparation of nanoparticles which reduces or eliminates the use and generation of hazardous substances is described. The use of vitamins B1 and B2, which can function both as reducing and capping agents, provides a simple, one-pot, greener method to ...

  11. Hollow microspheres with a tungsten carbide kernel for PEMFC application.

    PubMed

    d'Arbigny, Julien Bernard; Taillades, Gilles; Marrony, Mathieu; Jones, Deborah J; Rozière, Jacques

    2011-07-28

    Tungsten carbide microspheres comprising an outer shell and a compact kernel prepared by a simple hydrothermal method exhibit very high surface area promoting a high dispersion of platinum nanoparticles, and an exceptionally high electrochemically active surface area (EAS) stability compared to the usual Pt/C electrocatalysts used for PEMFC application.

  12. Ancient Pyramids Help Students Learn Math Concepts

    ERIC Educational Resources Information Center

    Smith, Courtney D.; Stump, Amanda M.; Lazaros, Edward J.

    2010-01-01

    This article presents an activity that allows students to use mathematics and critical-thinking skills to emulate processes used by the ancient Egyptians to prepare the site for the Pyramids of Giza. To accomplish this, they use three different methods. First, they create a square using only simple technological tools that were available to the…

  13. Fabrication of uniformly dispersed Ag nanoparticles loaded TiO{sub 2} nanotube arrays for enhancing photoelectrochemical and photocatalytic performances under visible light irradiation

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

    Yi, Junhui; Zhang, Shengsen; Wang, Hongjuan

    2014-12-15

    Graphical abstract: Uniformly dispersed Ag nanoparticles (NPs) were successfully loaded on both the outer and inner surface of the TiO{sub 2} nanotube arrays (NTs) through a simple polyol method, which exhibited the enhanced photoelectrochemical and photocatalytic performances under visible-light irradiation due to the more effective separation of photo-generated electron–hole pairs and faster interfacial charge transfer. - Highlights: • Highly dispersed Ag nanoparticles (NPs) are successfully prepared by polyol method. • Ag NPs are uniformly loaded on the surface of the TiO{sub 2} nanotube arrays (NTs). • Ag/TiO{sub 2}-NTs exhibit the enhanced photocatalytic activity under visible-light. • The enhanced photocurrent ismore » explained by electrochemical impedance spectroscopy. - Abstract: Uniformly dispersed Ag nanoparticles (NPs) were successfully loaded on both the outer and inner surface of the TiO{sub 2} nanotube arrays (NTs) through a simple polyol method. The as-prepared Ag/TiO{sub 2}-NTs were characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy and UV–vis diffusion reflectance spectroscopy. Photoelectrochemical behaviors were investigated via photocurrent response and electrochemical impedance spectroscopy (EIS). Photocatalytic activity of Ag/TiO{sub 2}-NTs was evaluated by degradation of acid orange II under visible light irradiation. The results showed that photocatalytic efficiency of Ag/TiO{sub 2}-NTs is more than 5 times higher than that of pure TiO{sub 2} NTs. Comparing with the electrochemical deposition method, the photocatalytic activity of Ag/TiO{sub 2}-NTs prepared by polyol method has been obviously increased.« less

  14. Preparation of protein- and cell-resistant surfaces by hyperthermal hydrogen induced cross-linking of poly(ethylene oxide).

    PubMed

    Bonduelle, Colin V; Lau, Woon M; Gillies, Elizabeth R

    2011-05-01

    The functionalization of surfaces with poly(ethylene oxide) (PEO) is an effective means of imparting resistance to the adsorption of proteins and the attachment and growth of cells, properties that are critical for many biomedical applications. In this work, a new hyperthermal hydrogen induced cross-linking (HHIC) method was explored as a simple one-step approach for attaching PEO to surfaces through the selective cleavage of C-H bonds and subsequent cross-linking of the resulting carbon radicals. In order to study the effects of the process on the polymer, PEO-coated silicon wafers were prepared and the effects of different treatment times were investigated. Subsequently, using an optimized treatment time and a modified butyl polymer with increased affinity for PEO, the technique was applied to butyl rubber surfaces. All of the treated surfaces exhibited significantly reduced protein adsorption and cell growth relative to control surfaces and compared favorably with surfaces that were functionalized with PEO using conventional chemical methods. Thus HHIC is a simple and effective means of attaching PEO to non-functional polymer surfaces.

  15. Investigation on structural and optical properties of ZnO film prepared by simple wet chemical method

    NASA Astrophysics Data System (ADS)

    Sholehah, Amalia; Mulyadi, Rendi; Haryono, Didied; Muttakin, Imamul; Rusbana, Tb Bahtiar; Mardiyanto

    2018-04-01

    ZnO thin layer has a broad potential application in electronic and optoelectronic devices. In this study, vertically align ZnO layers were deposited on ITO glass using wet chemistry method. The seed layers were prepared using electrodeposition technique at 3°C. The growing process was carried out using chemical bath deposition at 90°C. To improve the structural properties, two different hydrothermal treatment variations were applied separately. From the experiment, it is shown that the hydrothermal process using N2 gas has given the best result, with average diameter, crystallite size, and band-gap energy of 68.83 nm; 56.37 nm; and 3.16 eV, respectively.

  16. Peregrine: A rapid and unbiased method to produce strand-specific RNA-Seq libraries from small quantities of starting material.

    PubMed

    Langevin, Stanley A; Bent, Zachary W; Solberg, Owen D; Curtis, Deanna J; Lane, Pamela D; Williams, Kelly P; Schoeniger, Joseph S; Sinha, Anupama; Lane, Todd W; Branda, Steven S

    2013-04-01

    Use of second generation sequencing (SGS) technologies for transcriptional profiling (RNA-Seq) has revolutionized transcriptomics, enabling measurement of RNA abundances with unprecedented specificity and sensitivity and the discovery of novel RNA species. Preparation of RNA-Seq libraries requires conversion of the RNA starting material into cDNA flanked by platform-specific adaptor sequences. Each of the published methods and commercial kits currently available for RNA-Seq library preparation suffers from at least one major drawback, including long processing times, large starting material requirements, uneven coverage, loss of strand information and high cost. We report the development of a new RNA-Seq library preparation technique that produces representative, strand-specific RNA-Seq libraries from small amounts of starting material in a fast, simple and cost-effective manner. Additionally, we have developed a new quantitative PCR-based assay for precisely determining the number of PCR cycles to perform for optimal enrichment of the final library, a key step in all SGS library preparation workflows.

  17. Preparation of an exponentially rising optical pulse for efficient excitation of single atoms in free space.

    PubMed

    Dao, Hoang Lan; Aljunid, Syed Abdullah; Maslennikov, Gleb; Kurtsiefer, Christian

    2012-08-01

    We report on a simple method to prepare optical pulses with exponentially rising envelope on the time scale of a few ns. The scheme is based on the exponential transfer function of a fast transistor, which generates an exponentially rising envelope that is transferred first on a radio frequency carrier, and then on a coherent cw laser beam with an electro-optical phase modulator. The temporally shaped sideband is then extracted with an optical resonator and can be used to efficiently excite a single (87)Rb atom.

  18. Preparation and the influencing factors of timozolomide liposomes.

    PubMed

    Kong, Bin; Sun, Yong; Li, Yongjian; Hu, Dejian

    2009-01-01

    To prepare timozolomide liposomes for administration through nasal mucous membrane, we studied the factors of the preparation of the liposomes. The timozolomide liposomes were prepared by the ammonium sulphate gradient method; electroscopy and laser particle analyzer were utilized to determine the conformation, size and distribution of timozolomide liposomes; high performance liquid chromatography (HPLC) was applied to determine the entrapping efficiency of timozolomide liposomes; then we studied the influences of the concentration of ammonium sulphate solution, temperature, and the drug-to-lipid ratio on the entrapping efficiency. The average size of timozolomide liposomes was 185 nm; the entrapping efficiency was 90.3%. The entrapping efficiency was enhanced with the increasing of the concentration of ammonium sulphate solution and the rising of temperature, and decreased with the increasing of the drug-to-lipid ratio. The timozolomide liposomes with high entrapping efficiency, small and even particle sizes could be prepared by the simple and convenient ammonium sulphate gradient method. The primary influencing factors on the entrapping efficiency of timozolomide liposomes were the concentration of ammonium sulphate solution, the temperature, and the drug-to-lipid ratio.

  19. Volatility-dependent 2D IR correlation analysis of traditional Chinese medicine ‘Red Flower Oil’ preparation from different manufacturers

    NASA Astrophysics Data System (ADS)

    Wu, Yan-Wen; Sun, Su-Qin; Zhou, Qun; Tao, Jia-Xun; Noda, Isao

    2008-06-01

    As a traditional Chinese medicine (TCM), 'Red Flower Oil' preparation is widely used as a household remedy in China and Southeast Asia. Usually, the preparation is a mixture of several plant essential oils with different volatile features, such as wintergreen oil, turpentine oil and clove oil. The proportions of these plant essential oils in 'Red Flower Oil' vary from different manufacturers. Thus, it is important to develop a simple and rapid evaluation method for quality assurance of the preparations. Fourier transform infrared (FT-IR) was applied and two-dimensional correlation infrared spectroscopy (2D IR) based on the volatile characteristic of samples was used to enhance the resolution of FT-IR spectra. 2D IR technique could, not only easily provide the composition and their volatile sequences in 'Red flower Oil' preparations, but also rapidly discriminate the subtle differences in products from different manufacturers. Therefore, FT-IR combined with volatility-dependent 2D IR correlation analysis provides a very fast and effective method for the quality control of essential oil mixtures in TCM.

  20. Stability indicating methods for the analysis of cefprozil in the presence of its alkaline induced degradation product

    NASA Astrophysics Data System (ADS)

    Attia, Khalid A. M.; Nassar, Mohammed W. I.; El-Zeiny, Mohamed B.; Serag, Ahmed

    2016-04-01

    Three simple, specific, accurate and precise spectrophotometric methods were developed for the determination of cefprozil (CZ) in the presence of its alkaline induced degradation product (DCZ). The first method was the bivariate method, while the two other multivariate methods were partial least squares (PLS) and spectral residual augmented classical least squares (SRACLS). The multivariate methods were applied with and without variable selection procedure (genetic algorithm GA). These methods were tested by analyzing laboratory prepared mixtures of the above drug with its alkaline induced degradation product and they were applied to its commercial pharmaceutical products.

  1. A comparative study of three pillars system and banking methods in accounting long-term purposes of retiree in Indonesian saving account

    NASA Astrophysics Data System (ADS)

    Hasbullah, E. S.; Suyudi, M.; Halim, N. A.; Sukono; Gustaf, F.; Putra, A. S.

    2018-03-01

    Human productivity is the main capital in economic activity. This main factor leads to the fact that the continuity of human resources in economic sector depends on the limited productivity age. In other word, once the economic agents has reach the limit of the productivity age. Hence they enter the pension state. In this case, the preparation of ‘old-age’ fund become crucial and should be initiated before the pension state to avoid the destitute condition of retiree. Two most simple and familiar methods in preparing the pension fund are The Three Pillars system and banking methods. Here we simulate the both of the methods for the synthetic data of investment program and analyse the result. The result gives the idea that the Three Pillar System has effective prospect in Long-term scheme. However, the banking method is likely adapted to the short-term plan.

  2. Direct synthesis of catalyzed hydride compounds

    DOEpatents

    Gross, Karl J.; Majzoub, Eric

    2004-09-21

    A method is disclosed for directly preparing alkali metal aluminum hydrides such as NaAlH.sub.4 and Na.sub.3 AlH.sub.6 from either the alkali metal or its hydride, and aluminum. The hydride thus prepared is doped with a small portion of a transition metal catalyst compound, such as TiCl.sub.3, TiF.sub.3, or a mixture of these materials, in order to render them reversibly hydridable. The process provides for mechanically mixing the dry reagents under an inert atmosphere followed by charging the mixed materials with high pressure hydrogen while heating the mixture to about 125.degree. C. The method is relatively simple and inexpensive and provides reversible hydride compounds which are free of the usual contamination introduced by prior art wet chemical methods.

  3. Direct synthesis of calcium borohydride

    DOEpatents

    Ronnebro, Ewa Carin Ellinor [Dublin, CA; Majzoub, Eric H [Pleasanton, CA

    2009-10-27

    A method is disclosed for directly preparing an alkaline earth metal borohydride, i.e. Ca(BH.sub.4).sub.2, from the alkaline earth metal hydride and the alkaline earth metal boride. The borohydride thus prepared is doped with a small portion of a metal chloride catalyst compound, such as RuCl.sub.3, TiCl.sub.3, or a mixture of TiCl.sub.3 and palladium metal. The process provides for mechanically mixing the dry reagents under an inert atmosphere followed by charging the mixed materials with high pressure hydrogen at about 70 MPa while heating the mixture to about 400.degree. C. The method is relatively simple and inexpensive and provides reversible hydride compounds which are free of the usual contamination introduced by prior art wet chemical methods.

  4. A simple method to synthesize modified Fe3O4 for the removal of organic pollutants on water surface

    NASA Astrophysics Data System (ADS)

    Zhu, Ling; Li, Chuanhao; Wang, Juan; Zhang, Hui; Zhang, Jian; Shen, Yuhua; Li, Cun; Wang, Cuiping; Xie, Anjian

    2012-06-01

    In this article, a simple, economic and environment-friendly approach is explored to prepare Fe3O4 nanoparticles by using air oxidation at room temperature. Furthermore, the Fe3O4 magnetic nanoparticles (MNPs) have been modified with sodium oleate successfully to form super-hydrophobic surfaces. The alkali source played an important role in controlling the morphologies of Fe3O4 MNPs. Either Fe3O4 MNPs or sodium oleate modified Fe3O4 MNPs possessed good magnetic property, and the as-prepared modified Fe3O4 nanoparticles are both hydrophobic and lipophilic. Therefore, Fe3O4/sodium oleate could be dispersed stable in the oil medium and have been applied in the cleanup engine oil from the water surface. It will open up a potential and broad application in wastewater treatment.

  5. Platelet-rich preparations to improve healing. Part II: platelet activation and enrichment, leukocyte inclusion, and other selection criteria.

    PubMed

    Davis, Vicki L; Abukabda, Alaeddin B; Radio, Nicholas M; Witt-Enderby, Paula A; Clafshenkel, William P; Cairone, J Vito; Rutkowski, James L

    2014-08-01

    Multiple platelet-rich preparations have been reported to improve wound and bone healing, such as platelet-rich plasma (PRP) and platelet rich fibrin (PRF). The different methods employed during their preparation are important, as they influence the quality of the product applied to a wound or surgical site. Besides the general protocol for preparing the platelet-rich product (discussed in Part 1 of this review), multiple choices need to be considered during its preparation. For example, activation of the platelets is required for the release and enmeshment of growth factors, but the method of activation may influence the resulting matrix, growth factor availability, and healing. Additionally, some methods enrich leukocytes as well as platelets, but others are designed to be leukocyte-poor. Leukocytes have many important roles in healing and their inclusion in PRP results in increased platelet concentrations. Platelet and growth factor enrichment reported for the different types of platelet-rich preparations are also compared. Generally, TGF-β1 and PDGF levels were higher in preparations that contain leukocytes compared to leukocyte-poor PRP. However, platelet concentration may be the most reliable criterion for comparing different preparations. These and other criteria are described to help guide dental and medical professionals, in large and small practices, in selecting the best procedures for their patients. The healing benefits of platelet-rich preparations along with the low risk and availability of simple preparation procedures should encourage more clinicians to incorporate platelet-rich products in their practice to accelerate healing, reduce adverse events, and improve patient outcomes.

  6. Fluorine-free preparation of titanium carbide MXene quantum dots with high near-infrared photothermal performances for cancer therapy.

    PubMed

    Yu, Xinghua; Cai, Xingke; Cui, Haodong; Lee, Seung-Wuk; Yu, Xue-Feng; Liu, Bilu

    2017-11-23

    Titanium carbide MXene quantum dots (QDs) were synthesized using an effective fluorine-free method as a biocompatible and highly efficient nanoagent for photothermal therapy (PTT) applications. In contrast to the traditional, hazardous and time-consuming process of HF pretreatment, our fluorine-free method is safe and simple. More importantly, abundant Al oxoanions were found to be modified on the MXene QD surface by the fluorine-free method, which endowed the QDs with strong and broad absorption in the NIR region. As a result, the as-prepared MXene QDs exhibited an extinction coefficient as large as 52.8 Lg -1 cm -1 at 808 nm and a photothermal conversion efficiency as high as 52.2%. Both the values are among the best reported so far. The as-prepared MXene QDs achieved simultaneous photoacoustic (PA) imaging and the remarkable PTT effect of tumors. Moreover, MXene QDs showed great biocompatibility without causing noticeable toxicity in vitro and in vivo, indicating their high potential for clinical applications.

  7. Mechanochemical synthesis and intercalation of Ca(II)Fe(III)-layered double hydroxides

    NASA Astrophysics Data System (ADS)

    Ferencz, Zs.; Szabados, M.; Varga, G.; Csendes, Z.; Kukovecz, Á.; Kónya, Z.; Carlson, S.; Sipos, P.; Pálinkó, I.

    2016-01-01

    A mechanochemical method (grinding the components without added water - dry grinding, followed by further grinding in the presence of minute amount of water or NaOH solution - wet grinding) was used in this work for the preparation and intercalation of CaFe-layered double hydroxides (LDHs). Both the pristine LDHs and the amino acid anion (cystinate and tyrosinate) intercalated varieties were prepared by the two-step grinding procedure in a mixer mill. By systematically changing the conditions of the preparation method, a set of parameters could be determined, which led to the formation of close to phase-pure LDH. The optimisation procedure was also applied for the intercalation processes of the amino acid anions. The resulting materials were structurally characterised by a range of methods (X-ray diffractometry, scanning electron microscopy, energy dispersive analysis, thermogravimetry, X-ray absorption and infra-red spectroscopies). It was proven that this simple mechanochemical procedure was able to produce complex organic-inorganic nanocomposites: LDHs intercalated with amino acid anions.

  8. Determination of traces of cobalt in soils: A field method

    USGS Publications Warehouse

    Almond, H.

    1953-01-01

    The growing use of geochemical prospecting methods in the search for ore deposits has led to the development of a field method for the determination of cobalt in soils. The determination is based on the fact that cobalt reacts with 2-nitroso-1-naphthol to yield a pink compound that is soluble in carbon tetrachloride. The carbon tetrachloride extract is shaken with dilute cyanide to complex interfering elements and to remove excess reagent. The cobalt content is estimated by comparing the pink color in the carbon tetrachloride with a standard series prepared from standard solutions. The cobalt 2-nitroso-1-naphtholate system in carbon tetrachloride follows Beer's law. As little as 1 p.p.m. can be determined in a 0.1-gram sample. The method is simple and fast and requires only simple equipment. More than 40 samples can be analyzed per man-day with an accuracy within 30% or better.

  9. Time-dependent preparation of gelatin-stabilized silver nanoparticles by pulsed Nd:YAG laser

    NASA Astrophysics Data System (ADS)

    Darroudi, Majid; Ahmad, M. B.; Zamiri, Reza; Abdullah, A. H.; Ibrahim, N. A.; Sadrolhosseini, A. R.

    2011-03-01

    Colloidal silver nanoparticles (Ag-NPs) were successfully prepared using a nanosecond pulsed Nd:YAG laser, λ = 1064 nm, with laser fluence of approximately about 360 mJ/pulse, in an aqueous gelatin solution. In this work, gelatin was used as a stabilizer, and the size and optical absorption properties of samples were studied as a function of the laser ablation times. The results from the UV-vis spectroscopy demonstrated that the mean diameter of Ag-NPs decrease as the laser ablation time increases. The Ag-NPs have mean diameters ranging from approximately 10 nm to 16 nm. Compared with other preparation methods, this work is clean, rapid, and simple to use.

  10. Straightforward synthesis of non-natural L-chalcogen and L-diselenide N-Boc-protected-γ-amino acid derivatives.

    PubMed

    Kawasoko, Cristiane Y; Foletto, Patricia; Rodrigues, Oscar E D; Dornelles, Luciano; Schwab, Ricardo S; Braga, Antonio L

    2013-08-21

    The synthesis of new chiral seleno-, telluro-, and thio-N-Boc-γ-amino acids is described herein. These new compounds were prepared through a simple and short synthetic route, from the inexpensive and commercially-available amino acid L-glutamic acid. The products, with a highly modular character, were obtained in good to excellent yields, via hydrolysis of chalcogen pyroglutamic derivatives with overall retention of the L-glutamic acid stereochemistry. Also, an L-diselenide-N-Boc-γ-amino acid was prepared in good yield. This new synthetic route represents an efficient method for preparing new L-chalcogen- and L-diselenide-γ-amino acids with biological potential.

  11. In-house preparation of iodine -131 metaiodo benzyl guanidine for scintigraphy of neuroendocrine tumors. Fourteen years experience in South India.

    PubMed

    Oommen, Regi; Shanthly, Nylla; Subramani, Narasimhan; Devadhas, Devakumar; Hephzibah, Julie; Theodore, Bernice; Srinivasan, Jayashankar

    2007-01-01

    Iodine-131 metaiodobenzyl guanidine ((131)I-MIBG) is routinely used for imaging and treatment of neuroendocrine tumors (NET). As the commercially available radiopharmaceutical was very expensive, we developed an in-house method of labeling MIBG with (131)I in 1993. A total of 247 batches of (131)I-MIBG were prepared and used in our hospital between April 1993 and September 2006. We report our experience over these 14 years of preparation of this tracer in our hospital radiopharmacy, for the scintigraphy of NET. The technique of preparation is simple and the labeled product was found to be of acceptable quality. With the routine availability and cost effectiveness, the utilization of this radiopharmaceutical for scintigraphy increased remarkably in our institution.

  12. Autonomously Self-Adhesive Hydrogels as Building Blocks for Additive Manufacturing.

    PubMed

    Deng, Xudong; Attalla, Rana; Sadowski, Lukas P; Chen, Mengsu; Majcher, Michael J; Urosev, Ivan; Yin, Da-Chuan; Selvaganapathy, P Ravi; Filipe, Carlos D M; Hoare, Todd

    2018-01-08

    We report a simple method of preparing autonomous and rapid self-adhesive hydrogels and their use as building blocks for additive manufacturing of functional tissue scaffolds. Dynamic cross-linking between 2-aminophenylboronic acid-functionalized hyaluronic acid and poly(vinyl alcohol) yields hydrogels that recover their mechanical integrity within 1 min after cutting or shear under both neutral and acidic pH conditions. Incorporation of this hydrogel in an interpenetrating calcium-alginate network results in an interfacially stiffer but still rapidly self-adhesive hydrogel that can be assembled into hollow perfusion channels by simple contact additive manufacturing within minutes. Such channels withstand fluid perfusion while retaining their dimensions and support endothelial cell growth and proliferation, providing a simple and modular route to produce customized cell scaffolds.

  13. Simple and inexpensive microfluidic devices for the generation of monodisperse multiple emulsions

    NASA Astrophysics Data System (ADS)

    Li, Er Qiang; Zhang, Jia Ming; Thoroddsen, Sigurdur T.

    2014-01-01

    Droplet-based microfluidic devices have become a preferred versatile platform for various fields in physics, chemistry and biology. Polydimethylsiloxane soft lithography, the mainstay for fabricating microfluidic devices, usually requires the usage of expensive apparatus and a complex manufacturing procedure. Here, we report the design and fabrication of simple and inexpensive microfluidic devices based on microscope glass slides and pulled glass capillaries, for generating monodisperse multiple emulsions. The advantages of our method lie in a simple manufacturing procedure, inexpensive processing equipment and flexibility in the surface modification of the designed microfluidic devices. Different types of devices have been designed and tested and the experimental results demonstrated their robustness for preparing monodisperse single, double, triple and multi-component emulsions.

  14. Comparative artificial neural network and partial least squares models for analysis of Metronidazole, Diloxanide, Spiramycin and Cliquinol in pharmaceutical preparations.

    PubMed

    Elkhoudary, Mahmoud M; Abdel Salam, Randa A; Hadad, Ghada M

    2014-09-15

    Metronidazole (MNZ) is a widely used antibacterial and amoebicide drug. Therefore, it is important to develop a rapid and specific analytical method for the determination of MNZ in mixture with Spiramycin (SPY), Diloxanide (DIX) and Cliquinol (CLQ) in pharmaceutical preparations. This work describes simple, sensitive and reliable six multivariate calibration methods, namely linear and nonlinear artificial neural networks preceded by genetic algorithm (GA-ANN) and principle component analysis (PCA-ANN) as well as partial least squares (PLS) either alone or preceded by genetic algorithm (GA-PLS) for UV spectrophotometric determination of MNZ, SPY, DIX and CLQ in pharmaceutical preparations with no interference of pharmaceutical additives. The results manifest the problem of nonlinearity and how models like ANN can handle it. Analytical performance of these methods was statistically validated with respect to linearity, accuracy, precision and specificity. The developed methods indicate the ability of the previously mentioned multivariate calibration models to handle and solve UV spectra of the four components' mixtures using easy and widely used UV spectrophotometer. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Spectrofluorimetric determination of tobramycin in human serum and pharmaceutical preparations by derivatization with fluorescamine.

    PubMed

    Tekkeli, Serife Evrim Kepekci; Önal, Armağan; Sağırlı, A Olcay

    2014-02-01

    A simple, sensitive and selective spectrofluorimetric method has been developed for the determination of tobramycin (TOB) in human serum and pharmaceutical preparations. The method is based on the reaction between the primary amino group of TOB and fluorescamine in borate buffer, pH 8.5, to give a highly fluorescent derivative which is measured at 469 nm after excitation at 388 nm. The fluorescence intensity was directly proportional to the concentration over the range 300-1500 ng/mL, with a limit of detection of 65 ng/mL and limit of quantitation of 215 ng/mL. All variables were investigated to optimize the reaction conditions. The method was validated according to International Conference on Harmonization guidelines in terms of specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness. Good recoveries were obtained ranging from 97.4 to 100.64%, indicating that no interference was observed from concomitants usually present in pharmaceutical dosage forms. The method was successfully, applied for the analysis of the drug substance in its pharmaceutical preparations and spiked serum samples. Copyright © 2013 John Wiley & Sons, Ltd.

  16. Kinetic Spectrophotometric Determination of Biotin in Pharmaceutical Preparations

    PubMed Central

    Walash, M. I.; Rizk, M.; Sheribah, Z. A.; Salim, M. M.

    2008-01-01

    A simple accurate kinetic spectrophotometric method was developed for the determination of biotin in pure form and pharmaceutical preparations. The proposed method is based on a catalytic acceleration of biotin on the reaction between sodium azide and tri-iodide in an aqueous solution. Concentration range of 4-16 μg/mL for biotin was determined by measuring the decrease in the absorbance of tri-iodide at 348 nm by a fixed time method. The decrease in absorbance after 14 min from the initiation of the reaction was markedly correlated to the concentration with correlation coefficient of 0.9999. The detection limit (LOD) of biotin was 0.18 μg/mL while quantitation limit (LOQ) was 0.54 μg/mL. The percentage recovery of the spiked samples was 100.08 ± 0.761. The proposed procedure was successfully applied for the determination of biotin in its pharmaceutical preparations with mean recoveries of 101.17 ± 2.05 and 97.87 ± 1.50 for biotin ampoules and capsules, respectively. The results obtained were in good agreement with those obtained using official method. PMID:23675096

  17. Comparative artificial neural network and partial least squares models for analysis of Metronidazole, Diloxanide, Spiramycin and Cliquinol in pharmaceutical preparations

    NASA Astrophysics Data System (ADS)

    Elkhoudary, Mahmoud M.; Abdel Salam, Randa A.; Hadad, Ghada M.

    2014-09-01

    Metronidazole (MNZ) is a widely used antibacterial and amoebicide drug. Therefore, it is important to develop a rapid and specific analytical method for the determination of MNZ in mixture with Spiramycin (SPY), Diloxanide (DIX) and Cliquinol (CLQ) in pharmaceutical preparations. This work describes simple, sensitive and reliable six multivariate calibration methods, namely linear and nonlinear artificial neural networks preceded by genetic algorithm (GA-ANN) and principle component analysis (PCA-ANN) as well as partial least squares (PLS) either alone or preceded by genetic algorithm (GA-PLS) for UV spectrophotometric determination of MNZ, SPY, DIX and CLQ in pharmaceutical preparations with no interference of pharmaceutical additives. The results manifest the problem of nonlinearity and how models like ANN can handle it. Analytical performance of these methods was statistically validated with respect to linearity, accuracy, precision and specificity. The developed methods indicate the ability of the previously mentioned multivariate calibration models to handle and solve UV spectra of the four components’ mixtures using easy and widely used UV spectrophotometer.

  18. An Authentic Research Experience for Undergraduates on a Budget: Using Data from Simple Experiments to Develop Mini-Research Proposals

    ERIC Educational Resources Information Center

    Robertson, Katherine

    2016-01-01

    The benefits of undergraduate research are well documented, and many colleges and universities include a senior research requirement for graduation. In addition, most science curricula attempt to include discoverystyle, laboratory components to prepare students for their research experiences and to expose them to research methods in different…

  19. A Simple, Safe Method for Preparation of Biodiesel

    ERIC Educational Resources Information Center

    Behnia, Mahin S.; Emerson, David W.; Steinberg, Spencer M.; Alwis, Rasika M.; Duenas, Josue A.; Serafino, Jessica O.

    2011-01-01

    An experiment suitable for organic chemistry students is described. Biodiesel, a "green" fuel, consists of methyl or ethyl esters of long-chain fatty acids called FAMES (fatty acid methyl esters) or FAEES (fatty acid ethyl esters). A quick way to make FAMES is a base-catalyzed transesterification of oils or fats derived from plants or from animal…

  20. The Preparation and Use of Specialist Material in Foreign Language Teaching for Industry.

    ERIC Educational Resources Information Center

    Conlin, Christine

    1984-01-01

    Outlines methods by which dialogs are produced in a program which teaches foreign languages to local British industries. Recommends that such dialogs on specialized topics be short and simple. Also discusses how role play and materials such as graphs, charts, forms, and diagrams can be used as language teaching material. (SED)

  1. Determination of free sulfites (SO3-2) in dried fruits processed with sulfur dioxide by ion chromatography through anion exchange column and conductivity detection.

    PubMed

    Liao, Benjamin S; Sram, Jacqueline C; Files, Darin J

    2013-01-01

    A simple and effective anion ion chromatography (IC) method with anion exchange column and conductivity detector has been developed to determine free sulfites (SO3-2) in dried fruits processed with sulfur dioxide. No oxidation agent, such as hydrogen peroxide, is used to convert sulfites to sulfates for IC analysis. In addition, no stabilizing agent, such as formaldehyde, fructose or EDTA, is required during the sample extraction. This method uses aqueous 0.2 N NaOH as the solvent for standard preparation and sample extraction. The sulfites, either prepared from standard sodium sulfite powder or extracted from food samples, are presumed to be unbound SO3-2 in aqueous 0.2 N NaOH (pH > 13), because the bound sulfites in the sample matrix are released at pH > 10. In this study, sulfites in the standard solutions were stable at room temperature (i.e., 15-25 degrees C) for up to 12 days. The lowest standard of the linear calibration curve is set at 1.59 microg/mL SO3-2 (equivalent to 6.36 microg/g sample with no dilution) for analysis of processed dried fruits that would contain high levels (>1000 microg/g) of sulfites. As a consequence, this method typically requires significant dilution of the sample extract. Samples are prepared with a simple procedure of sample compositing, extraction with aqueous 0.2 N NaOH, centrifugation, dilution as needed, and filtration prior to IC. The sulfites in these sample extracts are stable at room temperature for up to 20 h. Using anion IC, the sulfites are eluted under isocratic conditions with 10 mM aqueous sodium carbonate solution as the mobile phase passing through an anion exchange column. The sulfites are easily separated, with an analysis run time of 18 min, regardless of the dried fruit matrix. Recoveries from samples spiked with sodium sulfites were demonstrated to be between 81 and 105% for five different fruit matrixes (apricot, golden grape, white peach, fig, and mango). Overall, this method is simple to perform and effective for the determination of high levels of sulfites in dried fruits.

  2. Taenia solium metacestode preparation in rural areas of sub-Saharan Africa: a source for diagnosis and research on cysticercosis.

    PubMed

    Schmidt, V; Sikasunge, C S; Odongo-Aginya, E; Simukoko, C; Mwanjali, G; Alarakol, S; Ovuga, E; Matuja, W; Kihamia, C; Löscher, T; Winkler, A S; Bretzel, G

    2015-03-01

    Taenia solium metacestodes/cysts obtained from pig carcasses constitute a primary source for diagnostic tools used for the detection of human cysticercosis. Data on T. solium cyst preparation in Africa is still scarce but required to establish independent reference laboratories. The aim of the present study is a) to present the likely yield of T. solium cyst material by the use of two different preparation methods in the field and b) to investigate its suitability for immunodiagnosis of human cysticercosis. In Zambia, Uganda and Tanzania 670 pigs were screened for T. solium infection. Cysts were prepared by 'shaking method' and 'washing method'. Generated crude antigens were applied in a standard western blot assay. 46 out of 670 pigs (6.9%) were found positive for T. solium (Zambia: 12/367, 3.3%; Uganda: 11/217, 5.1%; Tanzania 23/86, 26.7%). Mean values of 77.7 ml whole cysts, 61.8 ml scolices/membranes and 10.9 ml cyst fluid were obtained per pig. Suitability of collected material for the use as crude antigen and molecular diagnostic techniques was demonstrated. This study clearly shows that T. solium cyst preparation in African settings by simple field methods constitutes an effective way to obtain high quality material as source for diagnostic tools and research purposes.

  3. Rapid determination of isoamyl nitrite in pharmaceutical preparations by flow injection analysis with on-line UV irradiation and luminol chemiluminescence detection.

    PubMed

    Kishikawa, Naoya; Kondo, Naoko; Amponsaa-Karikari, Abena; Kodamatani, Hitoshi; Ohyama, Kaname; Nakashima, Kenichiro; Yamazaki, Shigeo; Kuroda, Naotaka

    2014-02-01

    Isoamyl nitrite is used as a therapeutic reagent for cardiac angina and as an antidote for cyanide poisoning, but it is abused because of its euphoric properties. Therefore, a method to determine isoamyl nitrite is required in many fields, including pharmaceutical and forensic studies. In this study, a simple, rapid and sensitive method for the determination of isoamyl nitrite was developed using a flow injection analysis system equipped with a chemiluminescence detector and on-line photoreactor. This method is based on on-line ultraviolet irradiation of isoamyl nitrite and subsequent luminol chemiluminescence detection without the addition of an oxidant. A linear standard curve was obtained up to 1.0 μM of isoamyl nitrite with a detection limit (blank + 3SD) of 0.03 μM. The method was successfully applied to determine isoamyl nitrite content in pharmaceutical preparations. Copyright © 2013 John Wiley & Sons, Ltd.

  4. The generation of myricetin-nicotinamide nanococrystals by top down and bottom up technologies

    NASA Astrophysics Data System (ADS)

    Liu, Mingyu; Hong, Chao; Li, Guowen; Ma, Ping; Xie, Yan

    2016-09-01

    Myricetin-nicotinamide (MYR-NIC) nanococrystal preparation methods were developed and optimized using both top down and bottom up approaches. The grinding (top down) method successfully achieved nanococrystals, but there were some micrometer range particles and aggregation. The key consideration of the grinding technology was to control the milling time to determine a balance between the particle size and distribution. In contrast, a modified bottom up approach based on a solution method in conjunction with sonochemistry resulted in a uniform MYR-NIC nanococrystal that was confirmed by powder x-ray diffraction, scanning electron microscopy, dynamic light scattering, and differential scanning calorimeter, and the particle dissolution rate and amount were significantly greater than that of MYR-NIC cocrystal. Notably, this was a simple method without the addition of any non-solvent. We anticipate our findings will provide some guidance for future nanococrystal preparation as well as its application in both chemical and pharmaceutical area.

  5. Preparation of 3D fibroin/chitosan blend porous scaffold for tissue engineering via a simplified method.

    PubMed

    Ruan, Yuhui; Lin, Hong; Yao, Jinrong; Chen, Zhengrong; Shao, Zhengzhong

    2011-03-10

    In this work, we developed a simple and flexible method to manufacture a 3D porous scaffold based on the blend of regenerated silk fibroin (RSF) and chitosan (CS). No crosslinker or other toxic reagents were used in this method. The pores of resulted 3D scaffolds were connected with each other, and their sizes could be easily controlled by the concentration of the mixed solution. Compared with pure RSF scaffolds, the water absorptivities of these RSF/CS blend scaffolds with significantly enhanced mechanical properties were greatly increased. The results of MTT and RT-PCR tests indicated that the chondrocytes grew very well in these blend RSF/CS porous scaffolds. This suggested that the RSF/CS blend scaffold prepared by this new method could be a promising candidate for applications in tissue engineering. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. High-performance thin-layer chromatography and three-dimensional image analysis for the determination of rutin in pharmaceutical preparations.

    PubMed

    Soponar, Florin; Moţ, Augustin C; Sârbu, Costel

    2010-01-01

    A novel HPTLC method was developed for fast and simple quantitative determination of rutin in pharmaceutical preparations. The proposed method combines the advantages of HPTLC with the comfort and the convenience of digital processing of images. For the separation of rutin, silica gel with attached amino groups was used as the stationary phase and ethyl acetate-formic acid-methanol-water (10 + 0.9 + 1.1 + 1.7, v/v/v/v) as the mobile phase. The chromatographic plate was sprayed with 2-aminoethyldiphenyl borate solution for visual detection of the spots. For the construction of a three-dimensional chromatogram, Melanie 7.0 software was used together with an HP flatbed scanner that allowed capture of the images on chromatographic plates. The calibration curve was linear within the range of 0.95-4.78 microg/spot with an r value of 0.9984. The RSD for six replicates at three concentration levels was less than 3%, while the recovery was between 97.28 and 103.27%. The proposed method was found to be simple, precise, sensitive, and accurate and has been applied for the determination of rutin in two commercial drugs. The results were compared with the results of other techniques that generate bidimensional chromatograms and validated by UV-Vis spectrophotometry.

  7. Simultaneous detection of morphine and codeine in urine samples of heroin addicts using multi-walled carbon nanotubes modified SnO2-Zn2SnO4 nanocomposites paste electrode

    NASA Astrophysics Data System (ADS)

    Taei, M.; Hasanpour, F.; Hajhashemi, V.; Movahedi, M.; Baghlani, H.

    2016-02-01

    The SnO2-Zn2SnO4 nanocomposite was successfully prepared via a simple solid state method. Then, a chemically modified electrode based on incorporating SnO2-Zn2SnO4 into multi-walled carbon nanotube paste matrix (MWCNTs/SnO2-Zn2SnO4/CPE) was prepared for the simultaneous determination of morphine(MO) and codeine (CO). The measurements were carried out by application of differential pulse voltammetry (DPV), cyclic voltammetry, and chronoamperometry. The MWCNTs/SnO2-Zn2SnO4/CPE showed an efficient electrocatalytic activity for the oxidation of MO and CO. The separation of the oxidation peak potential for MO-CO was about 550 mV. The calibration curves obtained for MO and CO were in the ranges of 0.1-310 μmol L-1 and 0.1-600.0 μmol L-1, respectively. The detection limits (S/N = 3) were 0.009 μmol L-1 for both drugs. The method also successfully employed as a selective, simple, and precise method for the determination of MO and CO in pharmaceutical and biological samples.

  8. Rapid prototyping of Fresnel zone plates via direct Ga(+) ion beam lithography for high-resolution X-ray imaging.

    PubMed

    Keskinbora, Kahraman; Grévent, Corinne; Eigenthaler, Ulrike; Weigand, Markus; Schütz, Gisela

    2013-11-26

    A significant challenge to the wide utilization of X-ray microscopy lies in the difficulty in fabricating adequate high-resolution optics. To date, electron beam lithography has been the dominant technique for the fabrication of diffractive focusing optics called Fresnel zone plates (FZP), even though this preparation method is usually very complicated and is composed of many fabrication steps. In this work, we demonstrate an alternative method that allows the direct, simple, and fast fabrication of FZPs using focused Ga(+) beam lithography practically, in a single step. This method enabled us to prepare a high-resolution FZP in less than 13 min. The performance of the FZP was evaluated in a scanning transmission soft X-ray microscope where nanostructures as small as sub-29 nm in width were clearly resolved, with an ultimate cutoff resolution of 24.25 nm, demonstrating the highest first-order resolution for any FZP fabricated by the ion beam lithography technique. This rapid and simple fabrication scheme illustrates the capabilities and the potential of direct ion beam lithography (IBL) and is expected to increase the accessibility of high-resolution optics to a wider community of researchers working on soft X-ray and extreme ultraviolet microscopy using synchrotron radiation and advanced laboratory sources.

  9. Degradation of Tetracycline with BiFeO3 Prepared by a Simple Hydrothermal Method

    PubMed Central

    Xue, Zhehua; Wang, Ting; Chen, Bingdi; Malkoske, Tyler; Yu, Shuili; Tang, Yulin

    2015-01-01

    BiFeO3 particles (BFO) were prepared by a simple hydrothermal method and characterized. BFO was pure, with a wide particle size distribution, and was visible light responsive. Tetracycline was chosen as the model pollutant in this study. The pH value was an important factor influencing the degradation efficiency. The total organic carbon (TOC) measurement was emphasized as a potential standard to evaluate the visible light photocatalytic degradation efficiency. The photo-Fenton process showed much better degradation efficiency and a wider pH adaptive range than photocatalysis or the Fenton process solely. The optimal residual TOC concentrations of the photocatalysis, Fenton and photo-Fenton processes were 81%, 65% and 21%, while the rate constants of the three processes under the same condition where the best residual TOC was acquired were 9.7 × 10−3, 3.2 × 10−2 and 1.5 × 10−1 min−1, respectively. BFO was demonstrated to have excellent stability and reusability. A comparison among different reported advanced oxidation processes removing tetracycline (TC) was also made. Our findings showed that the photo-Fenton process had good potential for antibiotic-containing waste water treatment. It provides a new method to deal with antibiotic pollution. PMID:28793568

  10. A simple method for collecting eggs of taeniid cestodes from fresh, frozen or ethanol-fixed segments.

    PubMed

    Takemoto, Y; Negita, T; Ohnishi, K; Suzuki, M; Ito, A

    1995-04-01

    A simple method was devised for collecting eggs of Taenia taeniaeformis and T. saginata. All gravid segments, either fresh or frozen or 70% ethanol-fixed, were gently scraped using a pestle on a 150 mesh stainless steel sieve. Eggs and tissue debris were washed out all together with mouse tonicity phosphate buffered saline (MTPBS) through the 150 mesh sieve into a glass beaker. Egg suspension with a huge amount of tissue debris in MTPBS was centrifuged 5 min at 3000 r.p.m. (x 1600 g) and the pellet of eggs and tissue debris was resuspended with 1 vol. of MTPBS and 2 vol. of Percoll (Pharmacia) and centrifuged 60 min at 3000 r.p.m. More than 90% of eggs sedimented in the pellet. The supernatant covered with tissue debris was decanted, and the egg pellet was resuspended and centrifuged several times with MTPBS to remove Percoll. It is suggested that this simple method may prove useful for preparation of eggs of biohazardous taeniid cestodes, such as Taenia solium and Echinococcus spp.

  11. Electrochemical properties of Ti3+ doped Ag-Ti nanotube arrays coated with hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Zhang, Hangzhou; Shi, Xiaoguo; Tian, Ang; Wang, Li; Liu, Chuangwei

    2018-04-01

    Ag-Ti nanotube array was prepared by simple anodic oxidation method and uniform hydroxyapatite were electrochemically deposited on the nanotubes, and then characterized by SEM, XRD, XPS and EIS. In order to investigate the influence of Ti3+ on the electrochemical deposition of hydroxyapatite on the nanotubes, the Ag-Ti nanotube array self-doped with Ti3+ was prepared by one step reduction method. The experiment results revealed that the Ti3+ can promote the grow rate of hydroxyapatite coatings on nanotube surface. The hydroxyapatite coated Ag-Ti nanotube arrays with Ti3+ exhibit excellent stability and higher corrosion resistance. Moreover, the compact and dense hydroxyapatite coating can also prevent the Ag atom erosion from the Ag-Ti nanotube.

  12. A procedure for preparing undecalcified and unembedded bone sections for light microscopy.

    PubMed

    Mancini, M; Spoliti, M; Botti, F; Ragazzoni, E; Cocchia, D

    1997-07-01

    We have developed a procedure for light microscopic investigation of undecalcified and unembedded bone sections. Biopsy samples of human metatarsus and femur and rat femur were fixed in aldehydes and sectioned with a cutting machine equipped with a diamond saw blade. Free sections 100-150 microns thick, stained with toluidine blue and von Kossa, did not show artifacts following the cutting, and the spatial relations of mineralized and nonmineralized components remained intact. Compact and trabecular bone, bone marrow and all cell types appeared well preserved and easily recognizable. Our procedure provides a simple and rapid method for preparing bone sections which undergo no chemical treatment other than fixation. This method is a useful alternative to standard histological protocols for studying bone specimens.

  13. Catalytic performance of Mn 3O 4 and Co 3O 4 nanocrystals prepared by sonochemical method in epoxidation of styrene and cyclooctene

    NASA Astrophysics Data System (ADS)

    Askarinejad, Azadeh; Bagherzadeh, Mojtaba; Morsali, Ali

    2010-09-01

    A simple sonochemical method was developed to synthesis uniform sphere-like Co 3O 4 and Mn 3O 4 nanocrystals. Epoxidation of styrene and cyclooctene by anhydrous tert-butyl hydroperoxide over the prepared Co 3O 4 and Mn 3O 4 nanocatalysts was investigated. The results of conversion activity were compared with bulk Co 3O 4 and Mn 3O 4. Under optimized reaction conditions, the nanocatalysts showed a superior catalytic performance as compared to the bulk catalysts. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and BET surface area, were used to characterize and investigate the nanocatalysts.

  14. Continuous preparation of carbon-nanotube-supported platinum catalysts in a flow reactor directly heated by electric current

    PubMed Central

    dos Santos, Antonio Rodolfo; Kunz, Ulrich; Turek, Thomas

    2011-01-01

    Summary In this contribution we present for the first time a continuous process for the production of highly active Pt catalysts supported by carbon nanotubes by use of an electrically heated tubular reactor. The synthesized catalysts show a high degree of dispersion and narrow distributions of cluster sizes. In comparison to catalysts synthesized by the conventional oil-bath method a significantly higher electrocatalytic activity was reached, which can be attributed to the higher metal loading and smaller and more uniformly distributed Pt particles on the carbon support. Our approach introduces a simple, time-saving and cost-efficient method for fuel cell catalyst preparation in a flow reactor which could be used at a large scale. PMID:22043252

  15. Facile fabrication of plate-shaped hydrohausmannite as electrode material for supercapacitors

    NASA Astrophysics Data System (ADS)

    Liang, Jun; Chai, Yao; Li, Deli; Li, Meng; Lu, Jiaxue; Li, Li; Luo, Min

    2017-08-01

    A simple and one-step solvothermal synthesis method has been developed to prepare two-dimensional (2-D) hydrohausmannite ((Mn4-2xMnx)Mn8O16-x(OH)x) nanoplates with radial length of 300 nm and thickness of about 25 nm in a binary ethanediamine/water solvent system. The formation mechanism of hydrohausmannite is suggested. As an anode material for electrochemical capacitors, the plate-shaped hydrohausmannite not only displays a high specific capacity (215 at 0.1 A g-1) and good rate capability, but also shows good stable performance along with 94% specific capacity retained after 3000 cycle tests. The method can be easily controlled and expected to be applicable for the large-scale preparation of the 2-D hydrohausmannite.

  16. [A simple method for the synthesis of phosphatidylcholine with the fatty acid substituted in the 2-position].

    PubMed

    Schulze, G; Jung, K; Kunze, D; Egger, E

    1976-01-01

    The preparation of PC with the 14C-fatty acids palmitic, stearic, oleic and linoleic acid at OH-group in position 2 is described. The starting material is egg yolk lecithin. By the attack of snake venom phospholiphase lyso-PC is produced which is reacylated by the appropriate fatty acid anhydride. In comparison with the methods published up to now this preparation has the advantage of higher yields and greater simplicity. By means of in vivo synthesis it is impossible to get PC species with only one fatty acid in a defined position. Working with radioactive fatty acids the specific radioactivity can be adapted to the requirements. The procedure can be made on a semi-technical scale.

  17. Interim overdentures.

    PubMed

    Fenton, A H

    1976-07-01

    The construction of an interim overdenture using existing removable partial dentures with natural tooth crowns and artificial teeth can be a simple and economical method of providing patients with dentures while tissues heal and teeth are prepared and restored. A more definite prognosis for both the patient and his remaining dentition can be established before the final overdenture is completed. The procedures necessary to provide three types of interim overdentures have been outlined. Patients tolerate this method of changing their dentitions extremely well.

  18. Recent Application of Solid Phase Based Techniques for Extraction and Preconcentration of Cyanotoxins in Environmental Matrices.

    PubMed

    Mashile, Geaneth Pertunia; Nomngongo, Philiswa N

    2017-03-04

    Cyanotoxins are toxic and are found in eutrophic, municipal, and residential water supplies. For this reason, their occurrence in drinking water systems has become a global concern. Therefore, monitoring, control, risk assessment, and prevention of these contaminants in the environmental bodies are important subjects associated with public health. Thus, rapid, sensitive, selective, simple, and accurate analytical methods for the identification and determination of cyanotoxins are required. In this paper, the sampling methodologies and applications of solid phase-based sample preparation methods for the determination of cyanotoxins in environmental matrices are reviewed. The sample preparation techniques mainly include solid phase micro-extraction (SPME), solid phase extraction (SPE), and solid phase adsorption toxin tracking technology (SPATT). In addition, advantages and disadvantages and future prospects of these methods have been discussed.

  19. Control of silk microsphere formation using polyethylene glycol (PEG).

    PubMed

    Wu, Jianbing; Zheng, Zhaozhu; Li, Gang; Kaplan, David L; Wang, Xiaoqin

    2016-07-15

    A one step, rapid method to prepare silk microspheres was developed, with particle size controlled by the addition of polyethylene glycol (PEG). PEG molecular weight (4.0K-20.0KDa) and concentration (20-50wt%), as well as silk concentration (5-20wt%), were key factors that determined particle sizes varying in a range of 1-100μm. Addition of methanol to the PEG-silk combinations increased the content of crystalline β-sheet in the silk microspheres. To track the distribution and degradation of silk microspheres in vivo, 3-mercaptopropionic acid (MPA)-coated CdTe quantum dots (QDs) were physically entrapped in the silk microspheres. QDs tightly bound to the β-sheet domains of silk via hydrophobic interactions, with over 96% of the loaded QDs remaining in the silk microspheres after exhaustive extraction. The fluorescence of QDs-incorporated silk microspheres less stable in cell culture medium than in phosphate buffer solution (PBS) and water. After subcutaneous injection in mice, microspheres prepared from 20% silk (approx. 30μm diameter particles) still fluoresced at 24h, while those prepared from 8% silk (approx. 4μm diameter particles) and free QDs were not detectable, reflecting the QDs quenching and particle size effect on microsphere clearance in vivo. The larger microspheres were more resistant to cell internalization and degradation. Since PEG is an FDA-approved polymer, and silk is FDA approved for some medical devices, the methods developed in the present study will be useful in a variety of biomedical applications where simple, rapid and scalable preparation of silk microspheres is required. The work is of significance to the biomaterial and controlled release society because it provides a new option for fabricating silk microspheres in one simple step of mixing silk and polyethylene glycol (PEG), with the size and properties of microspheres controllable by PEG molecular weight as well as PEG and silk concentrations. Although fabrication of silk microspheres have been reported previously using spray-drying, liposome-templating, polyvinyl alcohol (PVA) emulsification, etc., applications were hindered due to harsh conditions (temperature, solvents, etc.) and complicated procedures used as well as low yield and less controllable particle size (usually <10μm). Since PEG is an FDA-approved polymer, and silk is FDA approved for some medical devices, the methods developed in the present study will be useful in a variety of biomedical applications where simple, rapid and scalable preparation of silk microspheres is required. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

  20. Validated spectrophotometric method for the determination, spectroscopic characterization and thermal structural analysis of duloxetine with 1,2-naphthoquinone-4-sulphonate

    NASA Astrophysics Data System (ADS)

    Ulu, Sevgi Tatar; Elmali, Fikriye Tuncel

    2012-03-01

    A novel, selective, sensitive and simple spectrophotometric method was developed and validated for the determination of the antidepressant duloxetine hydrochloride in pharmaceutical preparation. The method was based on the reaction of duloxetine hydrochloride with 1,2-naphthoquinone-4-sulphonate (NQS) in alkaline media to yield orange colored product. The formation of this complex was also confirmed by UV-visible, FTIR, 1H NMR, Mass spectra techniques and thermal analysis. This method was validated for various parameters according to ICH guidelines. Beer's law is obeyed in a range of 5.0-60 μg/mL at the maximum absorption wavelength of 480 nm. The detection limit is 0.99 μg/mL and the recovery rate is in a range of 98.10-99.57%. The proposed methods was validated and applied to the determination of duloxetine hydrochloride in pharmaceutical preparation. The results were statistically analyzed and compared to those of a reference UV spectrophotometric method.

  1. Hollow carbon nanospheres using an asymmetric triblock copolymer structure directing agent.

    PubMed

    Li, Yunqi; Tan, Haibo; Salunkhe, Rahul R; Tang, Jing; Shrestha, Lok Kumar; Bastakoti, Bishnu Prasad; Rong, Hongpan; Takei, Toshiaki; Henzie, Joel; Yamauchi, Yusuke; Ariga, Katsuhiko

    2016-12-20

    We introduce a simple method to prepare hollow carbon nanospheres (HCNs) by using triblock copolymer poly(styrene-b-2-vinylpyridine-b-ethylene oxide) (PS-b-P2VP-b-PEO) micelles as a new class of soft-templates. Simply by changing the solvent we can prepare ultra-small sized micelles of the triblock copolymer PS-b-P2VP-b-PEO soft template to obtain HCNs with ultra-small diameters (43 nm) and hollow cores (19 nm). Furthermore, we use these HCNs to make electric double-layer capacitors (EDLCs) that exhibit superior performance.

  2. Preparative isolation and characterization of some minor impurities of astaxanthin by high-performance liquid chromatography.

    PubMed

    Rao, R Nageswara; Alvi, S Naseeruddin; Rao, B Nageswara

    2005-05-27

    A simple and rapid preparative high-performance liquid chromatography (HPLC) method has been developed to isolate and characterize some minor impurities of astaxanthin using a normal-phase Lichrosorb silica column with n-hexane-acetone-tetrahydrofuran (90:2:8, v/v/v) as mobile-phase and detection at 475 nm. The isolated impurities were characterized as astacene, dehydro astacene and apoastaxanthinal by UV-vis, ESI-MS, 1H and 13C NMR spectroscopy and the molecular structures were assigned. The impurities collected using the developed conditions were over 98% pure.

  3. Polymer-pyrolysis assisted synthesis of vanadium trioxide and carbon nanocomposites as high performance anode materials for lithium-ion batteries

    NASA Astrophysics Data System (ADS)

    Dong, Yucheng; Ma, Ruguang; Hu, Mingjun; Cheng, Hua; Lee, Jong-Min; Li, Yang Yang; Zapien, Juan Antonio

    2014-09-01

    We present a simple polymer-pyrolysis assisted method to prepare vanadium trioxide and carbon nanocomposites as an advanced anode material for lithium-ion batteries. The as-prepared material deliver a superior battery performance with highly retained capacity of ∼780 mAh g-1 over 100 cycles at a current density of 200 mA g-1, showing excellent cyclic stability, and good rate capability. The improved electrochemical performance of vanadium trioxide and carbon nanocomposites electrode makes it promising as a suitable anode material for practical battery applications.

  4. Nanoarchitectures for Metal-Organic Framework-Derived Nanoporous Carbons toward Supercapacitor Applications.

    PubMed

    Salunkhe, Rahul R; Kaneti, Yusuf Valentino; Kim, Jeonghun; Kim, Jung Ho; Yamauchi, Yusuke

    2016-12-20

    The future advances of supercapacitors depend on the development of novel carbon materials with optimized porous structures, high surface area, high conductivity, and high electrochemical stability. Traditionally, nanoporous carbons (NPCs) have been prepared by a variety of methods, such as templated synthesis, carbonization of polymer precursors, physical and chemical activation, etc. Inorganic solid materials such as mesoporous silica and zeolites have been successfully utilized as templates to prepare NPCs. However, the hard-templating methods typically involve several synthetic steps, such as preparation of the original templates, formation of carbon frameworks, and removal of the original templates. Therefore, these methods are not favorable for large-scale production. Metal-organic frameworks (MOFs) with high surface areas and large pore volumes have been studied over the years, and recently, enormous efforts have been made to utilize MOFs for electrochemical applications. However, their low conductivity and poor stability still present major challenges toward their practical applications in supercapacitors. MOFs can be used as precursors for the preparation of NPCs with high porosity. Their parent MOFs can be prepared with endless combinations of organic and inorganic constituents by simple coordination chemistry, and it is possible to control their porous architectures, pore volumes, surface areas, etc. These unique properties of MOF-derived NPCs make them highly attractive for many technological applications. Compared with carbonaceous materials prepared using conventional precursors, MOF-derived carbons have significant advantages in terms of a simple synthesis with inherent diversity affording precise control over porous architectures, pore volumes, and surface areas. In this Account, we will summarize our recent research developments on the preparation of three-dimensional (3-D) MOF-derived carbons for supercapacitor applications. This Account will be divided into three main sections: (1) useful background on carbon materials for supercapacitor applications, (2) the importance of MOF-derived carbons, and (3) potential future developments of MOF-derived carbons for supercapacitors. This Account focuses mostly on carbons derived from two types of MOFs, namely, zeolite imidazolate framework-8 (ZIF-8) and ZIF-67. By using examples from our previous works, we will show the uniqueness of these carbons for achieving high performance by control of the chemical reactions/conditions as well proper utilization in asymmetric/symmetric supercapacitor configurations. This Account will promote further developments of MOF-derived multifunctional carbon materials with controlled porous architectures for optimization of their electrochemical performance toward supercapacitor applications.

  5. Preparation and application of functionalized nano drug carriers.

    PubMed

    Gong, Rudong; Chen, Gaimin

    2016-05-01

    Targeting at category memory characteristics and preparation methods of functionalized nano drugs, preparation technology of functionalized nano drug carriers is studied, and then important role of functionalized nano drug carrier in preparation of medicine is studied. Carry out the relevant literature search with computer, change limited language in the paper to Chinese and necessarily remove repetitive studies. After first review of 1260 retrieved literature, it can be found that nano drug is with accurate quantity, relatively good targeting, specificity and absorbency. Necessary research of nano drug carriers can prevent and treat disease to a certain extent. Preparation of functionalized nanocarrier is simple and convenient, which can improve frequency of use of nano preparation technology and provide better development space for medical use. Therefore, nanocarriers should be combined with drugs with relatively strong specificity in clinics, in order to be able to conduct effective research on nanometer intelligent drug, effectively promote long-term development of nano biotechnology, and then provide favorable, reliable basis for clinical diagnosis and treatment.

  6. Methane adsorption capacity on graphene derived from glucose and ferric chloride

    NASA Astrophysics Data System (ADS)

    Ismail, M. S.; Yusof, N.; Yusop, M. Zamri; Ismail, A. F.; Nasri, N. S.; Othman, F. E. Che

    2018-05-01

    This study examines the methane adsorption capacity using graphene derived from glucose and ferric chloride (FeCl3). The graphene was prepared via simple method by dissolution of glucose and FeCl3 in water, vaporization of water in oven, and calcination process in quartz furnace. Graphene was successfully produced with impregnation ratio of glucose and FeCl3 at 1:1 and calcination temperature of 650 °C. The prepared graphene subsequently underwent a volumetric adsorption setup, to measure the adsorption capacity of methane (CH4). The highest CH4 adsorption capacity obtained was 6.37 mmol/g at 3.5 bar and 298 K for 40 minutes. These result shows that the prepared graphene displayed good adsorption characteristic for CH4.

  7. Electrochemical Determination of Chlorpyrifos on a Nano-TiO₂Cellulose Acetate Composite Modified Glassy Carbon Electrode.

    PubMed

    Kumaravel, Ammasai; Chandrasekaran, Maruthai

    2015-07-15

    A rapid and simple method of determination of chlorpyrifos is important in environmental monitoring and quality control. Electrochemical methods for the determination of pesticides are fast, sensitive, reproducible, and cost-effective. The key factor in electrochemical methods is the choice of suitable electrode materials. The electrode materials should have good stability, reproducibility, more sensitivity, and easy method of preparation. Mercury-based electrodes have been widely used for the determination of chlorpyrifos. From an environmental point of view mercury cannot be used. In this study a biocompatible nano-TiO2/cellulose acetate modified glassy carbon electrode was prepared by a simple method and used for the electrochemical sensing of chlorpyrifos in aqueous methanolic solution. Electroanalytical techniques such as cyclic voltammetry, differential pulse voltammetry, and amperometry were used in this work. This electrode showed very good stability, reproducibility, and sensitivity. A well-defined peak was obtained for the reduction of chlorpyrifos in cyclic voltammetry and differential pulse voltammetry. A smooth noise-free current response was obtained in amperometric analysis. The peak current obtained was proportional to the concentration of chlorpyrifos and was used to determine the unknown concentration of chlorpyrifos in the samples. Analytical parameters such as LOD, LOQ, and linear range were estimated. Analysis of real samples was also carried out. The results were validated through HPLC. This composite electrode can be used as an alternative to mercury electrodes reported in the literature.

  8. A new and simple resonance Rayleigh scattering method for human serum albumin using graphite oxide as probe.

    PubMed

    Wang, Shengmian; Xu, Lili; Wang, Lisheng; Liang, Aihui; Jiang, Zhiliang

    2013-01-01

    Graphite oxide (GO) was prepared by the Hummer procedure, and can be dispersed to stable colloid solution by ultrasonic wave. The GO exhibited an absorption peak at 313 nm, and a resonance Rayleigh scattering (RRS) peak at 490 nm. In pH 4.6 HAc-NaAc buffer solution, human serum albumin (HSA) combined with GO probe to form large HSA-GO particles that caused the RRS peak increasing at 490 nm. The increased RRS intensity was linear to HSA concentration in the range 0.50-200 µg/mL. Thus, a new and simple RRS method was proposed for the determination of HSA in samples, with a recovery of 98.1-104%. Copyright © 2012 John Wiley & Sons, Ltd.

  9. Simple and Sensitive Molecularly Imprinted Polymer - Mn-Doped ZnS Quantum Dots Based Fluorescence Probe for Cocaine and Metabolites Determination in Urine.

    PubMed

    Chantada-Vázquez, María Pilar; Sánchez-González, Juan; Peña-Vázquez, Elena; Tabernero, María Jesús; Bermejo, Ana María; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

    2016-03-01

    A new molecularly imprinted polymer (MIP)-based fluorescent artificial receptor has been prepared by anchoring a selective MIP for cocaine (COC) on the surface of polyethylene glycol (PEG) modified Mn-doped ZnS quantum dots (QDs). The prepared material combines the high selectivity attributed to MIPs and the sensitive fluorescent property of the Mn-doped ZnS QDs. Simple and low cost methods have therefore been optimized for assessing cocaine abuse in urine by monitoring the fluorescence quenching when the template (COC) and also metabolites from COC [benzoylecgonine (BZE) and ecgonine methyl ester (EME)] are present. Fluorescence quenching was not observed when performing experiments with other drugs of abuse (and their metabolites) or when using nonimprinted polymer (NIP)-coated QDs. Under optimized operating conditions (1.5 mL of 200 mg L(-1) MIP-coated QDs solution, pH 5.5, and 15 min before fluorescence scanning) two analytical methods were developed/validated. One of the procedures (direct method) consisted of urine sample 1:20 dilution before fluorescence measurements. The method has been found to be fast, precise, and accurate, but the standard addition technique for performing the analysis was required because of the existence of matrix effect. The second procedure performed a solid phase extraction (SPE) first, avoiding matrix effect and allowing external calibration. The limits of detection of the methods were 0.076 mg L(-1) (direct method) and 0.0042 mg L(-1) (SPE based method), which are lower than the cutoff values for confirmative conclusions regarding cocaine abuse.

  10. Electrochemical preparation of poly(methylene blue)/graphene nanocomposite thin films

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

    Erçarıkcı, Elif; Dağcı, Kader; Topçu, Ezgi

    2014-07-01

    Highlights: • Poly(MB)/graphene thin films are prepared by a simple electrochemical approach. • Graphene layers in the film show a broad band in visible region of absorbance spectra. • Morphology of composite films indicates both disordered and ordered regions. • XRD reveals that nanocomposite films include rGO layers after electropolymerization process. • Chemically prepared graphene is better than electrochemically prepared graphene for electrooxidation of nitrite. - Abstract: Poly(methylene blue)/graphene nanocomposite thin films were prepared by electropolymerization of methylene blue in the presence of graphene which have been synthesized by two different methods of a chemical oxidation process and an electrochemicalmore » approach. Synthesized nanocomposite thin films were characterized by using cyclic voltammetry, UV–vis. absorption spectroscopy, powder X-ray diffraction, and scanning tunneling microscopy techniques. Electrocatalytical properties of prepared poly(methylene blue)/graphene nanocomposite films were compared toward electrochemical oxidation of nitrite. Under optimized conditions, electrocatalytical effect of nanocomposite films of chemically prepared graphene through electrochemical oxidation of nitrite was better than that of electrochemically prepared graphene.« less

  11. Simple glucose reduction route for one-step synthesis of copper nanofluids

    NASA Astrophysics Data System (ADS)

    Shenoy, U. Sandhya; Shetty, A. Nityananda

    2014-01-01

    One-step method has been employed in the synthesis of copper nanofluids. Copper nitrate is reduced by glucose in the presence of sodium lauryl sulfate. The synthesized particles are characterized by X-ray diffraction technique for the phase structure; electron diffraction X-ray analysis for chemical composition; transmission electron microscopy and field emission scanning electron microscopy for the morphology; Fourier-transform infrared spectroscopy and ultraviolet-visible spectroscopy for the analysis of ingredients of the solution. Thermal conductivity, sedimentation and rheological measurements have also been carried out. It is found that the reaction parameters have considerable effect on the size of the particle formed and rate of the reaction. The techniques confirm that the synthesized particles are copper. The reported method showed promising increase in the thermal conductivity of the base fluid and is found to be reliable, simple and cost-effective method for preparing heat transfer fluids with higher stability.

  12. A simple differential pulse polarographic method for the determination of thymoquinone in black seed oil.

    PubMed

    Michelitsch, Astrid; Rittmannsberger, Anna

    2003-01-01

    A reliable and simple differential pulse polarographic method is described for the determination of thymoquinone in black seed oil. The polarographic behaviour of thymoquinone was examined in various buffer systems over the pH range 5.0-10.0. Thymoquinone is reduced in a single, reversible peak at the dropping mercury electrode. The differential pulse polarogram showed a distinct peak in Sörensen buffer:methanol (3:7, v/v; pH 8.5) at a peak potential of -0.095 V (vs. silver/silver chloride electrode), and a plot of peak height against concentration was found to be linear over the range 0.2-15.0 microg/mL (R = 0.9998). The limit of detection was calculated to be 0.054 microg/mL. The polarographic method has been applied to determine thymoquinone in two black seed oil preparations available on the Austrian pharmaceutical market.

  13. High Shear Homogenization of Lignin to Nanolignin and Thermal Stability of Nanolignin-Polyvinyl Alcohol Blends

    Treesearch

    Sandeep S. Nair; Sudhir Sharma; Yunqiao Pu; Qining Sun; Shaobo Pan; J.Y. Zhu; Yulin Deng; Art J. Ragauskas

    2014-01-01

    A new method to prepare nanolignin using a simple high shear homogenizer is presented. The kraft lignin particles with a broad distribution ranging from large micron- to nano-sized particles were completely homogenized to nanolignin particles with sizes less than 100 nm after 4 h of mechanical shearing. The 13C nuclear magnetic resonance (NMR)...

  14. Multifunctional thin film surface

    DOEpatents

    Brozik, Susan M.; Harper, Jason C.; Polsky, Ronen; Wheeler, David R.; Arango, Dulce C.; Dirk, Shawn M.

    2015-10-13

    A thin film with multiple binding functionality can be prepared on an electrode surface via consecutive electroreduction of two or more aryl-onium salts with different functional groups. This versatile and simple method for forming multifunctional surfaces provides an effective means for immobilization of diverse molecules at close proximities. The multifunctional thin film has applications in bioelectronics, molecular electronics, clinical diagnostics, and chemical and biological sensing.

  15. Simple and effective preparation of nano-pulverized curcumin by femtosecond laser ablation and the cytotoxic effect on C6 rat glioma cells in vitro.

    PubMed

    Tagami, Tatsuaki; Imao, Yukino; Ito, Shunsuke; Nakada, Akiko; Ozeki, Tetsuya

    2014-07-01

    The pulverization of poorly water-soluble drugs and drug candidates into nanoscale particles is a simple and effective means of increasing their pharmacological effect. Consequently, efficient methods for pulverizing compounds are being developed. Femtosecond lasers, which emit ultrashort laser pulses, can be used to generate nanoscale particles without heating and are finding in various fields, including pharmaceutical science. Laser ablation holds promise as a novel top-down pulverization method for obtaining drug nanoparticles. We used a poorly water-soluble compound, curcumin (diferuloyl methane), to understand the characteristics of femtosecond laser pulverization. Various factors such as laser strength, laser scan speed, and the buffer solution affected the size of the curcumin particles. The minimum curcumin particle size was approximately 500 nm; the particle size was stable after 30 days. In vitro studies suggested that curcumin nanoparticles exhibited a cytotoxic effect on C6 rat glioma cells, and remarkable intracellular uptake of the curcumin nanoparticles was observed. The results suggest that femtosecond laser ablation is a useful approach for preparing curcumin nanoparticles that exhibit remarkable therapeutic effects. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Spectrofluorimetric determination of fluoroquinolones in pharmaceutical preparations.

    PubMed

    Ulu, Sevgi Tatar

    2009-02-01

    Simple, rapid and highly sensitive spectrofluorimetric method is presented for the determination of four fluoroquinolone (FQ) drugs, ciprofloxacin, enoxacin, norfloxacin and moxifloxacin in pharmaceutical preparations. Proposed method is based on the derivatization of FQ with 4-chloro-7-nitrobenzofurazan (NBD-Cl) in borate buffer of pH 9.0 to yield a yellow product. The optimum experimental conditions have been studied carefully. Beer's law is obeyed over the concentration range of 23.5-500 ng mL(-1) for ciprofloxacin, 28.5-700 ng mL(-1) for enoxacin, 29.5-800 ng mL(-1) for norfloxacin and 33.5-1000 ng mL(-1) for moxifloxacin using NBD-Cl reagent, respectively. The detection limits were found to be 7.0 ng mL(-1) for ciprofloxacin, 8.5 ng mL(-1) for enoxacin, 9.2 ng mL(-1) for norfloxacin and 9.98 ng mL(-1) for moxifloxacin, respectively. Intra-day and inter-day relative standard deviation and relative mean error values at three different concentrations were determined. The low relative standard deviation values indicate good precision and high recovery values indicate accuracy of the proposed methods. The method is highly sensitive and specific. The results obtained are in good agreement with those obtained by the official and reference method. The results presented in this report show that the applied spectrofluorimetric method is acceptable for the determination of the four FQ in the pharmaceutical preparations. Common excipients used as additives in pharmaceutical preparations do not interfere with the proposed method.

  17. A microscopy method for scanning transmission electron microscopy imaging of the antibacterial activity of polymeric nanoparticles on a biofilm with an ionic liquid.

    PubMed

    Takahashi, Chisato; Muto, Shunsuke; Yamamoto, Hiromitsu

    2017-08-01

    In this study, we developed a scanning transmission electron microscopy (STEM) method for imaging the antibacterial activity of organic polymeric nanoparticles (NPs) toward biofilms formed by Staphylococcus epidermidis bacterial cells, for optimizing NPs to treat biofilm infections. The combination of sample preparation method using a hydrophilic ionic liquid (IL) and STEM observation using the cooling holder eliminates the need for specialized equipment and techniques for biological sample preparation. The annular dark-field STEM results indicated that the two types of biodegradable poly-(DL-lactide-co-glycolide) (PLGA) NPs: PLGA modified with chitosan (CS), and clarithromycin (CAM)-loaded + CS-modified PLGA, prepared by emulsion solvent diffusion exhibited different antibacterial activities in nanoscale. To confirm damage to the sample during STEM observation, we observed the PLGA NPs and the biofilm treated with PLGA NPs by both the conventional method and the newly developed method. The optimized method allows microstructure of the biofilm treated with PLGA NPs to be maintained for 25 min at a current flow of 40 pA. The developed simple sample preparation method would be helpful to understand the interaction of drugs with target materials. In addition, this technique could contribute to the visualization of other deformable composite materials at the nanoscale level. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 1432-1437, 2017. © 2016 Wiley Periodicals, Inc.

  18. A novel method for preparing histology slides to integrate the teaching of gross and microscopic anatomy.

    PubMed

    Provo-Klimek, Judy A; Troyer, Deryl L

    2002-01-01

    The authors have previously reported the development of a novel technique for sampling and preparing tissue slides for routine microscopic examination, without the use of a microtome. Termed "RAMP" (Rapid Adhesive Mediated Procedure), this simple, albeit somewhat crude, technique holds promise as a method that can be used in the field by veterinary practitioners for rapid microscopic evaluations to obtain early preliminary estimates of the nature of a mass or lesion. We incorporated the use of this method into a gross anatomy course in an attempt to gauge its utility for novices in tissue sampling and histology slide preparation. By having each group of students take a tissue sample from their cadaver, the activity simulated an actual necropsy situation in which practitioners in the field might use the technique. Because students were able to follow their specimen from sampling to microscopic examination, the activity provided a valuable integration of their learning of gross and microscopic anatomy. We conducted an evaluation of the process and the resulting slides with two successive classes of students. We conclude that the RAMP method is reasonably successful in the hands of individuals not trained in tissue preparation; was well received by the students as a valuable learning tool; and could potentially yield useful histological information for practicing veterinarians. Limitations of the method are also discussed.

  19. Simple synthesis of PbSe nanocrystals and their self-assembly into 2D ‘flakes’ and 1D ‘ribbons’ structures

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

    Díaz-Torres, E., E-mail: ediaz@cinvestav.mx; Ortega-López, M.; Matsumoto, Y.

    2016-08-15

    Highlights: • PbSe is obtained in a simple way by the co-precipitation method at low-temperature. • The structural, morphological and optical properties of PbSe were studied. • Adding NH{sub 4}OH to the precursor solutions influences on the morphology. • 2D- and 1D-PbSe structures assemble by oriented attachment. • PbSe can be a potential candidate for thermoelectric applications. - Abstract: This work presents a simple and low-temperature method to prepare a variety of Lead selenide (PbSe) nanostructures, using aqueous solutions of Pb(NO{sub 3}){sub 2} and NaHSe. Nanostructures with different morphology were obtained by varying the Pb:Se molar ratio, as well asmore » the mixing sequence of NH{sub 4}OH with either Pb(NO{sub 3}){sub 2} or NaHSe. Nanoparticles with different shapes (spherical and octahedral), and self-assembled structures (flakes and ribbons) were observed by Transmission Electron Microscopy. X-ray results confirmed that the PbSe rock-salt crystalline structure was obtained for all of the prepared samples. The crystal size is in the order of 7.3 to 8.9 nm for single nanocrystals. The absorption spectra of the samples show exciton absorption bands at 1395 nm and 1660 nm. This material could be used to develop more advanced structures for thermoelectric generators.« less

  20. Bandwidth optimization of femtosecond pure-rotational coherent anti-Stokes Raman scattering by pump/Stokes spectral focusing.

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

    Kearney, Sean Patrick

    A simple spectral focusing scheme for bandwidth optimization of gas-phase rotational coherent anti-Stokes Raman scattering (CARS) spectra is presented. The method is useful when femtosecond pump/Stokes preparation of the Raman coherence is utilized. The approach is of practical utility when working with laser pulses that are not strictly transform limited, or when windows or other sources of pulse chirp may be present in the experiment. A delay between the femtosecond preparation pulses is introduced to shift the maximum Raman preparation away from zero frequency and toward the Stokes or anti-Stokes side of the spectrum with no loss in total preparationmore » bandwidth. Shifts of 100 cm -1 or more are attainable and allow for enhanced detection of high-energy (150-300 cm -1) rotational Raman transitions at near transform-limited optimum sensitivity. A simple theoretical treatment for the case of identical pump and Stokes pulses with linear frequency chirp is presented. The approach is then demonstrated experimentally for typical levels of transform-limited laser performance obtained our laboratory with nonresonant CARS in argon and Raman-resonant spectra from a lean H 2/air flat flame.« less

  1. Bandwidth optimization of femtosecond pure-rotational coherent anti-Stokes Raman scattering by pump/Stokes spectral focusing.

    DOE PAGES

    Kearney, Sean Patrick

    2014-07-01

    A simple spectral focusing scheme for bandwidth optimization of gas-phase rotational coherent anti-Stokes Raman scattering (CARS) spectra is presented. The method is useful when femtosecond pump/Stokes preparation of the Raman coherence is utilized. The approach is of practical utility when working with laser pulses that are not strictly transform limited, or when windows or other sources of pulse chirp may be present in the experiment. A delay between the femtosecond preparation pulses is introduced to shift the maximum Raman preparation away from zero frequency and toward the Stokes or anti-Stokes side of the spectrum with no loss in total preparationmore » bandwidth. Shifts of 100 cm -1 or more are attainable and allow for enhanced detection of high-energy (150-300 cm -1) rotational Raman transitions at near transform-limited optimum sensitivity. A simple theoretical treatment for the case of identical pump and Stokes pulses with linear frequency chirp is presented. The approach is then demonstrated experimentally for typical levels of transform-limited laser performance obtained our laboratory with nonresonant CARS in argon and Raman-resonant spectra from a lean H 2/air flat flame.« less

  2. Artificial receptor-functionalized nanoshell: facile preparation, fast separation and specific protein recognition

    NASA Astrophysics Data System (ADS)

    Ouyang, Ruizhuo; Lei, Jianping; Ju, Huangxian

    2010-05-01

    This work combined molecular imprinting technology with superparamagnetic nanospheres as the core to prepare artificial receptor-functionalized magnetic nanoparticles for separation of homologous proteins. Using dopamine as a functional monomer, novel surface protein-imprinted superparamagnetic polydopamine (PDA) core-shell nanoparticles were successfully prepared in physiological conditions, which could maintain the natural structure of a protein template and achieved the development of molecularly imprinted polymers (MIPs) from one dimension to zero dimension for efficient recognition towards large biomolecules. The resultant nanoparticles could be used for convenient magnetic separation of homologous proteins with high specificity. The nanoparticles possessed good monodispersibility, uniform surface morphology and high saturation magnetization value. The bound amounts of template proteins measured by both indirect and direct methods were in good agreement. The maximum number of imprinted cavities on the surface of the bovine hemoglobin (Hb)-imprinted nanoshell was 2.21 × 1018 g - 1, which well matched their maximum binding capacity toward bovine Hb. Both the simple method for preparation of MIPs and the magnetic nanospheres showed good application potential in fast separation, effective concentration and selective biosensing of large protein molecules.

  3. Preparation of Si-containing oxide coating and biomimetic apatite induction on magnesium alloy

    NASA Astrophysics Data System (ADS)

    Yu, Huijun; Dong, Qing; Dou, Jinhe; Pan, Yaokun; Chen, Chuanzhong

    2016-12-01

    Magnesium and its alloys are recently found important in the field of bone repairing for their ideal mechanical performance and excellent biocompatibility. Micro-arc oxidation (MAO) is a simple, controllable and efficient electrochemistry method that can prepare protective ceramic coatings on magnesium alloys. The properties of the MAO coating, such as thickness, microstructure, roughness and composition, can easily be controlled by adjusting the voltage, current density, duration or the electrolyte concentration. In this work, MAO coatings are prepared on ZK61 magnesium alloy at different voltages. The structure characteristics and element distributions of the coating are investigated by XRD, TEM, SEM and EPMA. The MAO samples are immersed in SBF for 7, 14 and 28 days respectively. The corrosion behaviors of the samples in SBF were also investigated by potentiodynamic polarization curves. The corrosion products were characterized by EDS and FT-IR. The MAO coated ZK61 alloy samples showed excellent corrosion resistance and bioactivity. The MAO method demonstrates a great potential in the preparation of degradable and bioactive orthopedic magnesium-based implants.

  4. Preparation and characterization of copper-graphite composites by electrical explosion of wire in liquid.

    PubMed

    Bien, T N; Gul, W H; Bac, L H; Kim, J C

    2014-11-01

    Copper-graphite nanocomposites containing 5 vol.% graphite were prepared by a powder metallurgy route using an electrical wire explosion (EEW) in liquid method and spark plasma sintering (SPS) process. Graphite rods with a 0.3 mm diameter and copper wire with a 0.2 mm diameter were used as raw materials for EEWin liquid. To compare, a pure copper and copper-graphite mixture was also prepared. The fabricated graphite was in the form of a nanosheet, onto which copper particles were coated. Sintering was performed at 900 degrees C at a heating rate of 30 degrees C/min for 10 min and under a pressure of 70 MPa. The density of the sintered composite samples was measured by the Archimedes method. A wear test was performed by a ball-on-disc tribometer under dry conditions at room temperature in air. The presence of graphite effectively reduced the wear of composites. The copper-graphite nanocomposites prepared by EEW had lower wear rates than pure copper material and simple mixed copper-graphite.

  5. Design and characterisation of a polyethylene oxide matrix with the potential use as a teat insert for prevention/treatment of bovine mastitis.

    PubMed

    Bhattarai, Sushila; Alany, Raid G; Bunt, Craig R; Abdelkader, Hamdy; Rathbone, Michael J

    2015-01-01

    This manuscript reports (for the first time) on antibiotic-free polymeric inserts for the prevention and/or treatment of bovine mastitis. Polyethylene oxide (PEO)-based inserts were prepared using different concentrations of various hydrophilic polymers and water-soluble and water-insoluble drug-release-modifying excipients. A simple and scalable melt-extrusion method was employed to prepare the inserts. The prepared inserts were characterised for their dimension, rheological and mechanical properties. The in vitro release of a model bacteriostatic drug (salicylic acid) from the prepared inserts was studied to demonstrate the effectiveness and reproducibility of the melt-extrusion manufacturing method. Further, the in vitro stability of the inserts was evaluated using gel permeation chromatography (GPC) to monitor any change in molecular weight under real-time and accelerated storage conditions. The investigated inserts were stable at accelerated storage conditions over a period of 6 months. PEO inserts have the potential to serve a dual purpose, act as a physical barrier against pathogens invading the teat canal of cows and possibly control the release of a drug.

  6. Initial Study on Thin Film Preparation of Carbon Nanodots Composites as Luminescence Material

    NASA Astrophysics Data System (ADS)

    Iskandar, F.; Aimon, A. H.; Akmaluddin, A. R.; Nuryadin, B. W.; Abdullah, M.

    2016-08-01

    Nowadays, the developments of phosphors materials require elements without noble metals and simple production process. Carbon nanodots (C-dots) are one of phosphor materials with wide range of emission band, and high biocompatibility. In this research thin film carbon nanodots composite have been prepared by spin coating method. Prior deposition, powder carbon nanodots were synthesized from a mixture of commercial urea as the nitrogen sources and citric acid as a carbon source by using hydrothermal and microwave-assisted heating method. The prepared powder was dispersed in transparent epoxy resin and then coated on glass substrate. The photoluminescence result for sample with 0.035 g citric acid exhibited an intense, single, homogeneous and broad spectrum with yellowish emission upon excitation at 365 nm. The Fourier Transform Infrared Spectroscopy (FTIR) result showed the existences of C=C, C-H, C=O, N-H and O-H functional groups which confirmed the quality of the sample. Further, based on UV-Vis measurement, the prepared thin film was highly transparent (transmittance 90%) with estimated film thickness around 764 nm. This result may open an opportunity for optoelectronic devices.

  7. Electrochemical synthesis of gold nanoparticles on the surface of multi-walled carbon nanotubes with glassy carbon electrode and their application

    NASA Astrophysics Data System (ADS)

    Song, Y. Z.; Li, X.; Song, Y.; Cheng, Z. P.; Zhong, H.; Xu, J. M.; Lu, J. S.; Wei, C. G.; Zhu, A. F.; Wu, F. Y.; Xu, J.

    2013-01-01

    Gold nanoparticles on the surface of multi-walled carbon nanotubes with glassy carbon electrode were prepared using electrochemical synthesis method. The thin films of gold Nanoparticles/multi-walled carbon nanotubes were characterized by scanning electron microscopy, powder X-ray diffraction, and cyclic voltammetry. Electrochemical behavior of adrenaline hydrochloride at gold nanoparticles/multi-walled carbon nanotube modified glassy carbon electrode was investigated. A simple, sensitive, and inexpensive method for determination of adrenaline hydrochloride was proposed.

  8. Microbial reduction of graphene oxide by Escherichia coli: a green chemistry approach.

    PubMed

    Gurunathan, Sangiliyandi; Han, Jae Woong; Eppakayala, Vasuki; Kim, Jin-Hoi

    2013-02-01

    Graphene and graphene related materials are an important area of research in recent years due to their unique properties. The extensive industrial application of graphene and related compounds has led researchers to devise novel and simple methods for the synthesis of high quality graphene. In this paper, we developed an environment friendly, cost effective, simple method and green approaches for the reduction of graphene oxide (GO) using Escherichia coli biomass. In biological method, we can avoid use of toxic and environmentally harmful reducing agents commonly used in the chemical reduction of GO to obtain graphene. The biomass of E. coli reduces exfoliated GO to graphene at 37°C in an aqueous medium. The E. coli reduced graphene oxide (ERGO) was characterized with UV-visible absorption spectroscopy, particle analyzer, high resolution X-ray diffractometer, scanning electron microscopy and Raman spectroscopy. Besides the reduction potential, the biomass could also play an important role as stabilizing agent, in which synthesized graphene exhibited good stability in water. This method can open up the new avenue for preparing graphene in cost effective and large scale production. Our findings suggest that GO can be reduced by simple eco-friendly method by using E. coli biomass to produce water dispersible graphene. Copyright © 2012 Elsevier B.V. All rights reserved.

  9. A simple and selective colorimetric mercury (II) sensing system based on chitosan stabilized gold nanoparticles and 2,6-pyridinedicarboxylic acid.

    PubMed

    Tian, Kun; Siegel, Gene; Tiwari, Ashutosh

    2017-02-01

    The development of simple and cost-effective methods for the detection and treatment of Hg 2+ in the environment is an important area of research due to the serious health risk that Hg 2+ poses to humans. Colorimetric sensing based on the induced aggregation of nanoparticles is of great interest since it offers a low cost, simple, and relatively rapid procedure, making it perfect for on-site analysis. Herein we report the development of a simple colorimetric sensor for the selective detection and estimation of mercury ions in water, based on chitosan stabilized gold nanoparticles (AuNPs) and 2,6-pyridinedicarboxylic acid (PDA). In the presence of Hg 2+ , PDA induces the aggregation of AuNPs, causing the solution to change colors varying from red to blue, depending on the concentration of Hg 2+ . The formation of aggregated AuNPs in the presence of Hg 2+ was confirmed using transmission electron microscopy (TEM) and UV-Vis spectroscopy. The method exhibits linearity in the range of 300nM to 5μM and shows excellent selectivity towards Hg 2+ among seventeen different metal ions and was successfully applied for the detection of Hg 2+ in spiked river water samples. The developed technique is simple and superior to the existing techniques in that it allows detection of Hg 2+ using the naked eye and simple and rapid colorimetric analysis, which eliminates the need for sophisticated instruments and sample preparation methods. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Square Wave Voltammetric Determination of Diclofenac in Pharmaceutical Preparations and Human Serum

    PubMed Central

    Ciltas, Ulvihan; Yilmaz, Bilal; Kaban, Selcuk; Akcay, Bilge Kaan; Nazik, Gulsah

    2015-01-01

    In this study, a simple and reliable square wave voltammetric (SWV) method was developed and validated for determination of diclofenac in pharmaceutical preparations and human serum. The proposed method was based on electrooxidation of diclofenac at platinum electrode in 0.1 M TBAClO4/acetonitrile solution. The well-defined two oxidation peaks were observed at 0.87 and 1.27 V, respectively. Calibration curves that were obtained by using current values measured for second peak were linear over the concentration range of 1.5-17.5 μg mL-1 and 2-20 μg mL-1 in supporting electrolyte and serum, respectively. Precision and accuracy were also checked in all media. Intra- and inter-day precision values for diclofenac were less than 3.64, and accuracy (relative error) was better than 2.49%. Developed method in this study is accurate, precise and can be easily applied to Diclomec, Dicloflam and Voltaren tablets as pharmaceutical preparation. Also, the proposed technique was successfully applied to spiked human serum samples. No electroactive interferences from the endogenous substances were found in human serum. PMID:26330859

  11. Square Wave Voltammetric Determination of Diclofenac in Pharmaceutical Preparations and Human Serum.

    PubMed

    Ciltas, Ulvihan; Yilmaz, Bilal; Kaban, Selcuk; Akcay, Bilge Kaan; Nazik, Gulsah

    2015-01-01

    In this study, a simple and reliable square wave voltammetric (SWV) method was developed and validated for determination of diclofenac in pharmaceutical preparations and human serum. The proposed method was based on electrooxidation of diclofenac at platinum electrode in 0.1 M TBAClO4/acetonitrile solution. The well-defined two oxidation peaks were observed at 0.87 and 1.27 V, respectively. Calibration curves that were obtained by using current values measured for second peak were linear over the concentration range of 1.5-17.5 μg mL(-1) and 2-20 μg mL(-1) in supporting electrolyte and serum, respectively. Precision and accuracy were also checked in all media. Intra- and inter-day precision values for diclofenac were less than 3.64, and accuracy (relative error) was better than 2.49%. Developed method in this study is accurate, precise and can be easily applied to Diclomec, Dicloflam and Voltaren tablets as pharmaceutical preparation. Also, the proposed technique was successfully applied to spiked human serum samples. No electroactive interferences from the endogenous substances were found in human serum.

  12. Preparation of vinyl acetate grafted natural rubber by irradiation method

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

    Porntrairat, A.; Pattamaprom, C.

    Improvement in properties of natural rubber could be done by several methods. In this research, gamma radiation technique, which is simple, accurate, easy to control and clean, was applied to enhance the properties of natural rubber (NR) in latex state. The purpose of this research is to study the appropriate condition for preparing grafted natural rubber latex by using irradiation method. Vinyl acetate monomers (VAc) were grafted onto natural rubber latex (NR-g-PVAc) at 0-10 kGys by gamma radiation from Cobalt-60 source at room temperature. Physical properties of grafted natural rubber such as chloroform number, swelling ratio and gel content weremore » measured. The VAc content of NR-g-PVAc was investigated by titration and visualized by FTIR spectroscopy. The FTIR spectra of NR-g-PVAc prepared at 0-10 kGys showed characteristic peaks of the vinyl acetate confirming that VAc could be grafted onto natural rubber molecular chains effectively under appropriate irradiation conditions. From the result, radiation grafting was found to be a useful technique for grafting of vinyl acetate onto natural rubber.« less

  13. A comparative study of alumina-supported Ni catalysts prepared by photodeposition and impregnation methods on the catalytic ozonation of 2,4-dichlorophenoxyacetic acid

    NASA Astrophysics Data System (ADS)

    Rodríguez, Julia L.; Valenzuela, Miguel A.; Tiznado, Hugo; Poznyak, Tatiana; Chairez, Isaac; Magallanes, Diana

    2017-02-01

    The heterogeneous catalytic ozonation on unsupported and supported oxides has been successfully tested for the removal of several refractory compounds in aqueous solution. In this work, alumina-supported nickel catalysts prepared by photodeposition and impregnation methods were compared in the catalytic ozonation of 2,4-dichlorophenoxyacetic acid (2,4-D). The catalysts were characterized by high-resolution electron microscopy and X-ray photoelectron spectroscopy. The photochemical decomposition of Ni acetylacetonate to produce Ni(OH)2, NiO, and traces of Ni° deposited on alumina was achieved in the presence of benzophenone as a sensitizer. A similar surface composition was found with the impregnated catalyst after its reduction with hydrogen at 500 °C and exposed to ambient air. Results indicated a higher initial activity and maleic acid (byproduct) concentration with the photodeposited catalyst (1 wt% Ni) compared to the impregnated catalyst (3 wt% Ni). These findings suggest the use of the photodeposition method as a simple and reliable procedure for the preparation of supported metal oxide/metal catalysts under mild operating conditions.

  14. Laponite as carrier for controlled in vitro delivery of dexamethasone in vitreous humor models.

    PubMed

    Fraile, José M; Garcia-Martin, Elena; Gil, Cristina; Mayoral, José A; Pablo, Luis E; Polo, Vicente; Prieto, Esther; Vispe, Eugenio

    2016-11-01

    Laponite clay is able to retain dexamethasone by simple physisorption, presumably accomplished by hydrogen bonding formation and/or complexation with sodium counterions, as shown by solid state NMR. The physisorption can be somehow modulated by changing the solvent in the adsorption process. This simple system is able to deliver dexamethasone in a controlled manner to solutions used as models for vitreous humor. The proven biocompatibility of laponite as well as its transparency in the gel state, together with the simplicity of the preparation method, makes this system suitable for future in vivo tests of ophthalmic treatment. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Rapid and simple procedure for homogenizing leaf tissues suitable for mini-midi-scale DNA extraction in rice.

    PubMed

    Yi, Gihwan; Choi, Jun-Ho; Lee, Jong-Hee; Jeong, Unggi; Nam, Min-Hee; Yun, Doh-Won; Eun, Moo-Young

    2005-01-01

    We describe a rapid and simple procedure for homogenizing leaf samples suitable for mini/midi-scale DNA preparation in rice. The methods used tungsten carbide beads and general vortexer for homogenizing leaf samples. In general, two samples can be ground completely within 11.3+/-1.5 sec at one time. Up to 20 samples can be ground at a time using a vortexer attachment. The yields of the DNA ranged from 2.2 to 7.6 microg from 25-150 mg of young fresh leaf tissue. The quality and quantity of DNA was compatible for most of PCR work and RFLP analysis.

  16. A simple approach for large-area fabrication of Ag nanorings

    NASA Astrophysics Data System (ADS)

    Yuan, Zhi-hao; Zhou, Wei; Duan, Yue-qin; Bie, Li-jian

    2008-02-01

    A simple and low-cost method based on a two-step heat treatment of AgNO3/SiO2 film has been developed for fabricating metal Ag nanoring arrays. The as-prepared nanorings have an inner diameter of 70-250 nm and an average wall thickness (namely wire diameter) of approximately 30 nm with a number density of approximately 109 cm-2 on the surface of the SiO2 matrix. X-ray diffraction (XRD) results reveal that these nanorings exhibit a face-centered cubic crystal structure. Furthermore, a new growth mechanism, namely a molten metal bubble as a self-template, is tentatively proposed for Ag nanorings.

  17. A solid-phase microextraction fiber with carbon nanoparticles as sorbent material prepared by a simple flame-based preparation process.

    PubMed

    Sun, Min; Feng, Juanjuan; Qiu, Huamin; Fan, Lulu; Li, Leilei; Luo, Chuannan

    2013-07-26

    A novel carbon nanoparticles-coated solid-phase microextraction (SPME) fiber was prepared via a simple and low-cost flame-based preparation process, with stainless steel wire as support. Surface characteristic of the fiber was studied with scanning electron microscope. A nano-scaled brushy structure was observed. Coupled to gas chromatography (GC), the fiber was used to extract phthalate esters (PAEs) and polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Analytical performances of the proposed method were investigated under the optimum extraction conditions (extraction temperature, 40°C; content of KCl, 30% (w/v); extraction time, 50min for PAEs and 40min for PAHs) and compared with other reports for the same analytes. Calibration ranges were 0.06-500μgL(-1) for di-n-butyl phthalate (DBP), and 0.1-300μgL(-1) for di-cyclohexyl phthalate (DCHP) and di-(2-ethyl-hexyl) phthalate (DEHP). For the eight PAHs, good linearity was obtained ranging from 0.01 to 150μgL(-1). Limits of detection were 0.005μgL(-1) for three PAEs and 0.001-0.003μgL(-1) for eight PAHs. The fiber exhibited excellent stability. It can be used for 100 times with RSDs of extraction efficiency less than 22.4%. The as-established SPME-GC method was applied to determine PAEs in food-wrap and PAHs in cigarette ash and snow water, and satisfactory results were obtained. The carbon nanoparticles-coated SPME fiber was efficient for sampling of organic compounds from aqueous samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Effective Surfactants Blend Concentration Determination for O/W Emulsion Stabilization by Two Nonionic Surfactants by Simple Linear Regression.

    PubMed

    Hassan, A K

    2015-01-01

    In this work, O/W emulsion sets were prepared by using different concentrations of two nonionic surfactants. The two surfactants, tween 80(HLB=15.0) and span 80(HLB=4.3) were used in a fixed proportions equal to 0.55:0.45 respectively. HLB value of the surfactants blends were fixed at 10.185. The surfactants blend concentration is starting from 3% up to 19%. For each O/W emulsion set the conductivity was measured at room temperature (25±2°), 40, 50, 60, 70 and 80°. Applying the simple linear regression least squares method statistical analysis to the temperature-conductivity obtained data determines the effective surfactants blend concentration required for preparing the most stable O/W emulsion. These results were confirmed by applying the physical stability centrifugation testing and the phase inversion temperature range measurements. The results indicated that, the relation which represents the most stable O/W emulsion has the strongest direct linear relationship between temperature and conductivity. This relationship is linear up to 80°. This work proves that, the most stable O/W emulsion is determined via the determination of the maximum R² value by applying of the simple linear regression least squares method to the temperature-conductivity obtained data up to 80°, in addition to, the true maximum slope is represented by the equation which has the maximum R² value. Because the conditions would be changed in a more complex formulation, the method of the determination of the effective surfactants blend concentration was verified by applying it for more complex formulations of 2% O/W miconazole nitrate cream and the results indicate its reproducibility.

  19. A simple route to vertical array of quasi-1D ZnO nanofilms on FTO surfaces: 1D-crystal growth of nanoseeds under ammonia-assisted hydrolysis process

    PubMed Central

    2011-01-01

    A simple method for the synthesis of ZnO nanofilms composed of vertical array of quasi-1D ZnO nanostructures (quasi-NRs) on the surface was demonstrated via a 1D crystal growth of the attached nanoseeds under a rapid hydrolysis process of zinc salts in the presence of ammonia at room temperature. In a typical procedure, by simply controlling the concentration of zinc acetate and ammonia in the reaction, a high density of vertically oriented nanorod-like morphology could be successfully obtained in a relatively short growth period (approximately 4 to 5 min) and at a room-temperature process. The average diameter and the length of the nanostructures are approximately 30 and 110 nm, respectively. The as-prepared quasi-NRs products were pure ZnO phase in nature without the presence of any zinc complexes as confirmed by the XRD characterisation. Room-temperature optical absorption spectroscopy exhibits the presence of two separate excitonic characters inferring that the as-prepared ZnO quasi-NRs are high-crystallinity properties in nature. The mechanism of growth for the ZnO quasi-NRs will be proposed. Due to their simplicity, the method should become a potential alternative for a rapid and cost-effective preparation of high-quality ZnO quasi-NRs nanofilms for use in photovoltaic or photocatalytics applications. PACS: 81.07.Bc; 81.16.-c; 81.07.Gf. PMID:22027275

  20. Validation and Uncertainty Estimation of an Ecofriendly and Stability-Indicating HPLC Method for Determination of Diltiazem in Pharmaceutical Preparations

    PubMed Central

    Sadeghi, Fahimeh; Navidpour, Latifeh; Bayat, Sima; Afshar, Minoo

    2013-01-01

    A green, simple, and stability-indicating RP-HPLC method was developed for the determination of diltiazem in topical preparations. The separation was based on a C18 analytical column using a mobile phase consisted of ethanol: phosphoric acid solution (pH = 2.5) (35 : 65, v/v). Column temperature was set at 50°C and quantitation was achieved with UV detection at 240 nm. In forced degradation studies, the drug was subjected to oxidation, hydrolysis, photolysis, and heat. The method was validated for specificity, selectivity, linearity, precision, accuracy, and robustness. The applied procedure was found to be linear in diltiazem concentration range of 0.5–50 μg/mL (r 2 = 0.9996). Precision was evaluated by replicate analysis in which % relative standard deviation (RSD) values for areas were found below 2.0. The recoveries obtained (99.25%–101.66%) ensured the accuracy of the developed method. The degradation products as well as the pharmaceutical excipients were well resolved from the pure drug. The expanded uncertainty (5.63%) of the method was also estimated from method validation data. Accordingly, the proposed validated and sustainable procedure was proved to be suitable for routine analyzing and stability studies of diltiazem in pharmaceutical preparations. PMID:24163778

  1. The Industrial Age of Biocatalytic Transamination.

    PubMed

    Fuchs, Michael; Farnberger, Judith E; Kroutil, Wolfgang

    2015-11-01

    During the last decade the use of ω-transaminases has been identified as a very powerful method for the preparation of optically pure amines from the corresponding ketones. Their immense potential for the preparation of chiral amines, together with their ease of use in combination with existing biocatalytic methods, have made these biocatalysts a competitor to any chemical methodology for (asymmetric) amination. An increasing number of examples, especially from industry, shows that this biocatalytic technology outmaneuvers existing chemical processes by its simple and flexible nature. In the last few years numerous publications and patents on synthetic routes, mainly to pharmaceuticals, involving ω-transaminases have been published. The review gives an overview of the application of ω-transaminases in organic synthesis with a focus on active pharmaceutical ingredients (APIs) and the developments during the last few years.

  2. A facile method for the preparation of monodisperse beads with uniform pore sizes for cell culture.

    PubMed

    Moon, Seung-Kwan; Oh, Myeong-Jin; Paik, Dong-Hyun; Ryu, Tae-Kyung; Park, Kyeongsoon; Kim, Sung-Eun; Park, Jong-Hoon; Kim, Jung-Hyun; Choi, Sung-Wook

    2013-03-12

    This paper describes a facile method for the preparation of porous gelatin beads with uniform pore sizes using a simple fluidic device and their application as supporting materials for cell culture. An aqueous gelatin droplet containing many uniform toluene droplets, produced in the fluidic device, is dropped into liquid nitrogen for instant freezing and the small toluene droplets evolve into pores in the gelatin beads after removal of toluene and then freeze-drying. The porous gelatin beads exhibit a uniform pore size and monodisperse diameter as well as large open pores at the surface. Fluorescence microscopy images of fibroblast-loaded gelatin beads confirm the attachment and proliferation of the cells throughout the porous gelatin beads. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Graphene oxide foams and their excellent adsorption ability for acetone gas

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

    He, Yongqiang; School of Science, Tianjin University, Tianjin 300072; Zhang, Nana

    2013-09-01

    Graphical abstract: - Highlights: • GO and RGO foams were prepared using a simple and green method, unidirectional freeze-drying. • The porous structure of the foams can be adjusted by changing GO concentrations. • GO and RGO foams show good adsorption efficiency for acetone gas. - Abstract: Graphene oxide (GO) and reduced graphene oxide (RGO) foams were prepared using a unidirectional freeze-drying method. These porous carbon materials were characterized by thermal gravimetric analysis, differential scanning calorimetry, X-ray photoelectron spectroscopy and scanning electron microscopy. The adsorption behavior of the two kinds of foams for acetone was studied. The result showed thatmore » the saturated adsorption efficiency of the GO foams was over 100%, and was higher than that of RGO foams and other carbon materials.« less

  4. Pt-decorated PdCo@Pd/C core-shell nanoparticles with enhanced stability and electrocatalytic activity for the oxygen reduction reaction.

    PubMed

    Wang, Deli; Xin, Huolin L; Yu, Yingchao; Wang, Hongsen; Rus, Eric; Muller, David A; Abruña, Hector D

    2010-12-22

    A simple method for the preparation of PdCo@Pd core-shell nanoparticles supported on carbon based on an adsorbate-induced surface segregation effect has been developed. The stability of these PdCo@Pd nanoparticles and their electrocatalytic activity for the oxygen reduction reaction (ORR) were enhanced by decoration with a small amount of Pt deposited via a spontaneous displacement reaction. The facile method described herein is suitable for large-scale, lower-cost production and significantly lowers the Pt loading and thus the cost. The as-prepared PdCo@Pd and Pd-decorated PdCo@Pd nanocatalysts have a higher methanol tolerance than Pt/C in the ORR and are promising cathode catalysts for fuel cell applications.

  5. Pt-Decorated PdCo@Pd/C Core-Shell Nanoparticles with Enhanced Stability and Electrocatalytic Activity for the Oxygen Reduction Reaction

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

    Wang, Deli; Xin, Huolin L.; Yu, Yingchao

    2010-11-24

    A simple method for the preparation of PdCo@Pd core-shell nanoparticles supported on carbon based on an adsorbate-induced surface segregation effect has been developed. The stability of these PdCo@Pd nanoparticles and their electrocatalytic activity for the oxygen reduction reaction (ORR) were enhanced by decoration with a small amount of Pt deposited via a spontaneous displacement reaction. The facile method described herein is suitable for large-scale, lower-cost production and significantly lowers the Pt loading and thus the cost. The as-prepared PdCo@Pd and Pd-decorated PdCo@Pd nanocatalysts have a higher methanol tolerance than Pt/C in the ORR and are promising cathode catalysts for fuelmore » cell applications.« less

  6. Soft template synthesis of yolk/silica shell particles.

    PubMed

    Wu, Xue-Jun; Xu, Dongsheng

    2010-04-06

    Yolk/shell particles possess a unique structure that is composed of hollow shells that encapsulate other particles but with an interstitial space between them. These structures are different from core/shell particles in that the core particles are freely movable in the shell. Yolk/shell particles combine the properties of each component, and can find potential applications in catalysis, lithium ion batteries, and biosensors. In this Research News article, a soft-template-assisted method for the preparation of yolk/silica shell particles is presented. The demonstrated method is simple and general, and can produce hollow silica spheres incorporated with different particles independent of their diameters, geometry, and composition. Furthermore, yolk/mesoporous silica shell particles and multishelled particles are also prepared through optimization of the experimental conditions. Finally, potential applications of these particles are discussed.

  7. The optical and structural properties of graphene nanosheets and tin oxide nanocrystals composite

    NASA Astrophysics Data System (ADS)

    Farheen, Parveen, Azra; Azam, Ameer

    2018-05-01

    A nanocomposite material consisting of metal oxide and reduced graphene oxide was prepared via simple, economic, and effective chemical reduction method. The synthesis strategy was based on the reduction of GO with Sn2+ ion that combines tin oxidation and GO reduction in one step, which provides a simple, low-cost and effective way to prepare graphene nanosheets/SnO2 nanocrystals composites because no additional chemicals were needed. SEM and TEM images shows the uniform distribution of the SnO2 nanocrystals on the Graphene nanosheets (GNs) surface and transmission electron microscope shows an average particle size of 2-4 nm. The mean crystallite size was calculated by Debye Scherrer formula and was found to be about 4.0 nm. Optical analysis was done by using UV-Visible spectroscopy technique and the band gap energy of the GNs/SnO2 nanocomposite was calculated by Tauc relation and came out to be 3.43eV.

  8. Nanoparticles speckled by ready-to-conjugate lanthanide complexes for multimodal imaging

    NASA Astrophysics Data System (ADS)

    Biju, Vasudevanpillai; Hamada, Morihiko; Ono, Kenji; Sugino, Sakiko; Ohnishi, Takashi; Shibu, Edakkattuparambil Sidharth; Yamamura, Shohei; Sawada, Makoto; Nakanishi, Shunsuke; Shigeri, Yasushi; Wakida, Shin-Ichi

    2015-09-01

    Multimodal and multifunctional contrast agents receive enormous attention in the biomedical imaging field. Such contrast agents are routinely prepared by the incorporation of organic molecules and inorganic nanoparticles (NPs) into host materials such as gold NPs, silica NPs, polymer NPs, and liposomes. Despite their non-cytotoxic nature, the large size of these NPs limits the in vivo distribution and clearance and inflames complex pharmacokinetics, which hinder the regulatory approval for clinical applications. Herein, we report a unique method that combines magnetic resonance imaging (MRI) and fluorescence imaging modalities together in nanoscale entities by the simple, direct and stable conjugation of novel biotinylated coordination complexes of gadolinium(iii) to CdSe/ZnS quantum dots (QD) and terbium(iii) to super paramagnetic iron oxide NPs (SPION) but without any host material. Subsequently, we evaluate the potentials of such lanthanide-speckled fluorescent-magnetic NPs for bioimaging at single-molecule, cell and in vivo levels. The simple preparation and small size make such fluorescent-magnetic NPs promising contrast agents for biomedical imaging.

  9. Comparison of HPLC & spectrophotometric methods for estimation of antiretroviral drug content in pharmaceutical products.

    PubMed

    Hemanth Kumar, A K; Sudha, V; Swaminathan, Soumya; Ramachandran, Geetha

    2010-10-01

    Simple and reliable methods to estimate drugs in pharmaceutical products are needed. In most cases, antiretroviral drug estimations are performed using a HPLC method, requiring expensive equipment and trained technicians. A relatively simple and accurate method to estimate antiretroviral drugs in pharmaceutical preparations is by spectrophotometric method, which is cheap and simple to use as compared to HPLC. We undertook this study to standardise methods for estimation of nevirapine (NVP), lamivudine (3TC) and stavudine (d4T) in single tablets/capsules by HPLC and spectrophotometry and to compare the content of these drugs determined by both these methods. Twenty tablets/capsules of NVP, 3TC and d4T each were analysed for their drug content by HPLC and spectrophotometric methods. Suitably diluted drug solutions were run on HPLC fitted with a C18 column using UV detection at ambient temperature. The absorbance of the diluted drug solutions were read in a spectrophotometer at 300, 285 and 270 nm for NVP, 3TC and d4T respectively. Pure powders of the drugs were used to prepare calibration standards of known drug concentrations, which was set up with each assay. The inter-day variation (%) of standards for NVP, 3TC and d4T ranged from 2.5 to 6.7, 2.1 to 7.7 and 6.2 to 7.7, respectively by HPLC. The corresponding values by spectrophotometric method were 2.7 to 4.7, 4.2 to 7.2 and 3.8 to 6.0. The per cent variation between the HPLC and spectrophotometric methods ranged from 0.45 to 4.49 per cent, 0 to 4.98 per cent and 0.35 to 8.73 per cent for NVP, 3TC and d4T,respectively. The contents of NVP, 3TC and d4T in the tablets estimated by HPLC and spectrophotometric methods were similar, and the variation in the amount of these drugs estimated by HPLC and spectrophotometric methods was below 10 per cent. This suggests that the spectrophotometric method is as accurate as the HPLC method for estimation of NVP, 3TC and d4T in tablet/capsule. Hence laboratories that do not have HPLC equipment can also undertake these drug estimations using spectrophotometer.

  10. Direct Identification of On-Bead Peptides Using Surface-Enhanced Raman Spectroscopic Barcoding System for High-Throughput Bioanalysis

    PubMed Central

    Kang, Homan; Jeong, Sinyoung; Koh, Yul; Geun Cha, Myeong; Yang, Jin-Kyoung; Kyeong, San; Kim, Jaehi; Kwak, Seon-Yeong; Chang, Hye-Jin; Lee, Hyunmi; Jeong, Cheolhwan; Kim, Jong-Ho; Jun, Bong-Hyun; Kim, Yong-Kweon; Hong Jeong, Dae; Lee, Yoon-Sik

    2015-01-01

    Recently, preparation and screening of compound libraries remain one of the most challenging tasks in drug discovery, biomarker detection, and biomolecular profiling processes. So far, several distinct encoding/decoding methods such as chemical encoding, graphical encoding, and optical encoding have been reported to identify those libraries. In this paper, a simple and efficient surface-enhanced Raman spectroscopic (SERS) barcoding method using highly sensitive SERS nanoparticles (SERS ID) is presented. The 44 kinds of SERS IDs were able to generate simple codes and could possibly generate more than one million kinds of codes by incorporating combinations of different SERS IDs. The barcoding method exhibited high stability and reliability under bioassay conditions. The SERS ID encoding based screening platform can identify the peptide ligand on the bead and also quantify its binding affinity for specific protein. We believe that our SERS barcoding technology is a promising method in the screening of one-bead-one-compound (OBOC) libraries for drug discovery. PMID:26017924

  11. Direct identification of on-bead peptides using surface-enhanced Raman spectroscopic barcoding system for high-throughput bioanalysis.

    PubMed

    Kang, Homan; Jeong, Sinyoung; Koh, Yul; Geun Cha, Myeong; Yang, Jin-Kyoung; Kyeong, San; Kim, Jaehi; Kwak, Seon-Yeong; Chang, Hye-Jin; Lee, Hyunmi; Jeong, Cheolhwan; Kim, Jong-Ho; Jun, Bong-Hyun; Kim, Yong-Kweon; Hong Jeong, Dae; Lee, Yoon-Sik

    2015-05-28

    Recently, preparation and screening of compound libraries remain one of the most challenging tasks in drug discovery, biomarker detection, and biomolecular profiling processes. So far, several distinct encoding/decoding methods such as chemical encoding, graphical encoding, and optical encoding have been reported to identify those libraries. In this paper, a simple and efficient surface-enhanced Raman spectroscopic (SERS) barcoding method using highly sensitive SERS nanoparticles (SERS ID) is presented. The 44 kinds of SERS IDs were able to generate simple codes and could possibly generate more than one million kinds of codes by incorporating combinations of different SERS IDs. The barcoding method exhibited high stability and reliability under bioassay conditions. The SERS ID encoding based screening platform can identify the peptide ligand on the bead and also quantify its binding affinity for specific protein. We believe that our SERS barcoding technology is a promising method in the screening of one-bead-one-compound (OBOC) libraries for drug discovery.

  12. Application of sulphanilamides disazo dyes with Tropaeolin O for simple, rapid and sensitive spectrophotometric assay of medicines.

    PubMed

    Boiko, Maria; Vrublevska, Teodoziya; Korkuna, Olha; Teslyar, Grigory

    2011-07-01

    A rapid, simple and sensitive spectrophotometric method for the determination of some sulphanilamides is described. The method is based on the formation of blue coloured disazo dyes by the diazotization of sulphonamides viz. sulphanilamide (SA), sulphamerazine (SMR), sulphamethazine (SMZ), sulphadimethoxine (SDM), sulphamethoxazole (SMX), sulphadiazine (SDA), sulfathiazole (STZ), sulphaguanidine (SGN), sulphamonomethoxine (SMM), sulphamethoxypyridazine (SMP) in 0.5M hydrochloric acid media at ice bath followed by the azocoupling reaction with acid monoazo dye Tropaeolin O (TrO) at pH=10.5. Formed products are stable for 10h at room temperature. Effective molar absorptivities at absorbance maxima 595nm for disazo dyes were ∼10(4)M(-1)cm(-1). Stoichiometric ratios of the components of disazo dyes were determined by means of mole ratio and continuous variations methods. Linear ranges for sulphanilamides determination were 0.4-14.0μgml(-1). The methods were successfully approved at suphanilamides determination in model solutions and commercial pharmaceutical preparations. Copyright © 2011 Elsevier B.V. All rights reserved.

  13. A SIMPLE FREEZE-FRACTURE REPLICATION METHOD FOR ELECTRON MICROSCOPY

    PubMed Central

    Bullivant, Stanley; Ames, Adelbert

    1966-01-01

    A simple method to achieve results similar to the freeze-etching technique of Moor et al. (1961) is described. The frozen tissue is cut under liquid nitrogen with a razor blade outside the evaporator rather than inside with a cooled microtome. The conditions of the experiment do not favor sublimation, and it is proposed that the structure of the replica be explained by local faults in the cleavage plane which leaves structures, such as membranes, standing above the ice. Micrographs of replicas of glycerol-protected frozen small intestine of mouse prepared by the method are presented and the structural details they show are discussed. The problem of vapor-deposited contamination is discussed. It is concluded that this is a practical method for obtaining electron micrographs that are relatively free of artifact, and that further improvements may be expected from the use of rapidly frozen fresh tissue and a clean vacuum system, possibly of the ion-pumped type. PMID:5962938

  14. CdS nanoparticles-enhanced chemiluminescence and determination of baicalin in pharmaceutical preparations.

    PubMed

    Chen, Xiaolan; Tan, Xinmei; Wang, Jianxiu

    2013-01-01

    CdS nanoparticles (CdS NPs) of different sizes were synthesized by the citrate reduction method. It was found that CdS NPs could enhance the chemiluminescence (CL) of the luminol-potassium ferricyanide system and baicalin could inhibit CdS NPs-enhanced luminol-potassium ferricyanide CL signals in alkaline solution. Based on this inhibition, a flow-injection CL method was established for determination of baicalin in pharmaceutical preparations and human urine samples. Under optimized conditions, the linear range for determination of baicalin was 5.0 x 10(-6) to 1.0 x 10(-3) g/L. The detection limit at a signal-to-noise ratio of 3 was 1.7 x 10(-6) g/L. CL spectra, UV-visible spectra and transmission electron microscopy (TEM) were used to investigate the CL mechanism. The method described is simple, selective and obviates the need of extensive sample pretreatment. Copyright © 2012 John Wiley & Sons, Ltd.

  15. Cellulose acetate fibers prepared from different raw materials with rapid synthesis method.

    PubMed

    Chen, Jinghuan; Xu, Jikun; Wang, Kun; Cao, Xuefei; Sun, Runcang

    2016-02-10

    Transesterification is a mild process to prepare cellulose acetate (CA) as compared with the traditional method. In this study, CA fibers were produced from six cellulose raw materials based on a simple and rapid transesterification method. The properties of the CA solutions and the obtained CA fibers were investigated in detail. Results showed that all of the cellulose raw materials were esterified within 15 min, and spinning dopes could be obtained by concentrating the CA solutions via vacuum distillation. The XRD, FT-IR, (1)H, (13)C and HSQC NMR analysis confirmed the successful synthesis of CA. The degree of substitution (DS) of the obtained CA was significantly affected by the degree of polymerization (DP) of cellulose raw materials, which further influenced the viscosity of CA solutions as well as the structural, thermal and mechanical properties of the CA fibers. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Solution-mediated cladding doping of commercial polymer optical fibers

    NASA Astrophysics Data System (ADS)

    Stajanca, Pavol; Topolniak, Ievgeniia; Pötschke, Samuel; Krebber, Katerina

    2018-03-01

    Solution doping of commercial polymethyl methacrylate (PMMA) polymer optical fibers (POFs) is presented as a novel approach for preparation of custom cladding-doped POFs (CD-POFs). The presented method is based on a solution-mediated diffusion of dopant molecules into the fiber cladding upon soaking of POFs in a methanol-dopant solution. The method was tested on three different commercial POFs using Rhodamine B as a fluorescent dopant. The dynamics of the diffusion process was studied in order to optimize the doping procedure in terms of selection of the most suitable POF, doping time and conditions. Using the optimized procedure, longer segment of fluorescent CD-POF was prepared and its performance was characterized. Fiber's potential for sensing and illumination applications was demonstrated and discussed. The proposed method represents a simple and cheap way for fabrication of custom, short to medium length CD-POFs with various dopants.

  17. Development and validation of RP HPLC method to determine nandrolone phenylpropionate in different pharmaceutical formulations.

    PubMed

    Mukherjee, Jayanti; Das, Ayan; Chakrabarty, Uday Sankar; Sahoo, Bijay Kumar; Dey, Goutam; Choudhury, Hira; Pal, Tapan Kumar

    2011-01-01

    This study describes development and subsequent validation of a reversed phase high performance liquid chromatographic (RP-HPLC) method for the estimation of nandrolone phenylpropionate, an anabolic steroid, in bulk drug, in conventional parenteral dosage formulation and in prepared nanoparticle dosage form. The chromatographic system consisted of a Luna Phenomenex, CN (250 mm x 4.6 mm, 5 microm) column, an isocratic mobile phase comprising 10 mM phosphate buffer and acetonitrile (50:50, v/v) and UV detection at 240 nm. Nandrolone phenylpropionate was eluted about 6.3 min with no interfering peaks of excipients used for the preparation of dosage forms. The method was linear over the range from 0.050 to 25 microg/mL in raw drug (r2 = 0.9994). The intra-day and inter-day precision values were in the range of 0.219-0.609% and 0.441-0.875%, respectively. Limits of detection and quantitation were 0.010 microg/mL and 0.050 microg/mL, respectively. The results were validated according to International Conference on Harmonization (ICH) guidelines in parenteral and prepared nanoparticle formulation. The validated HPLC method is simple, sensitive, precise, accurate and reproducible.

  18. Simultaneous Determination of Procainamide and N-acetylprocainamide in Rat Plasma by Ultra-High-Pressure Liquid Chromatography Coupled with a Diode Array Detector and Its Application to a Pharmacokinetic Study in Rats.

    PubMed

    Balla, Anusha; Cho, Kwan Hyung; Kim, Yu Chul; Maeng, Han-Joo

    2018-03-30

    A simple, sensitive, and reliable reversed-phase, Ultra-High-Pressure Liquid Chromatography (UHPLC) coupled with a Diode Array Detector (DAD) method for the simultaneous determination of Procainamide (PA) and its major metabolite, N -acetylprocainamide (NAPA), in rat plasma was developed and validated. A simple deproteinization method with methanol was applied to the rat plasma samples, which were analyzed using UHPLC equipped with DAD at 280 nm, and a Synergi™ 4 µm polar, reversed-phase column using 1% acetic acid (pH 5.5) and methanol (76:24, v / v ) as eluent in isocratic mode at a flow rate 0.2 mL/min. The method showed good linearity ( r ² > 0.998) over the concentration range of 20-100,000 and 20-10,000 ng/mL for PA and NAPA, respectively. Intra- and inter-day accuracies ranged from 97.7 to 110.9%, and precision was <10.5% for PA and 99.7 to 109.2 and <10.5%, respectively, for NAPA. The lower limit of quantification was 20 ng/mL for both compounds. This is the first report of the UHPLC-DAD bioanalytical method for simultaneous measurement of PA and NAPA. The most obvious advantage of this method over previously reported HPLC methods is that it requires small sample and injection volumes, with a straightforward, one-step sample preparation. It overcomes the limitations of previous methods, which use large sample volume and complex sample preparation. The devised method was successfully applied to the quantification of PA and NAPA after an intravenous bolus administration of 10 mg/kg procainamide hydrochloride to rats.

  19. A method for reducing the sloughing of thick blood films for malaria diagnosis.

    PubMed

    Norgan, Andrew P; Arguello, Heather E; Sloan, Lynne M; Fernholz, Emily C; Pritt, Bobbi S

    2013-07-08

    The gold standard for malaria diagnosis is the examination of thick and thin blood films. Thick films contain 10 to 20 times more blood than thin films, correspondingly providing increased sensitivity for malaria screening. A potential complication of thick film preparations is sloughing of the blood droplet from the slide during staining or rinsing, resulting in the loss of sample. In this work, two methods for improving thick film slide adherence ('scratch' (SCM) and 'acetone dip' (ADM) methods) were compared to the 'standard method' (SM) of thick film preparation. Standardized blood droplets from 26 previously examined EDTA whole blood specimens (22 positive and four negative) were concurrently spread on glass slides using the SM, ADM, and SCM. For the SM and ADM prepared slides, the droplet was gently spread to an approximate 22 millimeters in diameter spot on the slide using the edge of a second glass slide. For the SCM, the droplet was spread by carefully grinding (or scratching) it into the slide with the point of a second glass slide. Slides were dried for one hour in a laminar flow hood. For the ADM, slides were dipped once in an acetone filled Coplin jar and allowed to air dry. All slides were then Giemsa-stained and examined in a blinded manner. Adherence was assessed by blinded reviewers. No significant or severe defects were observed for slides prepared with the SCM. In contrast, 8 slides prepared by the ADM and 3 prepared using the SM displayed significant or severe defects. Thick films prepared by the three methods were microscopically indistinguishable and concordant results (positive or negative) were obtained for the three methods. Estimated parasitaemia of the blood samples ranged from 25 to 429,169 parasites/μL of blood. The SCM is an inexpensive, rapid, and simple method that improves the adherence of thick blood films to standard glass slides without altering general slide preparation, microscopic appearance or interpretability. Using the SCM, thick films can be reliably examined less than two hours after sample receipt. This represents a significant diagnostic improvement over protocols requiring extended drying periods.

  20. Preparation of Supported Palladium Catalysts using Deep Eutectic Solvents.

    PubMed

    Iwanow, Melanie; Finkelmeyer, Jasmin; Söldner, Anika; Kaiser, Manuela; Gärtner, Tobias; Sieber, Volker; König, Burkhard

    2017-09-12

    Deep eutectic solvents (DESs) dissolve metal salts or oxides and are used as solvent and carbon source for the preparation of supported palladium catalysts. After dissolving of the palladium salt in the DES, the pyrolysis of the mixture under nitrogen atmosphere yields catalytically active palladium on supporting material composed of carbon, nitrogen and oxygen (CNO) by a simple single step preparation method without further activation. The catalysts were characterized by scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) and CHNS/O elementary analysis. The amount of functional groups on the surface of the supporting material was determined by Boehm titrations. Moreover, the activity of the prepared catalysts was evaluated in the hydrogenation of linear alkenes and compared with a commercial Pd/C catalyst. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Peregrine

    PubMed Central

    Langevin, Stanley A.; Bent, Zachary W.; Solberg, Owen D.; Curtis, Deanna J.; Lane, Pamela D.; Williams, Kelly P.; Schoeniger, Joseph S.; Sinha, Anupama; Lane, Todd W.; Branda, Steven S.

    2013-01-01

    Use of second generation sequencing (SGS) technologies for transcriptional profiling (RNA-Seq) has revolutionized transcriptomics, enabling measurement of RNA abundances with unprecedented specificity and sensitivity and the discovery of novel RNA species. Preparation of RNA-Seq libraries requires conversion of the RNA starting material into cDNA flanked by platform-specific adaptor sequences. Each of the published methods and commercial kits currently available for RNA-Seq library preparation suffers from at least one major drawback, including long processing times, large starting material requirements, uneven coverage, loss of strand information and high cost. We report the development of a new RNA-Seq library preparation technique that produces representative, strand-specific RNA-Seq libraries from small amounts of starting material in a fast, simple and cost-effective manner. Additionally, we have developed a new quantitative PCR-based assay for precisely determining the number of PCR cycles to perform for optimal enrichment of the final library, a key step in all SGS library preparation workflows. PMID:23558773

  2. Motor imagery: lessons learned in movement science might be applicable for spaceflight

    PubMed Central

    Bock, Otmar; Schott, Nadja; Papaxanthis, Charalambos

    2015-01-01

    Before participating in a space mission, astronauts undergo parabolic-flight and underwater training to facilitate their subsequent adaptation to weightlessness. Unfortunately, similar training methods can’t be used to prepare re-adaptation to planetary gravity. Here, we propose a quick, simple and inexpensive approach that could be used to prepare astronauts both for the absence and for the renewed presence of gravity. This approach is based on motor imagery (MI), a process in which actions are produced in working memory without any overt output. Training protocols based on MI have repeatedly been shown to modify brain circuitry and to improve motor performance in healthy young adults, healthy seniors and stroke victims, and are routinely used to optimize performance of elite athletes. We propose to use similar protocols preflight, to prepare for weightlessness, and late inflight, to prepare for landing. PMID:26042004

  3. Preparation of graphene oxide as biomaterials for drug adsorption

    NASA Astrophysics Data System (ADS)

    Usca, G. Tubón; Gómez, C. Vacacela; Fiallos, D. Coello; Tavolaro, P.; Martino, G.; Caputi, L. S.; Tavolaro, A.

    2015-02-01

    Doxorubicin hydrochloride (DOX), is a class I anthracycline antibiotic (FDA approved in the 1970s) widely used as an effective chemotherapeutic drug for the treatment of many human neoplasms. Like most anticancer drugs, DOX can provoke severe toxicity to the body when it is administered at high doses systemically. Here we report the results of an investigation of drug adsorption on graphene oxide (GO) materials prepared by the Improved Hummer's method. High-purity GO has been prepared, characterized by XPS, UV-vis, FTIR-ATR, FESEM, UV- vis analyses, Zero Point Charge determinations and applied in the immobilization of doxorubicin, via simple noncovalent method. The adsorption percentage of the drug at pH 7 on GO was observed to be higher (equal to 90 %) than that obtained at acidic pH 3 (equal to 85%). Experimental result of adsorption of DOX on GO, obtained by FTIR-ATR spectroscopy analysis indicate that the inorganic material and the drug form and adduct by π-π stacking interactions.

  4. Structural and optical properties of Cu2ZnSnS4 synthesized by ultrasonic assisted sol-gel method

    NASA Astrophysics Data System (ADS)

    Rajwar, Birendra Kumar; Sharma, Shailendra Kumar

    2018-05-01

    Cu2ZnSnS4 (CZTS) nanocrystals were synthesized by a simple ultrasonic assisted sol-gel method using two different solvents. Structure and purity of the phase formed were investigated using X-ray diffraction (XRD) and Raman measurements. The average crystallite size were estimated by using Scherrer's formula and found to be 2.09 and 7.15 nm. Raman study reveals the kesterite-phase of prepared samples. The influence of solvent in the morphologies of prepared samples was investigated by field emission scanning electron microscopy (FESEM). Ultraviolet-visible-near-infrared absorption measurement was carried out to calculate the optical band gap of samples. Oxidation state of the constitute elements of as-prepared samples were investigated by X-ray photoelectron spectroscopy (XPS) analysis and the results are in good agreement with the literature. The surface area and pore volume were estimated after analysis of nitrogen adsorption-desorption isotherm curves and found to be 16.5 m2/gm and 0.01 cm3/gm respectively.

  5. A Surface Plasmon Resonance-Based Optical Fiber Probe Fabricated with Electropolymerized Molecular Imprinting Film for Melamine Detection

    PubMed Central

    Zheng, Yongping; Zhang, Tingwei; Wu, Songjie; Zhang, Jue; Fang, Jing

    2018-01-01

    Molecularly imprinted polymer (MIP) films prepared by bulk polymerization suffer from numerous deficiencies, including poor mass transfer ability and difficulty in controlling reaction rate and film thickness, which usually result in poor repeatability. However, polymer film synthesized by electropolymerization methods benefit from high reproducibility, simplicity and rapidity of preparation. In the present study, an Au film served as the refractive index-sensitive metal film to couple with the light leaked out from optical fiber core and the electrode for electropolymerizing MIP film simultaneously. The manufactured probe exhibited satisfactory sensitivity and specificity. Furthermore, the surface morphology and functional groups of the synthesized MIP film were characterized by Atomic Force Microscopy (AFM) and Fourier transform infrared microspectroscopy (FTIR) for further insights into the adsorption and desorption processes. Given the low cost, label-free test, simple preparation process and fast response, this method has a potential application to monitor substances in complicated real samples for out-of-lab test in the future. PMID:29522472

  6. One-pot preparation of mRNA/cDNA display by a novel and versatile puromycin-linker DNA.

    PubMed

    Mochizuki, Yuki; Biyani, Manish; Tsuji-Ueno, Sachika; Suzuki, Miho; Nishigaki, Koichi; Husimi, Yuzuru; Nemoto, Naoto

    2011-09-12

    A rapid, easy, and robust preparation method for mRNA/cDNA display using a newly designed puromycin-linker DNA is presented. The new linker is structurally simple, easy to synthesize, and cost-effective for use in "in vitro peptide and protein selection". An introduction of RNase T1 nuclease site to the new linker facilitates the easy recovery of mRNA/cDNA displayed protein by an improvement of the efficiency of ligating the linker to mRNAs and efficient release of mRNA/cDNA displayed protein from the solid-phase (magnetic bead). For application demonstration, affinity selections were successfully performed. Furthermore, we introduced a "one-pot" preparation protocol to perform mRNA display easy. Unlike conventional approaches that require tedious and downstream multistep process including purification, this protocol will make the mRNA/cDNA display methods more practical and convenient and also facilitate the development of next-generation, high-throughput mRNA/cDNA display systems amenable to automation.

  7. Synthesis of water dispersible boron core silica shell (B@SiO2) nanoparticles

    NASA Astrophysics Data System (ADS)

    Walton, Nathan I.; Gao, Zhe; Eygeris, Yulia; Ghandehari, Hamidreza; Zharov, Ilya

    2018-04-01

    Water dispersible boron nanoparticles have great potential as materials for boron neutron capture therapy of cancer and magnetic resonance imaging, if they are prepared on a large scale with uniform size and shape and hydrophilic modifiable surface. We report the first method to prepare spherical, monodisperse, water dispersible boron core silica shell nanoparticles (B@SiO2 NPs) suitable for aforementioned biomedical applications. In this method, 40 nm elemental boron nanoparticles, easily prepared by mechanical milling and carrying 10-undecenoic acid surface ligands, are hydrosilylated using triethoxysilane, followed by base-catalyzed hydrolysis of tetraethoxysilane, which forms a 10-nm silica shell around the boron core. This simple two-step process converts irregularly shaped hydrophobic boron particles into the spherically shaped uniform nanoparticles. The B@SiO2 NPs are dispersible in water and the silica shell surface can be modified with primary amines that allow for the attachment of a fluorophore and, potentially, of targeting moieties. [Figure not available: see fulltext.

  8. A facile drug delivery system preparation through the interaction between drug and iron ion of transferrin

    NASA Astrophysics Data System (ADS)

    Zhou, Lin; Liu, Jihua; Wei, Shaohua; Ge, Xuefeng; Zhou, Jiahong; Yu, Boyang; Shen, Jian

    2013-09-01

    Many anticancer drugs have the capability to form stable complex with metal ions. Based on such property, a simple method to combine these drugs with transferrin, through the interaction between drug and Fe ion of transferrin, to improve their anticancer activity, is proposed. To demonstrate this technique, the complex of photosensitive anticancer drug hypocrellin A and transferrin was prepared by such facile method. The results indicated that the complex of hypocrellin A and transferrin can stabilize in aqueous solution. In vitro studies have demonstrated the superior cancer cell uptake ability of hypocrellin A-transferrin complex to the free hypocrellin A. Significant damage to such drug-impregnated tumor cells was observed upon irradiation and the cancer cells killing ability of hypocrellin A-transferrin was stronger than the free hypocrellin A within a certain range of concentrations. The above results demonstrated the validity and potential of our proposed strategy to prepare the drug delivery system of this type of anti-cancer drugs and transferrin.

  9. Microwave-Assisted Synthesis of Red-Light Emitting Au Nanoclusters with the Use of Egg White

    ERIC Educational Resources Information Center

    Tian, Jinghan; Yan, Lei; Sang, Aohua; Yuan, Hongyan; Zheng, Baozhan; Xiao, Dan

    2014-01-01

    We developed a simple, cost-effective, and eco-friendly method to synthesize gold nanoclusters (AuNCs) with red fluorescence. The experiment was performed using HAuCl[subscript 4], egg white, Na[subscript 2]CO[subscript 3] (known as soda ash or washing soda), and a microwave oven. In our experiment, fluorescent AuNCs were prepared within a…

  10. Development of a sensitive high-performance liquid chromatographic method with simple extraction for simultaneous determination of huperzine A and huperzine B in the species containing lycopodium alkaloids.

    PubMed

    Zhang, Yanqing; Xie, Junbo; Chen, Wen-Qian; Zhou, Tian-Yan; Lu, Wei

    2009-01-01

    A sensitive HPLC method with simple extraction was developed for simultaneous determination of huperzine A (HupA) and huperzine B (HupB) in Huperzia serrata, H. crispata, H. miyoshiana, and Lycopodiastrum casuarinoides. In order to avoid conventional multiple-step and time-consuming sample preparation methods, direct reflux extraction with alkaline chloroform was adopted. The quantitative determination was conducted by reversed-phase HPLC with a photodiode array detector set at 308 nm. Separation was performed on a Luna C18 column (250 x 4.6 mm id, 5 microm) with methanol-0.2% aqueous acetic acid (18 + 82, v/v) mobile phase. The method was validated for accuracy, reproducibility, precision, and limits of detection and quantification. Quantification of the two active compounds in the samples was performed by this newly developed method, and the content of HupA and HupB varied substantially among four different species. The satisfactory results indicated that the developed method can readily be utilized for quality control of the species of Huperziaceae and Lycopodiaceae containing the two compounds.

  11. Fast and economic immobilization methods described for non-commercial Pseudomonas lipases

    PubMed Central

    2014-01-01

    Background There is an increasing interest to seek new enzyme preparations for the development of new products derived from bioprocesses to obtain alternative bio-based materials. In this context, four non-commercial lipases from Pseudomonas species were prepared, immobilized on different low-cost supports, and examined for potential biotechnological applications. Results To reduce costs of eventual scaling-up, the new lipases were obtained directly from crude cell extracts or from growth culture supernatants, and immobilized by simple adsorption on Accurel EP100, Accurel MP1000 and Celite®545. The enzymes evaluated were LipA and LipC from Pseudomonas sp. 42A2, a thermostable mutant of LipC, and LipI.3 from Pseudomonas CR611, which were produced in either homologous or heterologous hosts. Best immobilization results were obtained on Accurel EP100 for LipA and on Accurel MP1000 for LipC and its thermostable variant. Lip I.3, requiring a refolding step, was poorly immobilized on all supports tested (best results for Accurel MP1000). To test the behavior of immobilized lipases, they were assayed in triolein transesterification, where the best results were observed for lipases immobilized on Accurel MP1000. Conclusions The suggested protocol does not require protein purification and uses crude enzymes immobilized by a fast adsorption technique on low-cost supports, which makes the method suitable for an eventual scaling up aimed at biotechnological applications. Therefore, a fast, simple and economic method for lipase preparation and immobilization has been set up. The low price of the supports tested and the simplicity of the procedure, skipping the tedious and expensive purification steps, will contribute to cost reduction in biotechnological lipase-catalyzed processes. PMID:24755191

  12. A Simple Surface-Enhanced Raman Spectroscopic Method for on-Site Screening of Tetracycline Residue in Whole Milk

    PubMed Central

    Dhakal, Sagar; Chao, Kuanglin; Huang, Qing; Kim, Moon; Schmidt, Walter; Qin, Jianwei; Broadhurst, C. Leigh

    2018-01-01

    Therapeutic and subtherapeutic use of veterinary drugs has increased the risk of residue contamination in animal food products. Antibiotics such as tetracycline are used for mastitis treatment of lactating cows. Milk expressed from treated cows before the withdrawal period has elapsed may contain tetracycline residue. This study developed a simple surface-enhanced Raman spectroscopic (SERS) method for on-site screening of tetracycline residue in milk and water. Six batches of silver colloid nanoparticles were prepared for surface enhancement measurement. Milk-tetracycline and water-tetracycline solutions were prepared at seven concentration levels (1000, 500, 100, 10, 1, 0.1, and 0.01 ppm) and spiked with silver colloid nanoparticles. A 785 nm Raman spectroscopic system was used for spectral measurement. Tetracycline vibrational modes were observed at 1285, 1317 and 1632 cm−1 in water-tetracycline solutions and 1322 and 1621 cm−1 (shifted from 1317 and 1632 cm−1, respectively) in milk-tetracycline solutions. Tetracycline residue concentration as low as 0.01 ppm was detected in both the solutions. The peak intensities at 1285 and 1322 cm−1 were used to estimate the tetracycline concentrations in water and milk with correlation coefficients of 0.92 for water and 0.88 for milk. Results indicate that this SERS method is a potential tool that can be used on-site at field production for qualitative and quantitative detection of tetracycline residues. PMID:29389871

  13. A Simple Surface-Enhanced Raman Spectroscopic Method for on-Site Screening of Tetracycline Residue in Whole Milk.

    PubMed

    Dhakal, Sagar; Chao, Kuanglin; Huang, Qing; Kim, Moon; Schmidt, Walter; Qin, Jianwei; Broadhurst, C Leigh

    2018-02-01

    Therapeutic and subtherapeutic use of veterinary drugs has increased the risk of residue contamination in animal food products. Antibiotics such as tetracycline are used for mastitis treatment of lactating cows. Milk expressed from treated cows before the withdrawal period has elapsed may contain tetracycline residue. This study developed a simple surface-enhanced Raman spectroscopic (SERS) method for on-site screening of tetracycline residue in milk and water. Six batches of silver colloid nanoparticles were prepared for surface enhancement measurement. Milk-tetracycline and water-tetracycline solutions were prepared at seven concentration levels (1000, 500, 100, 10, 1, 0.1, and 0.01 ppm) and spiked with silver colloid nanoparticles. A 785 nm Raman spectroscopic system was used for spectral measurement. Tetracycline vibrational modes were observed at 1285, 1317 and 1632 cm -1 in water-tetracycline solutions and 1322 and 1621 cm -1 (shifted from 1317 and 1632 cm -1 , respectively) in milk-tetracycline solutions. Tetracycline residue concentration as low as 0.01 ppm was detected in both the solutions. The peak intensities at 1285 and 1322 cm -1 were used to estimate the tetracycline concentrations in water and milk with correlation coefficients of 0.92 for water and 0.88 for milk. Results indicate that this SERS method is a potential tool that can be used on-site at field production for qualitative and quantitative detection of tetracycline residues.

  14. Foam separation of Rhodamine-G and Evans Blue using a simple separatory bottle system.

    PubMed

    Dasarathy, Dhweeja; Ito, Yoichiro

    2017-09-29

    A simple separatory glass bottle was used to improve separation effectiveness and cost efficiency while simultaneously creating a simpler system for separating biological compounds. Additionally, it was important to develop a scalable separation method so this would be applicable to both analytical and preparative separations. Compared to conventional foam separation methods, this method easily forms stable dry foam which ensures high purity of yielded fractions. A negatively charged surfactant, sodium dodecyl sulfate (SDS), was used as the ligand to carry a positively charged Rhodamine-G, leaving a negatively charged Evans Blue in the bottle. The performance of the separatory bottle was tested for separating Rhodamine-G from Evans Blue with sample sizes ranged from 1 to 12mg in preparative separations and 1-20μg in analytical separations under optimum conditions. These conditions including N 2 gas pressure, spinning speed of contents with a magnetic stirrer, concentration of the ligand, volume of the solvent, and concentration of the sample, were all modified and optimized. Based on the calculations at their peak absorbances, Rhodamine-G and Evans Blue were efficiently separated in times ranging from 1h to 3h, depending on sample volume. Optimal conditions were found to be 60psi N 2 pressure and 2mM SDS for the affinity ligand. This novel separation method will allow for rapid separation of biological compounds while simultaneously being scalable and cost effective. Published by Elsevier B.V.

  15. Chemiluminescence determination of streptomycin in pharmaceutical preparation and its application to pharmacokinetic study by a flow injection analysis assembly

    NASA Astrophysics Data System (ADS)

    Du, Bin; Li, Hongyan; Jin, Jianwen; Wang, Tiantian; Li, Yang; Shen, Guopeng; Li, Xiaotian

    2013-11-01

    A novel and rapid method for the determination of streptomycin has been established by chemiluminescence (CL) based on significant intensity enhancement of streptomycin on the weak CL of N-bromosuccinimide (NBS) and eosin in alkaline medium. The method is simple, rapid and effective to determine streptomycin in the range of 8.0 × 10-9-1.0 × 10-6 g mL-1 with a determination limit of 2.25 × 10-9 g mL-1. The relative standard deviation is 1.95% for the determination of 2.0 × 10-7 g mL-1 streptomycin (n = 11). The pharmacokinetics of streptomycin in plasma of rat coincides with the two-compartment open model. The T1/2α, T1/2β, CL/F, AUC(0-t), MRT, Tmax and Cmax were 18.83 ± 1.24 min, 82.14 ± 3.07 min, 0.0026 ± 0.0011 L kg-1 min-1, 36044.50 ± 105.02 mg min-1 L-1, 92.29 ± 8.21 min, 21.63 ± 1.26 min and 375.61 ± 8.50 μg mL-1, respectively. There was no significant difference between the results obtained by CL and HPLC. The FI-CL method can be used to determine streptomycin in pharmaceutical preparation and biological samples. The established method is simple, rapid and sensitive without expensive instruments. The possible enhancement mechanism was also investigated.

  16. Preparation of 20-HETE using multifunctional enzyme type 2-negative Starmerella bombicola[S

    PubMed Central

    Van Bogaert, Inge; Zhang, Guodong; Yang, Jun; Liu, Jun-Yan; Ye, Yonghao; Soetaert, Wim; Hammock, Bruce D.

    2013-01-01

    The metabolism of arachidonic acid (ARA) by cytochrome P450 ω/ω-1-hydroxylases leads to the formation of 20-hydroxyeicosatetraenoic acid (20-HETE), which is an important lipid-signaling molecule involved in regulation of vascular tone, angiogenesis, and inflammation. Development of a simple method to prepare 20-HETE would greatly facilitate the investigation of its biological activities. The nonpathogenic yeast Starmerella bombicola has been shown to convert exogenously added arachidonic acid to 20-HETE via the biosynthetic pathway of sophorolipids; however, the yield was low. Here we demonstrate that genetic knockout of multifunctional enzyme type 2 (MFE-2), which is involved in the β-oxidation of fatty acids, significantly increases the yield of ARA conversion to 20-HETE and allows practical preparation of 20-HETE. PMID:23966667

  17. [Development ideas of fine pharmaceutical materials of traditional Chinese medicine preparations based on active cluster theory].

    PubMed

    Ke, Zhong-Cheng; Hou, Xue-Feng; Jia, Xiao-Bin

    2016-07-01

    The pharmaceutical materials are divided into coarse and fine types in the development of traditional Chinese medicine preparations. Fine materials with clear composition, stable content and high quality control conform to the international development trend of traditional Chinese medicine preparations. In this paper, the status of fine materials was analyzed, and the development ideas were tentatively put forward. On the one hand, the study on simple methods and efficient equipment shall be strengthened for the simultaneous separation of multiple components of traditional Chinese medicine; on the other hand, the knowledge for traditional Chinese medicine shall be broadened to further develop the scientific compatibility of monomers under the guidance of the theory of traditional Chinese medicine. Copyright© by the Chinese Pharmaceutical Association.

  18. Measuring the Density of a Sugar Solution: A General Chemistry Experiment Using a Student-Prepared Unknown

    ERIC Educational Resources Information Center

    Peterson, Karen I.

    2008-01-01

    The experiment developed in this article addresses the concept of equipment calibration for reducing systematic error. It also suggests simple student-prepared sucrose solutions for which accurate densities are known, but not readily available to students. Densities are measured with simple glassware that has been calibrated using the density of…

  19. Evaluation of rapid and simple techniques for the enrichment of viruses prior to metagenomic virus discovery.

    PubMed

    Hall, Richard J; Wang, Jing; Todd, Angela K; Bissielo, Ange B; Yen, Seiha; Strydom, Hugo; Moore, Nicole E; Ren, Xiaoyun; Huang, Q Sue; Carter, Philip E; Peacey, Matthew

    2014-01-01

    The discovery of new or divergent viruses using metagenomics and high-throughput sequencing has become more commonplace. The preparation of a sample is known to have an effect on the representation of virus sequences within the metagenomic dataset yet comparatively little attention has been given to this. Physical enrichment techniques are often applied to samples to increase the number of viral sequences and therefore enhance the probability of detection. With the exception of virus ecology studies, there is a paucity of information available to researchers on the type of sample preparation required for a viral metagenomic study that seeks to identify an aetiological virus in an animal or human diagnostic sample. A review of published virus discovery studies revealed the most commonly used enrichment methods, that were usually quick and simple to implement, namely low-speed centrifugation, filtration, nuclease-treatment (or combinations of these) which have been routinely used but often without justification. These were applied to a simple and well-characterised artificial sample composed of bacterial and human cells, as well as DNA (adenovirus) and RNA viruses (influenza A and human enterovirus), being either non-enveloped capsid or enveloped viruses. The effect of the enrichment method was assessed by both quantitative real-time PCR and metagenomic analysis that incorporated an amplification step. Reductions in the absolute quantities of bacteria and human cells were observed for each method as determined by qPCR, but the relative abundance of viral sequences in the metagenomic dataset remained largely unchanged. A 3-step method of centrifugation, filtration and nuclease-treatment showed the greatest increase in the proportion of viral sequences. This study provides a starting point for the selection of a purification method in future virus discovery studies, and highlights the need for more data to validate the effect of enrichment methods on different sample types, amplification, bioinformatics approaches and sequencing platforms. This study also highlights the potential risks that may attend selection of a virus enrichment method without any consideration for the sample type being investigated. Copyright © 2013 The Authors. Published by Elsevier B.V. All rights reserved.

  20. Mechanochemical synthesis and intercalation of Ca(II)Fe(III)-layered double hydroxides

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

    Ferencz, Zs.; Szabados, M.; Varga, G.

    2016-01-15

    A mechanochemical method (grinding the components without added water – dry grinding, followed by further grinding in the presence of minute amount of water or NaOH solution – wet grinding) was used in this work for the preparation and intercalation of CaFe-layered double hydroxides (LDHs). Both the pristine LDHs and the amino acid anion (cystinate and tyrosinate) intercalated varieties were prepared by the two-step grinding procedure in a mixer mill. By systematically changing the conditions of the preparation method, a set of parameters could be determined, which led to the formation of close to phase-pure LDH. The optimisation procedure wasmore » also applied for the intercalation processes of the amino acid anions. The resulting materials were structurally characterised by a range of methods (X-ray diffractometry, scanning electron microscopy, energy dispersive analysis, thermogravimetry, X-ray absorption and infra-red spectroscopies). It was proven that this simple mechanochemical procedure was able to produce complex organic–inorganic nanocomposites: LDHs intercalated with amino acid anions. - Graphical abstract: Amino acid anion-Ca(II)Fe(III)-LDHs were successfully prepared by a two-step milling procedure. - Highlights: • Synthesis of pristine and amino acid intercalated CaFe-LDHs by two-step milling. • Identifying the optimum synthesis and intercalation parameters. • Characterisation of the samples with a range of instrumental methods.« less

  1. Dissolution enhancement of efavirenz by solid dispersion and PEGylation techniques

    PubMed Central

    Madhavi, B. Bindu; Kusum, B.; Chatanya, CH. Krishna; Madhu, M. Naga; Harsha, V. Sri; Banji, David

    2011-01-01

    Background: Efavirenz is the preferred nonnucleotide reverse transcriptase inhibitor for first-line antiretroviral treatment in many countries. It is orally active and is specific for human immunodeficiency virus type 1. Its effectiveness can be attributed to its long half-life, which is 52–76 h after multiple doses. The drug is having poor water solubility. The formulation of poorly soluble drug for oral delivery will be one of the biggest challenges for formulation scientists in the research field. Among the available approaches, the solid dispersion technique has often proved to be the most commonly used method in improving dissolution and bioavailability of the drugs because of its simplicity and economy in preparation and evaluation. Materials and Methods: Solid dispersions were prepared by solvent evaporation and physical mixture methods by using polyethylene glycol as the hydrophilic carrier and PEGylated product was also prepared. The prepared products were evaluated for various parameters, such as polymer interaction, saturation solubility study, and drug release studies. The drug release data were analyzed by fitting it into various kinetic models. Results: There is an improvement in the dissolution from 16% to 70% with solid dispersion technology. Higuchi model was found to be the best fit model. Conclusion: Solid dispersion is the simple, efficient, and economic method to improve the dissolution of the poorly water-soluble drugs. PMID:23071917

  2. Development of Semiautomated Module for Preparation of 131I Labeled Lipiodol for Liver Cancer Therapy.

    PubMed

    Mukherjee, Archana; Subramanian, Suresh; Ambade, Rajwardhan; Avhad, Bhaurao; Dash, Ashutosh; Korde, Aruna

    2017-02-01

    Intra-arterial injection of 131 I Lipiodol is an effective treatment option for primary hepatocellular carcinoma as it delivers high radiation dose to liver tumor tissue with minimal accumulation in adjacent normal tissue. The present article demonstrates design, fabrication, and utilization of a semiautomated radiosynthesis module for preparation of 131 I labeled Lipiodol. The radiolabeling method was standardized for preparation of patient dose of 131 I labeled Lipiodol radiochemical yield (RCY); radiochemical purity (RCP) and pharmaceutical purity of the product were determined using optimized procedures. Sterile and apyrogenic 131 I labeled Lipiodol in >60% RCY could be prepared with >95% RCP. Preclinical evaluation in animals indicated retention of more than 90% of activity at 24 hours postportal vein injection. This is the first report demonstrating potential application of simple user friendly and safe semiautomated system for routine production of 131 I labeled Lipiodol, which is adaptable at centralized hospital radiopharmacies. The described prototype module can be modified as per demand for preparation of other therapeutic radiopharmaceuticals.

  3. Facile synthesis of magnetic carbon nitride nanosheets and its application in magnetic solid phase extraction for polycyclic aromatic hydrocarbons in edible oil samples.

    PubMed

    Zheng, Hao-Bo; Ding, Jun; Zheng, Shu-Jian; Zhu, Gang-Tian; Yuan, Bi-Feng; Feng, Yu-Qi

    2016-01-01

    In this study, we proposed a method to fabricate magnetic carbon nitride (CN) nanosheets by simple physical blending. Low-cost CN nanosheets prepared by urea possessed a highly π-conjugated structure; therefore the obtained composites were employed as magnetic solid-phase extraction (MSPE) sorbent for extraction of polycyclic aromatic hydrocarbons (PAHs) in edible oil samples. Moreover, sample pre-treatment time could be carried out within 10 min. Thus, a simple and cheap method for the analysis of PAHs in edible oil samples was established by coupling magnetic CN nanosheets-based MSPE with gas chromatography-mass spectrometry (GC/MS) analysis. Limits of quantitation (LOQs) for eight PAHs ranged from 0.4 to 0.9 ng/g. The intra- and inter-day relative standard deviations (RSDs) were less than 15.0%. The recoveries of PAHs for spiked soybean oil samples ranged from 91.0% to 124.1%, with RSDs of less than 10.2%. Taken together, the proposed method offers a simple and cost-effective option for the convenient analysis of PAHs in oil samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. A validated silver-nanoparticle-enhanced chemiluminescence method for the determination of citalopram in pharmaceutical preparations and human plasma.

    PubMed

    Khan, Muhammad Naeem; Jan, Muhammad Rasul; Shah, Jasmin; Lee, Sang Hak

    2014-05-01

    A simple and sensitive chemiluminescence (CL) method was developed for the determination of citalopram in pharmaceutical preparations and human plasma. The method is based on the enhancement of the weak CL signal of the luminol-H2 O2 system. It was found that the CL signal arising from the reaction between alkaline luminol and H2 O2 was greatly increased by the addition of silver nanoparticles in the presence of citalopram. Prepared silver nanoparticles (AgNPs) were characterized by UV-visible spectroscopy and transmission electron microscopy (TEM). Various experimental parameters affecting CL intensity were studied and optimized for the determination of citalopram. Under optimized experimental conditions, CL intensity was found to be proportional to the concentration of citalopram in the range 40-2500 ng/mL, with a correlation coefficient of 0.9997. The limit of detection (LOD) and limit of quantification (LOQ) of the devised method were 3.78 and 12.62 ng/mL, respectively. Furthermore, the developed method was found to have excellent reproducibility with a relative standard deviation (RSD) of 3.65% (n = 7). Potential interference by common excipients was also studied. The method was validated statistically using recovery studies and was successfully applied to the determination of citalopram in the pure form, in pharmaceutical preparations and in spiked human plasma samples. Percentage recoveries were found to range from 97.71 to 101.99% for the pure form, from 97.84 to 102.78% for pharmaceutical preparations and from 95.65 to 100.35% for spiked human plasma. Copyright © 2013 John Wiley & Sons, Ltd.

  5. Effect of calcination temperature on structural and photocatalyst properties of nanofibers prepared from low-cost natural ilmenite mineral by simple hydrothermal method

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

    Simpraditpan, Athapon; Wirunmongkol, Thanakorn; Pavasupree, Sorapong, E-mail: sorapongp@yahoo.com

    2013-09-01

    Graphical abstract: - Highlights: • Nanofibers were prepared from low-cost ilmenite mineral via simple hydrothermal. • High photocatalyst nanofibers were prepared via post heat treatment method. • The nanofibers calcined at 100–700 °C for 2 h maintained nanofiber structure. • The calcined nanofibers at 400 °C showed the highest photocatalytic activity. - Abstract: Titanate nanofibers were synthesized via the hydrothermal method (120 °C for 72 h) using natural ilmenite mineral (FeTiO{sub 3}) as the starting material. The samples were characterized by X-ray diffraction (XRD), X-ray fluorescent (XRF), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Brunauer–Emmett–Teller (BET) for specificmore » surface area. The nanofibers were 20–90 nm in diameter and 2–7 μm in length. The as-synthesized nanofibers calcined at 300–400 °C showed TiO{sub 2} (B) whereas the nanofibers calcined at 500 °C revealed a mixture of two phases of TiO{sub 2} (B) and anatase. The nanofibers calcined at high temperature of 600–1000 °C showed a mixture of tri-crystalline of anatase, rutile, and Fe{sub 2}O{sub 3}. The rutile phase increased with increasing calcination temperature. The nanofibers calcined at 300–700 °C maintained their structure while the morphology of the nanofibers calcined at 800–1000 °C transformed into submicron rod-like structure. This increase of calcination temperature led to the phase transformation from thermodynamically metastable anatase to the most stable form of rutile phase. The crystallite size of prepared samples increased with increasing calcination temperature. Interestingly, with increasing calcination temperature, the absorption edge of the prepared samples shows an obvious shift to visible light region due to the change of crystallite phase and increased crystallite size. Therefore, the band gap energy of the prepared samples became narrower with increasing calcination temperature. Furthermore, the photocatalytic activity of the nanofibers calcined at 400 °C for 2 h was found to be not merely higher than those of the commercially available TiO{sub 2} nanoparticles powders (P-25, JRC-01, and JRC-03) but also the highest of all the samples in this study.« less

  6. Reduced graphene oxide-wrapped MoO3 composites prepared by using metal-organic frameworks as precursor for all-solid-state flexible supercapacitors.

    PubMed

    Cao, Xiehong; Zheng, Bing; Shi, Wenhui; Yang, Jian; Fan, Zhanxi; Luo, Zhimin; Rui, Xianhong; Chen, Bo; Yan, Qingyu; Zhang, Hua

    2015-08-26

    Reduced graphene oxide-wrapped MoO3M (rGO/MoO3 ) is prepared by a novel and simple method that is developed by using a metal-organic framework as the precursor. After a two-step annealing process, the obtained rGO/MoO3 composite is used for a high-performance supercapacitor electrode. Moreover, an all-solid-state flexible supercapacitor is fabricated based on the rGO/MoO3 composite, which shows stable performance under different bending states. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Facile synthesis of water-soluble and biocompatible fluorescent nitrogen-doped carbon dots for cell imaging.

    PubMed

    Wang, Weiping; Lu, Ya-Chun; Huang, Hong; Feng, Jiu-Ju; Chen, Jian-Rong; Wang, Ai-Jun

    2014-04-07

    A simple, facile and green hydrothermal method was developed in the synthesis of water-soluble nitrogen-doped carbon dots (N-CDs) from streptomycin. The as-prepared N-CDs displayed bright blue fluorescence under the irradiation of UV light, together with a high quantum yield of 7.6% and good biocompatibility as demonstrated by the cell viability assay. Thus, the N-CDs can be used as fluorescent probes for cell imaging, which have potential applications in bioimaging and related fields. This strategy opens a new way for the preparation of fluorescent carbon nanomaterials using small molecules as carbon sources.

  8. Preparation of radioactive iodinated cholylhistamine for use in the radioimmunoassay of cholic acid

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

    Weinberg, P.B.; Kinkade, J.M. Jr.; Collins, D.C.

    1977-11-01

    A major handicap in the development of simple and accurate radioimmunoassay procedures for bile acids has been the lack of a radioactive standard of high specific activity. To provide such a compound, we first synthesized cholylhistamine using the carbodiimide reaction. The hypothesized structure was confirmed by elemental analysis, thin-layer chromatography, infrared and mass spectral analysis. The cholylhistamine was then iodinated with /sup 125/I, using the choloramine-T method. The /sup 125/I-cholylhistamine was bound by antisera raised against a cholic acid-bovine serum albumin conjugate. This procedure should prove useful in preparing radioactive conjugates for all of the bile acids.

  9. Preparation of Ultraviolet Curing Type Silicone Rubbers Containing Mesoporous Silica Fillers.

    PubMed

    Abdullah, Nawfel; Hossain, Md Shahriar A; Fatehmulla, Amanullah; Farooq, Wazirzada Aslam; Islam, Md Tofazzal; Miyamoto, Nobuyoshi; Bando, Yoshio; Kamachi, Yuichiro; Malgras, Victor; Yamauchi, Yusuke; Suzuki, Norihiro

    2018-01-01

    Here we have been focusing on mesoporous silica (MPS) as inorganic filler material to improve the mechanical strength of silicone rubbers. The MPS particles are more effective in reducing the coefficient of thermal expansion (CTE) and hardening silicone rubber composites when compared to commercially available nonporous silica particles. In this study, we utilize ultraviolet curing type silicone rubbers and prepare MPS composites according to a simple single-step method. From an industrial viewpoint, simplifying the fabrication processes is critical. The thermal stability and mechanical strength are examined in detail in order to showcase the effectiveness of MPS particles as filler materials.

  10. Synthesis and characterization of rod like C doped ZnO nanoparticles with enhanced photocatalytic activities

    NASA Astrophysics Data System (ADS)

    Labhane, P. K.; Sapkal, B. M.; Sonawane, G. H.

    2018-05-01

    Carbon (C) doped ZnO rod like nanoparticles were prepared by simple co-precipitation method. The effect of C doping on ZnO has been evaluated by using XRD, Williamson-Hall Plot, FESEM and EDX data. UV light assisted photocatalytic activities of prepared samples were evaluated spectrophotometrically by the degradation of methylene blue (MB). C doped ZnO shows excellent catalytic efficiency compared to pure ZnO, degrading MB completely within 100 min under UV light. Photocatalysis follows the first order kinetics law and the calculated apparent reaction kinetics rate constant suggest the better activity of C-ZnO.

  11. Indirect potentiometric titration of ascorbic acid in pharmaceutical preparations using copper based mercury film electrode.

    PubMed

    Abdul Kamal Nazer, Meeran Mohideen; Hameed, Abdul Rahman Shahul; Riyazuddin, Patel

    2004-01-01

    A simple and rapid potentiometric method for the estimation of ascorbic acid in pharmaceutical dosage forms has been developed. The method is based on treating ascorbic acid with iodine and titration of the iodide produced equivalent to ascorbic acid with silver nitrate using Copper Based Mercury Film Electrode (CBMFE) as an indicator electrode. Interference study was carried to check possible interference of usual excipients and other vitamins. The precision and accuracy of the method was assessed by the application of lack-of-fit test and other statistical methods. The results of the proposed method and British Pharmacopoeia method were compared using F and t-statistical tests of significance.

  12. A method for retrieving endodontic or atypical nonendodontic separated instruments from the root canal: a report of two cases.

    PubMed

    Monteiro, Jardel Camilo do Carmo; Kuga, Milton Carlos; Dantas, Andrea Abi Rached; Jordão-Basso, Keren Cristina Fagundes; Keine, Katia Cristina; Ruchaya, Prashant Jay; Faria, Gisele; Leonardo, Renato de Toledo

    2014-11-01

    This clinical report presents a new method for retrieving separated instruments from the root canal with minimally invasive procedures. The presence of separated instrument in root canal may interfere in the endodontic treatment prognosis. There are several recommended methods to retrieve separated instruments, but some are difficult in clinically practice. This study describes two cases of separated instrument removal from the root canal using a stainless-steel prepared needle associated with a K-file. Case 1 presented a fractured gutta-percha condenser within the mandibular second premolar, it was separated during incorrect intracanal medication calcium hydroxide placement. Case 2 had a fractured sewing needle within the upper central incisor that the patient used to remove food debris from the root canal. After cervical preparation, the fractured instruments were fitted inside a prepared needle and then an endodontic instrument (#25 K-file) was adapted with clockwise turning motion between the needle inner wall and the fragment. The endodontic or atypical nonendodontic separated instrument may be easily pull on of the root canal using a single and low cost device. The methods for retrieving separated instruments from root canal are difficult and destructive procedures. The present case describes a simple method to solve this problem.

  13. Highly luminescent core-shell InP/ZnX (X = S, Se) quantum dots prepared via a phosphine synthetic route.

    PubMed

    Mordvinova, Natalia; Vinokurov, Alexander; Kuznetsova, Tatiana; Lebedev, Oleg I; Dorofeev, Sergey

    2017-01-24

    Here we report a simple method for the creation of highly luminescent core-shell InP/ZnX (X = S, Se) quantum dots (QDs) on the basis of a phosphine synthetic route. In this method a Zn precursor was added to the reaction mixture at the beginning of the synthesis to form an In(Zn)P alloy structure, which promoted the formation of a ZnX shell. Core-shell InP/ZnX QDs exhibit highly intensive emission with a quantum yield over 50%. The proposed method is primarily important for practical applications. Advantages of this method compared to the widely used SILAR technique are discussed. We further demonstrate that the SILAR approach consisting of consequent addition of Zn and chalcogen precursors to pre-prepared non-doped InP colloidal nanoparticles is not quite suitable for shell growth without the addition of special activator agents or the use of very reactive precursors.

  14. A simple one-step ultrasonic-assisted extraction and derivatization method coupling to high-performance liquid chromatographyfor the determination of ε-aminocaproic acid and amino acids in cosmetics.

    PubMed

    Du, Yuanqi; Xia, Ling; Xiao, Xiaohua; Li, Gongke; Chen, Xiaoguang

    2018-06-15

    Nowadays, the safety of cosmetics is a widespread concern. Amines are common cosmetic additives. Some of them such as amino acids are beneficial. Another kind of amines, however, ε-aminocaproic acid (EACA) is prohibited to add into cosmetics for its adverse reactions. In this study, a simple, rapid, sensitive and eco-friendly one-step ultrasonic-assisted extraction and derivatization (UAE-D) method was developed for determination of EACA and amino acids in cosmetics by coupling with high-performance liquid chromatography (HPLC). By using this sample preparation method, extraction and derivatization of EACA and amino acids were finished in one step in ultrasound field. During this procedure, 4-fluoro-7-nitrobenzofurazan (NBD-F)was applied as derivatization reagent. The extraction conditions including the amount of NBD-F, extraction and derivatization temperature, the ultrasonic vibration time and pH value of the aqueous phase were evaluated. Meanwhile, the extraction mechanism was investigated. Under optimized conditions, the method detection limits were 0.086-0.15 μg/L, and method quantitation limits were 0.29-0.47 μg/L with RSDs less than 3.7% (n = 3). The recoveries of EACA and amino acids obtained from cosmetic samples were in range from 76.9% to 122.3%. Amino acids were found in all selected samples and quantified in range from 1.9 ± 0.9 to 677.2 ± 17.9 μg/kg. And EACA was found and quantified with the contents of 1284.3 ± 22.1 μg/kg in a toner sample. This UAE-D-HPLC method shortened and simplified the sample pretreatment as well as enhanced the sensitivity of analytical method. In our record, only 10 min was needed for the total sample preparation process. And the method detection limits were two orders of magnitude less than literature reports. Furthermore, we reduced the consumption of solvent and minimized the usage of organic solvents, which made our method moving towards green analytical chemistry. In brief, our UAE-D-HPLC method is a simple, rapid, sensitive and eco-friendly analytical method for the determination of EACA and amino acids in cosmetics. Copyright © 2018 Elsevier B.V. All rights reserved.

  15. A simple way to prepare Au@polypyrrole/Fe3O4 hollow capsules with high stability and their application in catalytic reduction of methylene blue dye

    NASA Astrophysics Data System (ADS)

    Yao, Tongjie; Cui, Tieyu; Wang, Hao; Xu, Linxu; Cui, Fang; Wu, Jie

    2014-06-01

    Metal nanoparticles are promising catalysts for dye degradation in treating wastewater despite the challenges of recycling and stability. In this study, we have introduced a simple way to prepare Au@polypyrrole (PPy)/Fe3O4 catalysts with Au nanoparticles embedded in a PPy/Fe3O4 capsule shell. The PPy/Fe3O4 capsule shell used as a support was constructed in one-step, which not only dramatically simplified the preparation process, but also easily controlled the magnetic properties of the catalysts through adjusting the dosage of FeCl2.4H2O. The component Au nanoparticles could catalyze the reduction of methylene blue dye with NaBH4 as a reducing agent and the reaction rate constant was calculated through the pseudo-first-order reaction equation. The Fe3O4 nanoparticles permitted quick recycling of the catalysts with a magnet due to their room-temperature superparamagnetic properties; therefore, the catalysts exhibited good reusability. In addition to catalytic activity and reusability, stability is also an important property for catalysts. Because both Au and Fe3O4 nanoparticles were wrapped in the PPy shell, compared with precursor polystyrene/Au composites and bare Fe3O4 nanoparticles, the stability of Au@PPy/Fe3O4 hollow capsules was greatly enhanced. Since the current method is simple and flexible to create recyclable catalysts with high stability, it would promote the practicability of metal nanoparticle catalysts in industrial polluted water treatment.Metal nanoparticles are promising catalysts for dye degradation in treating wastewater despite the challenges of recycling and stability. In this study, we have introduced a simple way to prepare Au@polypyrrole (PPy)/Fe3O4 catalysts with Au nanoparticles embedded in a PPy/Fe3O4 capsule shell. The PPy/Fe3O4 capsule shell used as a support was constructed in one-step, which not only dramatically simplified the preparation process, but also easily controlled the magnetic properties of the catalysts through adjusting the dosage of FeCl2.4H2O. The component Au nanoparticles could catalyze the reduction of methylene blue dye with NaBH4 as a reducing agent and the reaction rate constant was calculated through the pseudo-first-order reaction equation. The Fe3O4 nanoparticles permitted quick recycling of the catalysts with a magnet due to their room-temperature superparamagnetic properties; therefore, the catalysts exhibited good reusability. In addition to catalytic activity and reusability, stability is also an important property for catalysts. Because both Au and Fe3O4 nanoparticles were wrapped in the PPy shell, compared with precursor polystyrene/Au composites and bare Fe3O4 nanoparticles, the stability of Au@PPy/Fe3O4 hollow capsules was greatly enhanced. Since the current method is simple and flexible to create recyclable catalysts with high stability, it would promote the practicability of metal nanoparticle catalysts in industrial polluted water treatment. Electronic supplementary information (ESI) available. See DOI: 10.1039/c4nr00023d

  16. A simple synthesis of MnN0.43@C nanocomposite: characterization and application as battery material

    NASA Astrophysics Data System (ADS)

    Milke, Bettina; Wall, Clemens; Metzke, Sarah; Clavel, Guylhaine; Fichtner, Maximilian; Giordano, Cristina

    2014-12-01

    In the search of new materials for advanced batteries, manganese nitride is an appealing choice. However, in order to fully explore its potentiality, a suitable synthesis is the first mandatory step. In this contribution, nanosized manganese nitride covered by a graphitic shell has been prepared by a simple sol-gel-based process. Since graphite has a high thermal and chemical stability, it acts as stabilizing agent for the MnN0.43 nanoparticles. As a consequence, the particles do not oxidize for instance during the handling of the material and can be stored in air without special precautions. Furthermore, the graphitic shell makes the material more interesting for electrochemical applications, because graphite provides on the one hand an electrical conductivity, which is necessary for the function of active materials, and on the other hand also contributes to the Li storage capacity. The as-prepared nanocomposite was tested as anode material versus lithium metal as counter electrode, showing excellent cyclic stability, 230 mAh/g of capacity, and coulombic efficiencies close to 100 %. Since MnN0.43 possesses a theoretical capacity higher than commercial graphite and exhibits less polarization than several previously reported metal nitrides, it represents an attractive candidate as alternative/novel anode material. The method presented herein offers a simple route to prepare MnN0.43 nanoparticles encapsulated in carbon. The formation mechanism has been investigated, and the detailed characterization of the material before and after battery test (via XRD, HR-TEM, SAED, EELS) is discussed in the text.

  17. Mommio’s Recipe Box: Assessment of the Cooking Habits of Mothers of Preschoolers and Their Perceptions of Recipes for a Video Game

    PubMed Central

    Ugalde, Maciel; Brand, Leah; Beltran, Alicia; Dadabhoy, Hafza; Chen, Tzu-An; O'Connor, Teresia M; Hughes, Sheryl O; Buday, Richard; Nicklas, Theresa A; Baranowski, Janice

    2017-01-01

    Background Vegetables are an important part of a healthy diet because they help prevent several chronic diseases. Mothers of preschoolers reported difficulty getting their young children to eat vegetables, and many did not know how to cook child-pleasing recipes. Objective The cooking habits of mothers of preschoolers, their perceptions of recipes designed for their children, and the involvement of their children in food preparation were assessed to inform a food parenting video game called Mommio. Methods A cross-sectional survey design was used. Eligibility criteria included mothers of 3- to 5-year-old children who reported difficulty getting their children to eat vegetables. Participants completed a demographic questionnaire with questions about their food preparation practices. They were asked to select up to 4 of the 10 provided recipes they wanted to try and to prepare and report back on their experiences. Results Most (46) of the 50 recipes included in Mommio’s in-game recipe box were evaluated at least once and some up to 5 times with a total of 85 evaluations. This well-educated, mostly employed, sample of 27 mothers of preschoolers preferred simple, quick recipes. They ate primarily at home, made dinners from scratch, and indicated that the 46 recipes were generally simple, quick, and easy to prepare. Involvement in preparation enhanced their child’s acceptance of the food. Prior food and preparation preferences influenced the children’s acceptance of the dish at the ensuing meal. Conclusions The high rate of home recipe preparation indicated that including a recipe selection and preparation component in a food parenting video game could be attractive and may enhance effectiveness. Mothers reported that the recipes provided were generally easy to prepare, tasted good, and the instructions were easy to understand, suggesting they could be helpful to the mothers when playing a vegetable parenting game. Some mothers reported that involving their children in recipe preparation influenced their children’s willingness to eat the vegetables. The highest rated recipes are being included in the game, and mothers will be encouraged to involve their children in recipe preparation. PMID:29042344

  18. Contribution of Temporal Preparation and Processing Speed to Simple Reaction Time in Persons with Alzheimer's Disease and Mild Cognitive Impairment

    ERIC Educational Resources Information Center

    Sylvain-Roy, Stephanie; Bherer, Louis; Belleville, Sylvie

    2010-01-01

    Temporal preparation was assessed in 15 Alzheimer's disease (AD) patients, 20 persons with mild cognitive impairment (MCI) and 28 healthy older adults. Participants completed a simple reaction time task in which the preparatory interval duration varied randomly within two blocks (short versus long temporal window). Results indicated that AD and…

  19. Preparing "Chameleon Balls" from Natural Plants: Simple Handmade pH Indicator and Teaching Material for Chemical Education

    NASA Astrophysics Data System (ADS)

    1996-05-01

    Some of the structures in Figure 1 from "Preparing "Chameleon Balls" from Natural Plants: Simple Handmade pH Indicator and Teaching Material for Chemical Education"[Kanda, N.; Asano, T.; Itoh, T.; Onoda, M. J. Chem. Educ. 1995, 72, 1131] were incorrect due to a staff error. The correct figure appears below.

  20. Using of Video Modeling in Teaching a Simple Meal Preparation Skill for Pupils of Down Syndrome

    ERIC Educational Resources Information Center

    AL-Salahat, Mohammad Mousa

    2016-01-01

    The current study aimed to identify the impact of video modeling upon teaching three pupils with Down syndrome the skill of preparing a simple meal (sandwich), where the training was conducted in a separate classroom in schools of normal students. The training consisted of (i) watching the video of an intellectually disabled pupil, who is…

  1. Importance of the rate of hydration of pharmaceutical preparations of guar gum; a new in vitro monitoring method.

    PubMed

    Ellis, P R; Morris, E R

    1991-05-01

    Dietary supplements of guar gum are known to improve blood glucose control in diabetic patients. The efficacy of guar is probably dependent mainly upon its capacity to hydrate rapidly and thus to increase viscosity in the small intestine post-prandially. Measurement of the rate of hydration in vitro might therefore be a useful index of the effectiveness of guar formulations. A simple method for monitoring the hydration rate of guar gum has been developed, which involves measuring the changes in viscosity at discrete time intervals over a period of 5 h using a Brookfield RVT rotoviscometer. Six different samples of guar gum (four pharmaceutical preparations and two food grades of guar flour) were hydrated in sealed glass jars rotated at 6 rev min-1 in order to prevent particle aggregation. Marked differences in hydration rate and ultimate (maximum) viscosity between the different guar samples were observed. Three of the four pharmaceutical preparations were lower in viscosity than the food grades of guar flour during the first 60 min of hydration. Two of the preparations hydrated so slowly that even after 5 h they attained viscosity levels of only 60% of their ultimate viscosity. These results may explain why some guar gum preparations are clinically ineffective.

  2. Preparation of silver-hydroyapatite/PVA nanocomposites: Giant dielectric material for industrial and clinical applications

    NASA Astrophysics Data System (ADS)

    Uddin, Md Jamal; Middya, T. R.; Chaudhuri, B. K.

    2015-02-01

    Pure hydroxyappatite Ca10(PO4)6(OH)2 (or HAP) was prepared from eggshell and potassium dihydrogen phosphate (KH2PO4) by a simple self-chemical reaction method. The clean eggshell was heated at 800 °C in air giving the source of CaO. Appropriate amount of CaO was dissolved in KH2PO4 solution at 37°C for few days. The PH value decreases with increasing the duration of preparation of HAP. Silver nanoparticles derived from silver nitrate solution using black tea leaf extract had been introduced to hydroxyapatite due to its biocompatibility. The unique size- dependent properties of nanomaterials make them superior and indispensable. In this work, hydroxyapatite-silver nanoparticles/polyvinyl alcohol (PVA) composites with 4 different concentrations of hydroxyapatite (1-4 wt %) were prepared by bio-reduction method. Several techniques like XRD and SEM were used to characterize the prepared samples. Frequency dependent capacitance and conductance of the samples were measured using an impedance analyzer. The results showed a remarkable increase in dielectric permittivity (~5117) with low loss (~0.23) at1000 HZ and room temperature (300K) for 4wt% Hydroxapatie-Silver/PVA nanocomposite. Such nanocomposite might be directly applied in manufacturing clinical devices and also for embedding capacitor applications.

  3. A novel nano-Ni/SiO2 catalyst for hydrogen production from steam reforming of ethanol.

    PubMed

    Wu, Chunfei; Williams, Paul T

    2010-08-01

    Catalytic steam reforming of ethanol has been regarded as a promising way to produce hydrogen. However, catalytic deactivation is a key problem in the process. In this paper, a novel nano-Ni/SiO2 catalyst was prepared by a simple sol-gel method and compared to catalysts prepared by an impregnation method in relation to the steam reforming ethanol process. Good Ni dispersion and high BET surface areas (>700 m2 g(-1)) were obtained for sol-gel catalysts, whereas only 1 m2 g(-1) surface area was obtained for the Ni/SiO2 impregnation catalyst. The results of catalytic steam reforming of ethanol showed that about twice of the hydrogen production was produced with the Ni/SiO2 catalyst prepared by sol-gel (around 0.2 g h(-1)) compared with that prepared by impregnation (around 0.1 g h(-1)). The analysis of the used catalysts showed that 10Ni/SiO2-B and 20Ni/SiO2-B presented the highest stability, while other catalysts were fragmented into small pieces after the reforming process, especially the catalysts prepared by impregnation. A novel catalyst has been produced that has been shown to be effective in the production of hydrogen from the steam reforming of ethanol.

  4. Foucault's method for measuring the speed of light with modern apparatus

    NASA Astrophysics Data System (ADS)

    Vörös, Zoltán; Weihs, Gregor

    2015-05-01

    In this paper, we introduce two simple and inexpensive, yet quite accurate versions of the well-known Foucault method for measuring the speed of light. In a compact footprint of just 20 cm by 270 cm with readily available laboratory items, a rotating mirror taken from a laser printer, and a webcam, we obtained c=296\\720+/- 3000 km s-1, and c=302\\295+/- 3000 km s-1, respectively, both within less than a per cent of the defined value. The experiment also prepares students for extracting data through image processing.

  5. Periodate oxidation of nanoscaled magnetic dextran composites

    NASA Astrophysics Data System (ADS)

    Hong, Xia; Guo, Wei; Yuan, Hang; Li, Jun; Liu, Yanmei; Ma, Lan; Bai, Yubai; Li, Tiejin

    2004-02-01

    Highly hydrophilic, uniform and nontoxic magnetic fluids consisting of magnetite (Fe 3O 4) and dextran were prepared. A periodate oxidation method was used to further activate the magnetic dextran, forming magnetic polyaldehyde-dextran, which could be conjugated to biomolecules such as proteins or antibodies. Oxidated Magnetic dextran composites were characterized by TEM, XRD and SQUID magnetometry. Moreover, a flexible, rapid and simple method to detect aldehydes was introduced to the magnetic composite system by utilizing 2,4-dinitrophenylhydrazine reagent. The result of the quantitative analysis of aldehyde was given by thermogravimetric analysis and elemental analysis.

  6. Determination of water pH using absorption-based optical sensors: evaluation of different calculation methods

    NASA Astrophysics Data System (ADS)

    Wang, Hongliang; Liu, Baohua; Ding, Zhongjun; Wang, Xiangxin

    2017-02-01

    Absorption-based optical sensors have been developed for the determination of water pH. In this paper, based on the preparation of a transparent sol-gel thin film with a phenol red (PR) indicator, several calculation methods, including simple linear regression analysis, quadratic regression analysis and dual-wavelength absorbance ratio analysis, were used to calculate water pH. Results of MSSRR show that dual-wavelength absorbance ratio analysis can improve the calculation accuracy of water pH in long-term measurement.

  7. Synthesis and Magnetic Properties of Nearly Monodisperse CoFe2O4Nanoparticles Through a Simple Hydrothermal Condition

    PubMed Central

    2010-01-01

    Nearly monodisperse cobalt ferrite (CoFe2O4) nanoparticles without any size-selection process have been prepared through an alluring method in an oleylamine/ethanol/water system. Well-defined nanospheres with an average size of 5.5 nm have been synthesized using metal chloride as the law materials and oleic amine as the capping agent, through a general liquid–solid-solution (LSS) process. Magnetic measurement indicates that the particles exhibit a very high coercivity at 10 K and perform superparamagnetism at room temperature which is further illuminated by ZFC/FC curves. These superparamagnetic cobalt ferrite nanomaterials are considered to have potential application in the fields of biomedicine. The synthesis method is possible to be a general approach for the preparation of other pure binary and ternary compounds. PMID:20672131

  8. Influence of Zr doping on structure and morphology of TiO2 nanorods prepared using hydrothermal method

    NASA Astrophysics Data System (ADS)

    Muslimin, Masliana; Jumali, Mohammad Hafizuddin; Tee, Tan Sin; Beng, Lee Hock; Hui, Tan Chun; Chin, Yap Chi

    2018-04-01

    The aim of this work is to investigate the effect of Zr doping on TiO2 nanostructure. TiO2 nanorods thin films with different Zr-doping concentrations (6 × 10-3 M, 13 × 10-3 M and 25 × 10-3 M) were successfully prepared using a simple hydrothermal method. The structural and morphological properties of the samples were evaluated using XRD and FESEM respectively. The XRD results revealed that the TiO2 in all samples stabilized as rutile phase. The FESEM micrographs confirmed that TiO2 exist as square like nanorods with blunt tips. Although the crystallographic nature remains unchanged, the introduction of Zr has altered the surface density, structure and morphology of TiO2 which subsequently will have significant effect on its properties.

  9. Development of an enzyme free glucose sensor based on copper oxide-graphene composite by using green reducing agent ascorbic acid

    NASA Astrophysics Data System (ADS)

    Palve, Yogesh Pandit; Jha, Neetu

    2018-05-01

    In this research work we have developed high sensitive and selective glucose sensor based on copper oxide-graphene composite which is prepared by green synthesis method and used for nonenzymatic glucose sensor. In present paper we report that present method highly selective, simple, efficient, accurate, ecofriendly, less toxic. The prepared composite were characterized by material characterization like SEM, XRD and also by electrochemical characterization like CV, chronoamperometry represents that copper oxide-graphene shows excellent electrocatalytic activity towards glucose, exhibiting a good sensitivity of 103.84 µA mM-1 cm-2, a fast response time 2s, a low detection limit 0.00033µM and linear range from 10 µM-3000 µM. The present sensor can successfully apply for determination of glucose concentration in human blood sample.

  10. Preparation of Graphene-Zinc Oxide Nanostructure Composite for Carbon Monoxide Gas Sensing

    NASA Astrophysics Data System (ADS)

    Muchtar, Ahmad Rifqi; Septiani, Ni Luh Wulan; Iqbal, Muhammad; Nuruddin, Ahmad; Yuliarto, Brian

    2018-03-01

    A simple method to synthesize graphene-zinc oxide nanocomposite has been developed. A reduced graphene oxide-ZnO nanocomposite was prepared using a reflux method with ethylene glycol as medium. X-ray diffraction analysis, scanning electron microscopy, energy-dispersive spectrometry, and nitrogen adsorption-desorption measurements were used to characterize the resulting composite materials. The highest response of about 98% was observed when using pure ZnO at 300°C, while the second highest sensor response of about 96% was achieved by graphene-ZnO with 1:3 composition. It was found that the graphene-zinc oxide hybrid has potential to improve sensor performance at low temperature. The graphene-ZnO hybrid with 1:3 composition showed good response of 36% at 125°C, an operating temperature at which pure ZnO showed no response.

  11. Preparation of Graphene-Zinc Oxide Nanostructure Composite for Carbon Monoxide Gas Sensing

    NASA Astrophysics Data System (ADS)

    Muchtar, Ahmad Rifqi; Septiani, Ni Luh Wulan; Iqbal, Muhammad; Nuruddin, Ahmad; Yuliarto, Brian

    2018-07-01

    A simple method to synthesize graphene-zinc oxide nanocomposite has been developed. A reduced graphene oxide-ZnO nanocomposite was prepared using a reflux method with ethylene glycol as medium. X-ray diffraction analysis, scanning electron microscopy, energy-dispersive spectrometry, and nitrogen adsorption-desorption measurements were used to characterize the resulting composite materials. The highest response of about 98% was observed when using pure ZnO at 300°C, while the second highest sensor response of about 96% was achieved by graphene-ZnO with 1:3 composition. It was found that the graphene-zinc oxide hybrid has potential to improve sensor performance at low temperature. The graphene-ZnO hybrid with 1:3 composition showed good response of 36% at 125°C, an operating temperature at which pure ZnO showed no response.

  12. Electrooxidative Tandem Cyclization of Activated Alkynes with Sulfinic Acids To Access Sulfonated Indenones

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

    Wen, Jiangwei; Shi, Wenyan; Zhang, Fan

    An,electrooxidative direct arylsulfonlylation of yones sulfintc acids via a radical tandem cyclization strategy has been developed for the construction of sulfonated ilicIenones:under oxidant, free conditions. This method provides a simple and efficient approach to prepare various sulfonylindenones in good to,excellent:Tyidds,, demonstrating the tremendous prospect of utilizing electrocatalysis in oxidative coupling, Notably, this reaction could Be easily scaled up with good, efficiency.

  13. Dual role of allylsamarium bromide as a Grignard reagent and a single electron transfer reagent in the one-pot synthesis of terminal olefins.

    PubMed

    Li, Ying; Hu, Yuan-Yuan; Zhang, Song-Lin

    2013-11-21

    The utility of allylsamarium bromide, both as a nucleophilic reagent and a single-electron transfer reagent, in the reaction of carbonyl compounds with allylsamarium bromide in the presence of diethyl phosphate is reported in this communication. From a synthetic point of view, a simple one-pot method for the preparation of terminal olefins is developed.

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

    Dhanavel, S.; Nivethaa, E. A. K.; Esther, G.

    Chitosan supported Palladium nanoparticles were synthesized by a simple cost effective chemical reduction method using NaBH{sub 4}. The prepared nanocomposite was characterized by X-Ray diffraction analysis, FESEM and Energy dispersive spectroscopy analysis of X-rays (EDAX). The catalytic performance of the nanocomposite was evaluated on the reduction of 2-Nitrophenol to the 2-Amino phenol with rate constant 1.08 × 10{sup −3} S{sup −1} by NaBH{sub 4} using Spectrophotometer.

  15. Effect of lignin derivatives in the bio-polyols from microwave liquefied bamboo on the properties of polyurethane foams

    Treesearch

    Jiulong Xie; Jinqiu Qi; Chung-Yun Hse; Todd F. Shupe

    2014-01-01

    Bamboo residues were subjected to a microwave-assisted liquefaction process for the production of crude bio-polyols (CBP). The fractionated bio-polyols (FBP) were obtained by the removal of lignin derivatives from the crude bio-polyols (CBP) using a simple method. Polyurethane (PU) foams were successfully prepared from both CBP and FBP. The object of this study was to...

  16. A simple method for the small scale synthesis and solid-phase extraction purification of steroid sulfates.

    PubMed

    Waller, Christopher C; McLeod, Malcolm D

    2014-12-01

    Steroid sulfates are a major class of steroid metabolite that are of growing importance in fields such as anti-doping analysis, the detection of residues in agricultural produce or medicine. Despite this, many steroid sulfate reference materials may have limited or no availability hampering the development of analytical methods. We report simple protocols for the rapid synthesis and purification of steroid sulfates that are suitable for adoption by analytical laboratories. Central to this approach is the use of solid-phase extraction (SPE) for purification, a technique routinely used for sample preparation in analytical laboratories around the world. The sulfate conjugates of sixteen steroid compounds encompassing a wide range of steroid substitution patterns and configurations are prepared, including the previously unreported sulfate conjugates of the designer steroids furazadrol (17β-hydroxyandrostan[2,3-d]isoxazole), isofurazadrol (17β-hydroxyandrostan[3,2-c]isoxazole) and trenazone (17β-hydroxyestra-4,9-dien-3-one). Structural characterization data, together with NMR and mass spectra are reported for all steroid sulfates, often for the first time. The scope of this approach for small scale synthesis is highlighted by the sulfation of 1μg of testosterone (17β-hydroxyandrost-4-en-3-one) as monitored by liquid chromatography-mass spectrometry (LCMS). Copyright © 2014 Elsevier Inc. All rights reserved.

  17. Fabrication of antibacterial blend film from poly (vinyl alcohol) and quaternized chitosan for packaging

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

    Hu, Dongying; Wang, Lijuan, E-mail: donglinwlj@163.com

    Highlights: • HTCC/PVA blend films were prepared through a simple mixing method. • The blend films had greater elongation at break and good optical transmittance. • The blend films had low oxygen permeability and water vapor permeability. • The films had good activity against Escherichia coli and Staphylococcus aureus. - Abstract: Blend films from poly (vinyl alcohol) (PVA) containing N-(2-hydroxy) propyl-3-trimethyl ammonium chloride chitosan (HTCC) were prepared via a simple mixing and casting method. The films were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction measurements (XRD), scanning electron microscopy and ultraviolet-visible measurements (UV–vis). The effects of HTCC amountmore » on mechanical properties, oxygen permeability, water vapor permeation, and antibacterial properties against Gram-negative (Escherichia coli) and Gram-positive (Staphylococcus aureus) of the films were investigated. FTIR and XRD analysis show that HTCC and PVA in the blend films interacted by hydrogen bonding. SEM and UV–vis analysis reveal the good compatibility between HTCC and PVA. Compared with pure PVA film, the blend films had greater elongation at break, lower water permeability, and higher antibacterial activity. The HTCC addition decreased the tensile strength and the light transmittance. The results suggest that HTCC/PVA blend films have a potential as packaging materials.« less

  18. Uniform manganese hexacyanoferrate hydrate nanocubes featuring superior performance for low-cost supercapacitors and nonenzymatic electrochemical sensors

    NASA Astrophysics Data System (ADS)

    Pang, Huan; Zhang, Yizhou; Cheng, Tao; Lai, Wen-Yong; Huang, Wei

    2015-09-01

    Uniform manganese hexacyanoferrate hydrate nanocubes are prepared via a simple chemical precipitation method at room temperature. Due to both micro/mesopores of the Prussian blue analogue and nanocubic structures, the manganese hexacyanoferrate hydrate nanocubes allow the efficient charge transfer and mass transport for electrolyte solution and chemical species. Thus, the manganese hexacyanoferrate hydrate nanocube electrode shows a good rate capability and cycling stability for electrochemical capacitors. Furthermore, electrodes modified with manganese hexacyanoferrate hydrate nanocubes demonstrate a sensitive electrochemical response to hydrogen peroxide (H2O2) in buffer solutions with a high selectivity.Uniform manganese hexacyanoferrate hydrate nanocubes are prepared via a simple chemical precipitation method at room temperature. Due to both micro/mesopores of the Prussian blue analogue and nanocubic structures, the manganese hexacyanoferrate hydrate nanocubes allow the efficient charge transfer and mass transport for electrolyte solution and chemical species. Thus, the manganese hexacyanoferrate hydrate nanocube electrode shows a good rate capability and cycling stability for electrochemical capacitors. Furthermore, electrodes modified with manganese hexacyanoferrate hydrate nanocubes demonstrate a sensitive electrochemical response to hydrogen peroxide (H2O2) in buffer solutions with a high selectivity. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr04322k

  19. Amorphous carbon nanoparticle used as novel resonance energy transfer acceptor for chemiluminescent immunoassay of transferrin.

    PubMed

    Gao, Hongfei; Wang, Wenwen; Wang, Zhenxing; Han, Jing; Fu, Zhifeng

    2014-03-28

    Amorphous carbon nanoparticles (ACNPs) showing highly efficient quenching of chemiluminescence (CL) were prepared from candle soot with a very simple protocol. The prepared ACNP was employed as the novel energy acceptor for a chemiluminescence resonance energy transfer (CRET)-based immunoassay. In this work, ACNP was linked with transferrin (TRF), and horseradish peroxidase (HRP) was conjugated to TRF antibody (HRP-anti-TRF). The immunoreaction rendered the distance between the ACNP acceptor and the HRP-catalyzed CL emitter to be short enough for CRET occurring. In the presence of TRF, this antigen competed with ACNP-TRF for HRP-anti-TRF, thus led to the decreased occurrence of CRET. A linear range of 20-400 ng mL(-1) and a limit of detection of 20 ng mL(-1) were obtained in this immunoassay. The proposed method was successfully applied for detection of TRF levels in human sera, and the results were in good agreement with ELISA method. Moreover, the ACNPs show higher energy transfer efficiency than other conventional nano-scaled energy acceptors such as graphene oxide in CRET assay. It is anticipated that this approach can be developed for determination of other analytes with low cost, simple manipulation and high specificity. Copyright © 2014 Elsevier Ltd. All rights reserved.

  20. Bridging the gap between sample collection and laboratory analysis: using dried blood spots to identify human exposure to chemical agents

    NASA Astrophysics Data System (ADS)

    Hamelin, Elizabeth I.; Blake, Thomas A.; Perez, Jonas W.; Crow, Brian S.; Shaner, Rebecca L.; Coleman, Rebecca M.; Johnson, Rudolph C.

    2016-05-01

    Public health response to large scale chemical emergencies presents logistical challenges for sample collection, transport, and analysis. Diagnostic methods used to identify and determine exposure to chemical warfare agents, toxins, and poisons traditionally involve blood collection by phlebotomists, cold transport of biomedical samples, and costly sample preparation techniques. Use of dried blood spots, which consist of dried blood on an FDA-approved substrate, can increase analyte stability, decrease infection hazard for those handling samples, greatly reduce the cost of shipping/storing samples by removing the need for refrigeration and cold chain transportation, and be self-prepared by potentially exposed individuals using a simple finger prick and blood spot compatible paper. Our laboratory has developed clinical assays to detect human exposures to nerve agents through the analysis of specific protein adducts and metabolites, for which a simple extraction from a dried blood spot is sufficient for removing matrix interferents and attaining sensitivities on par with traditional sampling methods. The use of dried blood spots can bridge the gap between the laboratory and the field allowing for large scale sample collection with minimal impact on hospital resources while maintaining sensitivity, specificity, traceability, and quality requirements for both clinical and forensic applications.

  1. Enhanced Catalytic Activities of NiPt Truncated Octahedral Nanoparticles toward Ethylene Glycol Oxidation and Oxygen Reduction in Alkaline Electrolyte.

    PubMed

    Xia, Tianyu; Liu, Jialong; Wang, Shouguo; Wang, Chao; Sun, Young; Gu, Lin; Wang, Rongming

    2016-05-04

    The high cost and poor durability of Pt nanoparticles (NPs) are great limits for the proton exchange membrane fuel cells (PEMFCs) from being scaled-up for commercial applications. Pt-based bimetallic NPs together with a uniform distribution can effectively reduce the usage of expensive Pt while increasing poison resistance of intermediates. In this work, a simple one-pot method was used to successfully synthesize ultrafine (about 7.5 nm) uniform NiPt truncated octahedral nanoparticles (TONPs) in dimethylformamid (DMF) without any seeds or templates. The as-prepared NiPt TONPs with Pt-rich surfaces exhibit greatly improved catalytic activities together with good tolerance and better stability for ethylene glycol oxidation reaction (EGOR) and oxygen reduction reaction (ORR) in comparison with NiPt NPs and commercial Pt/C catalysts in alkaline electrolyte. For example, the value of mass and specific activities for EGOR are 23.2 and 17.6 times higher comparing with those of commercial Pt/C, respectively. Our results demonstrate that the dramatic enhancement is mainly attributed to Pt-rich surface, larger specific surface area, together with coupling between Ni and Pt atoms. This developed method provides a promising pathway for simple preparation of highly efficient electrocatalysts for PEMFCs in the near future.

  2. Paclitaxel loaded phospholipid-based gel as a drug delivery system for local treatment of glioma.

    PubMed

    Chen, Tijia; Gong, Ting; Zhao, Ting; Liu, Xing; Fu, Yao; Zhang, Zhirong; Gong, Tao

    2017-08-07

    Paclitaxel (PTX) is a chemotherapeutic agent and has been widely used in clinic against human cancer. However, it has limited application in brain tumor treatment due to the poor penetration of blood brain barrier. Local delivery system is a promising carrier of PTX in the treatment of glioma. A biodegradable phospholipid-based gel (PG) system was developed for intratumoral injection and evaluated in brain glioma-bearing mice model. PTX loaded PG was composed of phospholipid, ethanol, medium chain triglyceride, triacetin and PTX. It was prepared by a very simple method. The system was a transparent solution with good fluidity, while turned into a gel after phase-transition when ethanol diffused. Both in vitro dissolution and in vivo imaging study proved the sustained release effect of PG system. In vivo tolerability study showed a better tolerability after mice treated with PTX PG compared with free PTX. The survival time of brain glioma-bearing mice after treatment with PTX PG was significantly prolonged compared with mice treated by free PTX (P<0.05). In conclusion, this study developed a novel PG based local PTX delivery system with simple preparation method, good tolerability and high therapeutic efficacy. It has a great potential to improve the clinical management of glioma. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Formation of ZnS nanostructures by a simple way of thermal evaporation

    NASA Astrophysics Data System (ADS)

    Yuan, H. J.; Xie, S. S.; Liu, D. F.; Yan, X. Q.; Zhou, Z. P.; Ci, L. J.; Wang, J. X.; Gao, Y.; Song, L.; Liu, L. F.; Zhou, W. Y.; Wang, G.

    2003-11-01

    The mass synthesis of ZnS nanobelts, nanowires, and nanoparticles has been achieved by a simple method of thermal evaporation of ZnS powders onto silicon substrates in the presence of Au catalyst. The temperature of the substrates and the concentration of ZnS vapor were the critical experimental parameters for the formation of different morphologies of ZnS nanostructures. Scanning electron microscopy and transmission electron microscopy show that the diameters of as-prepared nanowires were 30-70 nm. The UV emission at 374 nm is probably related to the exciton emission, while the mechanism of blue emission at 443 nm is probably mainly due to the presence of various surface states.

  4. Pd(OAc)2/Ph3P-catalyzed dimerization of isoprene and synthesis of monoterpenic heterocycles.

    PubMed

    Kellner, Dominik; Weger, Maximilian; Gini, Andrea; Mancheño, Olga García

    2017-01-01

    The palladium-catalyzed dimerization of isoprene is a practical approach of synthesizing monoterpenes. Though several highly selective methods have been reported, most of them still required pressure or costly ligands for attaining the active system and desired selectivity. Herein, we present a simple and economical procedure towards the tail-to-tail dimer using readily available Pd(OAc) 2 and inexpensive triphenylphosphine as ligand. Furthermore, simple screw cap vials are employed, allowing carrying out the reaction at low pressure. In addition, the potential of the dimer as a chemical platform for the preparation of heterocyclic terpenes by subsequent (hetero)-Diels-Alder or [4 + 1]-cycloadditions with nitrenes is also depicted.

  5. A simple control for sediment-toxicity exposures using the amphipod, Hyalella azteca

    USGS Publications Warehouse

    Lasier, Peter J.; Urich, Matthew L.

    2014-01-01

    Sediment-toxicity exposures comparing survival and growth of the freshwater amphipod, Hyalella azteca, are often components of aquatic-habitat assessments. Standardized exposure methods have been established and require evaluations for quality assurance. Test acceptability using performance-based criteria can be determined from exposures to control sediments, which are collected from the environment or formulated from commercially available components. Amending sand with leached alfalfa solids provided a simple formulated sediment that elicited consistently acceptable survival and growth in 28-day exposures with and without a daily feeding regime. A procedure is described for preparing the sediment along with results from comparisons among sand, amended sand, and field-collected sediments that incorporated three feeding regimes.

  6. Facile preparation of polypyrrole/graphene oxide nanocomposites with large areal capacitance using electrochemical codeposition for supercapacitors

    NASA Astrophysics Data System (ADS)

    Zhou, Haihan; Han, Gaoyi; Xiao, Yaoming; Chang, Yunzhen; Zhai, Hua-Jin

    2014-10-01

    A simple and low-cost electrochemical codeposition method has been introduced to fabricate polypyrrole/graphene oxide (PPy/GO) nanocomposites and the areal capacitance of conducting polymer/GO composites is reported for the first time. Fourier transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD) are implemented to determine the PPy/GO nanocomposites are successfully prepared and the interaction between PPy and GO. The as-prepared PPy/GO nanocomposites show the curly sheet-like morphology, superior capacitive behaviors and cyclic stability. Furthermore, the varying deposition time is implemented to investigate the impact of the loading amount on electrochemical behavior of the composites, and a high areal capacitance of 152 mF cm-2 is achieved at 10 mV s-1 CV scan. However, the thicker films caused by the long deposition time would result in larger diffusion resistance of electrolyte ions, consequently exhibit the relatively lower capacitance value at the high current density. The GCD tests indicate moderate deposition time is more suitable for the fast charge/discharge. Considering the very simple and effective synthetic process, the PPy/GO nanocomposites with relatively high areal capacitance are competitive candidate for supercapacitor application, and its capacitive performances can be easily tuned by varying the deposition time.

  7. Preparation of high affinity antibody for ribavirin with new haptens and residue analysis in chicken muscle, eggs and duck muscle.

    PubMed

    Wang, Zhaopeng; Yu, Xuezhi; Ma, Licai; Liu, Hebing; Ding, Shuangyang; Wang, Zhanhui; Zhang, Xiya; Shen, Jianzhong; Wen, Kai

    2018-05-23

    In this work, high affinity polyclonal antibodies for ribavirin (RBV) from new haptens were prepared and were used to analyse RBV residues in chicken muscle, eggs and duck muscle. The new haptens were synthesised with different spacers, and the best antibody was obtained with an IC 50 value as low as 0.61 ng/mL in indirect competitive enzyme-linked immunosorbent assay (ELISA). The cross-reactivities with another five antiviral drugs including amantadine, rimantadine, moroxydine, zanamivir and oseltamivir were less than 0.1%, which indicated the good specificity of the antibody. An ELISA was developed based on the antibody and applied to detect RBV in multi-food matrices. The sample preparation prior to detection only needed simple dilution after trichloroacetic acid extraction. The limits of detection were 1.07, 1.18 and 1.03 μg/kg in chicken muscle, eggs and duck muscle, respectively. Recoveries ranged from 89.0% to 112.7% with coefficients of variation below 13.0%. Ten blind samples of chicken muscle were analysed simultaneously by ELISA and liquid chromatography-tandem mass spectrometry, and a good correlation between the methods was observed. The results indicated that the high affinity antibody could be applied for the simple and fast detection of RBV in multi-food matrices.

  8. Highly uniform and monodisperse carbon nanospheres enriched with cobalt-nitrogen active sites as a potential oxygen reduction electrocatalyst

    NASA Astrophysics Data System (ADS)

    Wan, Xing; Wang, Hongjuan; Yu, Hao; Peng, Feng

    2017-04-01

    Uniform cobalt and nitrogen co-doped carbon nanospheres (CoN-CNS) with high specific surface area (865 m2 g-1) have been prepared by a simple but efficient method. The prepared CoN-CNS catalyst exhibits outstanding catalytic performance for the oxygen reduction reaction (ORR) in both alkaline and acidic electrolytes. In alkaline electrolyte, the prepared CoN-CNS has more positive half-wave potential and larger kinetic current density than commercial Pt/C. In acidic electrolyte, CoN-CNS also shows good ORR activity with high electron transfer number, its onset and half-wave potentials are all close to those of commercial carbon supported platinum catalyst (Pt/C). CoN-CNS catalyst shows more superior stability and higher methanol-tolerance than commercial Pt/C both in alkaline and in acidic electrolytes. The potassium thiocyanate-poisoning test further confirms that the cobalt-nitrogen active sites exist in CoN-CNS, which are dominating to endow high ORR catalytic activity in acidic electrolyte. This study develops a new method to prepare non-precious metal catalyst with excellent ORR performances for direct methanol fuel cells.

  9. Preparation and bactericide activity of gallic acid stabilized gold nanoparticles

    NASA Astrophysics Data System (ADS)

    Moreno-Álvarez, S. A.; Martínez-Castañón, G. A.; Niño-Martínez, N.; Reyes-Macías, J. F.; Patiño-Marín, N.; Loyola-Rodríguez, J. P.; Ruiz, Facundo

    2010-10-01

    In this work, gold nanoparticles with three different sizes (13.7, 39.4, and 76.7 nm) were prepared using a simple aqueous method with gallic acid as the reducing and stabilizing agent, the different sizes were obtained varying some experimental parameters as the pH of the reaction and the amount of the gallic acid. The prepared nanoparticles were characterized using X-ray diffraction, transmission electron microscopy, dynamic light scattering, and UV-Vis spectroscopy. Samples were identified as elemental gold and present spherical morphology, a narrow size distribution and good stabilization according to TEM and DLS results. The antibacterial activity of this gallic acid stabilized gold nanoparticles against S. mutans (the etiologic agent of dental caries) was assessed using a microdilution method obtaining a minimum inhibitory concentration of 12.31, 12.31, and 49.25 μg/mL for 13.7, 39.4, and 76.7 nm gold nanoparticles, respectively. The antibacterial assay showed that gold nanoparticles prepared in this work present a bactericide activity by a synergistic action with gallic acid. The MIC found for this nanoparticles are much lower than those reported for mixtures of gold nanoparticles and antibiotics.

  10. Bottom-up preparation and structural study of monodispersed lipid particles with internal structure

    NASA Astrophysics Data System (ADS)

    Kim, Hojun; Alfeche, Alana; Leal, Cecilia

    Lipid based nanoparticles having internal bicontinuous cubic phases, also known as cubosomes, are becoming increasingly interesting drug delivery platforms. Compared to the liposomes, they offer an augmented surface area for drug encapsulation. However, this simple argument is insufficient to explain the cellular delivery performance of cubosomes compared to other lipid-based nanoparticles. One could argue that their topology facilitates membrane fusion and endosomal escape but at the moment the exact mechanism of cubosome cellular internalization and endosomal escape is still unknown. This is partially because the practical use of cubosomes has been limited due to hurdles of uncontrollable size and shape distributions. The conventional top-down preparation methods (sonication/homogenization) yield large and polydisperse particles. In this presentation we introduce a new system based on microfluidic devices to prepare small (200 nm) and monodisperse cubosomes with a quality not possible using conventional methods. With this approach, we successfully prepared spherical and monodisperse cubosomes (PDI: 0.01) with and without drug loading. To characterize the cubosomes and the formation mechanisms, we utilize Small Angle X-ray Scattering (SAXS) and Cryogenic TEM. We acknowledge the funding source as a NIH.

  11. In Situ Preparation of Biomimetic Thin Films and Their Surface-Shielding Effect for Organisms in High Vacuum

    PubMed Central

    Muranaka, Yoshinori; Shimomura, Masatsugu; Hariyama, Takahiko

    2013-01-01

    Self-standing biocompatible films have yet to be prepared by physical or chemical vapor deposition assisted by plasma polymerization because gaseous monomers have thus far been used to create only polymer membranes. Using a nongaseous monomer, we previously found a simple fabrication method for a free-standing thin film prepared from solution by plasma polymerization, and a nano-suit made by polyoxyethylene (20) sorbitan monolaurate can render multicellular organisms highly tolerant to high vacuum. Here we report thin films prepared by plasma polymerization from various monomer solutions. The films had a flat surface at the irradiated site and were similar to films produced by vapor deposition of gaseous monomers. However, they also exhibited unique characteristics, such as a pinhole-free surface, transparency, solvent stability, flexibility, and a unique out-of-plane molecular density gradient from the irradiated to the unirradiated surface of the film. Additionally, covering mosquito larvae with the films protected the shape of the organism and kept them alive under the high vacuum conditions in a field emission-scanning electron microscope. Our method will be useful for numerous applications, particularly in the biological sciences. PMID:24236023

  12. A simple and sensitive method for the determination of hydroxylamine in fresh-water samples using hypochlorite followed by gas chromatography.

    PubMed

    Seike, Yasushi; Fukumori, Ryoko; Senga, Yukiko; Oka, Hiroki; Fujinaga, Kaoru; Okumura, Minoru

    2004-01-01

    A new and simple method for the determination of hydroxylamine in environmental water, such as fresh rivers and lakes using hypochlorite, followed by its gas choromatographic detection, has been developed. A glass vial filled with sample water was sealed by a butyl-rubber stopper and aluminum cap without head-space, and then sodium hypochlorite solution was injected into the vial through a syringe to convert hydroxylamine to nitrous oxide. The head-space in the glass vial was prepared with 99.9% grade N2 using a gas-tight syringe. After the glass vial was shaken for a few minutes, nitrous oxide in the gas-phase was measured by a gas chromatograph with an electron-capture detector. The dissolved nitrous oxide in the liquid-phase was calculated according to the solubility formula. The proposed method was applied to the analysis of fresh-water samples taken from Iu river and Hii river, flowing into brackish Lakes Nakaumi and Shinji, respectively.

  13. Antibacterial Activity Of ternary semiconductor compounds AgInSe2 Nanoparticles Synthesized by Simple Chemical Method

    NASA Astrophysics Data System (ADS)

    Shehab, A. A.; Fadaam, S. A.; Abd, A. N.; Mustafa, M. H.

    2018-05-01

    In this objective AgInSe2Nanoparticles (AgInSe2 NPs) were prepared by a simple chemical method (SCM). The optica structural l and morphological properties of the synthesized AgInSe2 NPs swere investigated by using UVVI absorption atomic force microscopy AFMmf, Fourier Transform Infrared Spectroscopy and x-ray diffraction. The resistance of bacteria represents a trouble and the outlook for the use of antibiotics in the future until now uncertain. Measures must be taken to decrease this problem. Antibacterial activity of the AgInSe2 nanoparticles were exposed against several pathogenic bacteriaa including Klebsiella pneumonia KPa, Staphylococcus aureus, Bacillus subtili, Enterobacter Cloacae and Esherichia Coliby. Using a good spread method the results showed that AgInSe2 NPs had inhibitory effect versus some pathogenic bacteria with suppression area 18, 14 and 17 mm for SAgInSe2 NPs had an inhibitory effect against S Bacillus Subtilis 11 mm K EnterobactercCloacae 12 mm.

  14. Development of a novel and simple method to evaluate disintegration of rapidly disintegrating tablets.

    PubMed

    Hoashi, Yohei; Tozuka, Yuichi; Takeuchi, Hirofumi

    2013-01-01

    The purpose of this study was to develop and test a novel and simple method for evaluating the disintegration time of rapidly disintegrating tablets (RDTs) in vitro, since the conventional disintegration test described in the pharmacopoeia produces poor results due to the difference of its environmental conditions from those of an actual oral cavity. Six RDTs prepared in our laboratory and 5 types of commercial RDTs were used as model formulations. Using our original apparatus, a good correlation was observed between in vivo and in vitro disintegration times by adjusting the height from which the solution was dropped to 8 cm and the weight of the load to 10 or 20 g. Properties of RDTs, such as the pattern of their disintegrating process, can be assessed by verifying the load. These findings confirmed that our proposed method for an in vitro disintegration test apparatus is an excellent one for estimating disintegration time and the disintegration profile of RDTs.

  15. Synthesis of stable ZnO nanocolloids with enhanced optical limiting properties via simple solution method

    NASA Astrophysics Data System (ADS)

    Ramya, M.; Nideep, T. K.; Vijesh, K. R.; Nampoori, V. P. N.; Kailasnath, M.

    2018-07-01

    In present work, we report the synthesis of stable ZnO nanocolloids through a simple solution method which exhibit enhanced optical limiting threshold. The influences of reaction temperature on the crystal structure as well as linear and nonlinear optical properties of prepared ZnO nanoparticles were carried out. The XRD and Raman analysis reveal that the prepared ZnO nanoparticles retain the hexagonal wurtzite crystal structure. HRTEM analysis confirms the effect of reaction temperature, solvent effect on crystallinity as well as nanostructure of ZnO nanoparticles. It has been found that crystallinity and average diameter increase with reaction temperature where ethylene glycol act as both solvent and growth inhibiter. EDS spectra shows formation of pure ZnO nanoparticles. The direct energy band gap of the nanoparticles increases with decrease in particle size due to quantum confinement effect. The third order nonlinear optical properties of ZnO nanoparticles were investigated by z scan technique using a frequency doubled Nd-YAG nanosecond laser at 532 nm wavelength. The z-scan result reveals that the prepared ZnO nanoparticles exhibit self - defocusing nonlinearity. The two photon absorption coefficient and third - order nonlinear optical susceptibility increases with increasing particle size. The third-order susceptibility of the ZnO nanoparticles is found to be in the order of 10-10 esu, which is at least three order magnitude greater than the bulk ZnO. The optical limiting threshold of the nanoparticles varies in the range of 54 to 17 MW/cm2. The results suggest that ZnO nanoparticles considered as a promising candidates for the future photonic devices.

  16. [Studies on hydroxyapatite applicatied in coprecipitate of total salvianolic acids phospholipid complex].

    PubMed

    Chen, Xiao-Yun; Zhang, Zhen-Hai; Liu, Dan; Sun, E; Jia, Xiao-Bin

    2014-03-01

    The purpose of this research was to prepare total salvianolic acids-phytosome-HA coprecipitate to improve drug dissolution and its micromeritic properties. Firstly, the coprecipitate was prepared by solvent method and in vitro dissolution of tripterine was performed with the salvianolic acid B and danshensu as criteria. At the same time, the micromeritic properties was characterizated, the structure of samples was characterized by TEM, DSC, XRD and FTIR. Results showed that when the ratio of drug to HA was 1:2, it had a better dissolution, the accumulative drug-release percent in vitro at 60 min was over 90%. At the same time, it has good liquidity and low moisture absorption. Its micromeritic properties have improved. It is proved that the drug still existed amorphously by microstructure analysis. The preparation process is simple and feasible, it has practical value.

  17. In situ generation of highly dispersed metal nanoparticles on two-dimensional layered SiO2 by topotactic structure conversion and their superior catalytic activity

    NASA Astrophysics Data System (ADS)

    Chen, Zhe; Jia, Da-Shuang; Zhou, Yue; Hao, Jiang; Liang, Yu; Cui, Zhi-Min; Song, Wei-Guo

    2018-03-01

    Metal nanoparticles such as Ag, Cu and Fe are effective catalysts for many reactions, whereas a facile method to prepare metal nanoparticles with high uniformed dispersion is still desirable. Herein, the topotactic structure conversion of layered silicate, RUB-15, was utilized to support metal nanoparticles. Through simple ion-exchange and following calcination step, metal nanoparticles were generated in situ inside the interlayer space of layered silica, and the topotactic structure conversion process assured nano-sized and highly uniformed dispersion of metal nanoparticles. The obtained Ag/SiO2 composite showed superior catalytic activity for the reduction of 4-nitrophenol (4-NP) and methylene blue (MB), with a rate constant as high as 0.0607 s-1 and 0.0778 s-1. The simple and universal synthesis method as well as high activity of the product composite endow the strategy good application prospect.

  18. Electrospray-deposition of graphene electrodes: a simple technique to build high-performance supercapacitors.

    PubMed

    Tang, Huaichao; Yang, Cheng; Lin, Ziyin; Yang, Quanhong; Kang, Feiyu; Wong, Ching Ping

    2015-05-28

    Here we report an electrostatic spray deposition method to prepare three-dimensional porous graphene electrodes for supercapacitor applications. The symmetric supercapacitor exhibits excellent specific capacitance (366 F g(-1) at 1 A g(-1) in 6 M KOH) and long cycle life (108% capacitance retention up to 40 000 cycles). Moreover, the energy densities of the organic and aqueous electrolyte based supercapacitors reach 22.9 and 8.1 Wh kg(-1) when the power densities are 119.2 and 15.4 kW kg(-1), respectively. Compared with the previously reported graphene based supercapacitors, the improved properties could be attributed to the excellent three-dimensional open porous electrode structure, which is favorable for the ion diffusion and electron transport. In addition, this method provides a simple electrode-fabrication route without the involvement of conducting additives and binders. It may find vast applications in thin and miniaturized energy storage scenarios.

  19. A simple method of fabricating mask-free microfluidic devices for biological analysis

    PubMed Central

    Yi, Xin; Kodzius, Rimantas; Gong, Xiuqing; Xiao, Kang; Wen, Weijia

    2010-01-01

    We report a simple, low-cost, rapid, and mask-free method to fabricate two-dimensional (2D) and three-dimensional (3D) microfluidic chip for biological analysis researches. In this fabrication process, a laser system is used to cut through paper to form intricate patterns and differently configured channels for specific purposes. Bonded with cyanoacrylate-based resin, the prepared paper sheet is sandwiched between glass slides (hydrophilic) or polymer-based plates (hydrophobic) to obtain a multilayer structure. In order to examine the chip’s biocompatibility and applicability, protein concentration was measured while DNA capillary electrophoresis was carried out, and both of them show positive results. With the utilization of direct laser cutting and one-step gas-sacrificing techniques, the whole fabrication processes for complicated 2D and 3D microfluidic devices are shorten into several minutes which make it a good alternative of poly(dimethylsiloxane) microfluidic chips used in biological analysis researches. PMID:20890452

  20. Comprehensive planning of data archive in Japanese planetary missions

    NASA Astrophysics Data System (ADS)

    Yamamoto, Yukio; Shinohara, Iku; Hoshino, Hirokazu; Tateno, Naoki; Hareyama, Makoto; Okada, Naoki; Ebisawa, Ken

    Comprehensive planning of data archive in Japanese planetary missions Japan Aerospace Exploration Agency (JAXA) provides HAYABUSA and KAGUYA data as planetary data archives. These data archives, however, were prepared independently. Therefore the inconsistency of data format has occurred, and the knowledge of data archiving activity is not inherited. Recently, the discussion of comprehensive planning of data archive has started to prepare up-coming planetary missions, which indicates the comprehensive plan of data archive is required in several steps. The framework of the comprehensive plan is divided into four items: Preparation, Evaluation, Preservation, and Service. 1. PREPARATION FRAMEWORK Data is classified into several types: raw data, level-0, 1, 2 processing data, ancillary data, and etc. The task of mission data preparation is responsible for instrument teams, but preparations beside mission data and support of data management are essential to make unified conventions and formats over instruments in a mission, and over missions. 2. EVALUATION FRAMEWORK There are two meanings of evaluation: format and quality. The format evaluation is often discussed in the preparation framework. The data quality evaluation which is often called quality assurance (QA) or quality control (QC) must be performed by third party apart from preparation teams. An instrument team has the initiative for the preparation itself, and the third-party group is organized to evaluate the instrument team's activity. 3. PRESERVATION FRAMEWORK The main topic of this framework is document management, archiving structure, and simple access method. The mission produces many documents in the process of the development. Instrument de-velopment is no exception. During long-term development of a mission, many documents are obsoleted and updated repeatedly. A smart system will help instrument team to reduce some troubles of document management and archiving task. JAXA attempts to follow PDS manners to do this management since PDS has highly sophisticated archiving structure. In addition, the access method to archived data must be simple and standard well over a decade. 4. SERVICE FRAMEWORK The service framework including planetary data access protocol, PDAP, has been developed to share a stored data effectively. The sophisticated service framework will work not only for publication data, but also for low-level data. JAXA's data query services is under developed based on PDAP, which means that the low-level data can be published in the same manner as level 2 data. In this presentation, we report the detail structure of these four frameworks adopting upcoming Planet-C, Venus Climate Orbiter, mission.

  1. Electrochemical properties of Sn-based nanopowders synthesized by a pulsed wire evaporation method and effect of binder coating

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

    Ha, Jong-Keun; Song, Ju-Seok; Cho, Gyu-Bong

    Highlights: • Sn-based nanoparticles are fabricated by using the pulsed wire evaporation method. • The electrodes are prepared by mixing the graphene and coating the surface. • Coating the surface of electrode is used with brushing of simple and facile method. • The electrochemical measurements are performed with galvanostatic experiments. • The coating electrode maintains capacity nearly of 501 mAh g{sup −1} up to 100 cycles. - Abstract: Sn-based nanoparticles are prepared with the O{sub 2} concentrations in chamber of Ar atmosphere (by v/v) by using the pulsed wire evaporation (PWE) method. The prepared electrodes are only Sn-based powder electrode,more » its binder coating electrode and Sn-based powder/graphene nanocomposite electrode. Morphology and structure of the synthesized powders and electrodes are investigated with a field emission scanning electron microscope (FE-SEM) and an X-ray diffraction (XRD) analysis. The electrochemical measurements were performed with galvanostatic cycling experiments using a coin type cell of CR2032 (Ø20, T3.2 mm). The binder coating electrode is superior to others and maintains delithiation capacity nearly of 501 mAh g{sup −1} as 58.3% of first delithiation capacity at 0.2 C-rate up to 100 cycles.« less

  2. Preparation and characterization of two new forced degradation products of letrozole and development of a stability-indicating RP-LC method for its determination.

    PubMed

    Elkady, Ehab Farouk; Fouad, Marwa Ahmed

    2015-11-01

    Two new hydrolytic products of letrozole were identified and proved to be true degradation products obtained by alkaline and acidic degradation of the drug. The acid and amide forms of the nitrile groups of letrozole were prepared and identified by IR and mass spectroscopic techniques. Subsequently, a simple, precise and selective stability-indicating RPLC method was developed and validated for the determination of letrozole in the presence of its degradation products. Letrozole was subjected to alkali and acid hydrolysis, oxidation, thermal degradation and photo-degradation. The degradation products were well isolated from letrozole. The chromatographic method was achieved using gradient elution of the drug and its degradation products on a reversed phase Zorbax Eclipse C18 column (100mm x 4.6mm, 3.5 μm) using a mobile phase consisting of 0.01M KH₂PO₄and methanol at a flow rate of 1 mL min⁻¹. Quantitation was achieved with UV detection at 230 nm. Linearity, accuracy and precision were found to be acceptable over the concentration range of 0.01-80 μgmL⁻¹. The proposed method was successfully applied to the determination of letrozole in bulk, plasma and in its pharmaceutical preparation.

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

    PubMed

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

    2015-01-01

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

  4. Silver/poly(vinyl alcohol) nanocomposite film prepared using water in oil microemulsion for antibacterial applications.

    PubMed

    Fatema, Ummul K; Rahman, M Muhibur; Islam, M Rakibul; Mollah, M Yousuf A; Susan, Md Abu Bin Hasan

    2018-03-15

    Water in oil microemulsion (w/o) is a simple preparative route for nanoparticles where water droplets (dispersed in continuous oil medium and stabilized by surfactants and cosurfactants) act as nanoreactors to carry out chemical reactions. If polymeric matrix is incorporated inside the core of the microemulsions, it should prevent the agglomeration of nanoparticles after separation from microemulsions. Thus polymer nanocomposite films prepared from w/o microemulsions are expected to give narrow and homogeneous size distribution of nanoparticles throughout the polymer host. Silver/poly(vinyl alcohol) (Ag/PVA) nanocomposite film was successfully prepared, for the first time, using Triton X-100 (TX-100)/1-butanol/cyclohexane/water microemulsion. Reduction of the metal salt was carried out in the core of w/o microemulsion droplets containing PVA polymeric matrix. After separation from the microemulsion, Ag/PVA nanocomposite film was then prepared by solution casting method. The antibacterial activity of the nanocomposites was tested against Gram-negative, Escherichia coli and Gram-positive, Staphylococcus aureus by agar diffusion method. Ag nanoparticles with an average diameter of 105 nm could be synthesized using PVA, whereas in the absence of PVA the nanoparticles agglomerated. The distribution of Ag nanoparticles on PVA surface of the nanocomposite film prepared using microemulsion was uniform, whereas the film prepared through in situ generation of Ag nanoparticles by chemical reduction process on PVA host showed non-uniform, coagulated, bunches of Ag nanoparticles. The film synthesized using microemulsion exhibited enhanced antibacterial efficacy compared to that prepared through in situ synthesis under the same test condition. Copyright © 2017 Elsevier Inc. All rights reserved.

  5. Preparation and stability of extemporaneous oral liquid formulations of oseltamivir using commercially available capsules.

    PubMed

    Winiarski, Aleksander P; Infeld, Martin H; Tscherne, Ronald; Bachynsky, Maria; Rucki, Richard; Nagano-Mate, Kathy

    2007-01-01

    To develop a simple, standardized method for the extemporaneous compounding of an oral liquid form of oseltamivir from commercially available Tamiflu 75 mg capsules (Roche Pharmaceuticals) and to determine the stability of oseltamivir in this preparation. Chemical and microbial stability study. Laboratory. None. Extemporaneous oral liquid formulations of oseltamivir (15 mg/mL) were prepared in Cherry Syrup (Humco) and Ora-Sweet SF (Paddock Laboratories) using methods consistent with current compounding practice in a pharmacy setting. Preparations were stored in amber glass and amber polyethyleneterephthalate bottles at 5 degrees C +/- 2 degrees C (41 degrees F +/- 4 degrees F) and 25 degrees C +/- 2 degrees C (77 degrees F +/- 4 degrees F) at 60% +/- 5% relative humidity (RH) for 35 days and 30 degrees C +/- 2 degrees C (86 degrees F +/- 4 degrees F) at 65% +/- 5% RH for 13 days. Samples were monitored for appearance, pH, assay, degradation products, and microbiologic stability. The Cherry Syrup preparation, in either bottle type, was stable for up to 35 days under refrigeration (5 degrees C) and up to 5 days at room temperature (25 degrees C). It was not stable when stored at 30 degrees C for 5 days. The Ora-Sweet SF preparation was stable for up to 35 days at 5 degrees C or 25 degrees C and for up to 13 days at 30 degrees C in either bottle type. Both preparations maintained microbiologic stability for 35 days. Both preparations are stable under the described conditions and may provide an option in situations where the marketed suspension is unavailable.

  6. Black silicon with self-cleaning surface prepared by wetting processes

    PubMed Central

    2013-01-01

    This paper reports on a simple method to prepare a hydrophobic surface on black silicon, which is fabricated by metal-assisted wet etching. To increase the reaction rate, the reaction device was placed in a heat collection-constant temperature type magnetic stirrer and set at room temperature. It was demonstrated that the micro- and nanoscale spikes on the black silicon made the surface become hydrophobic. As the reaction rate increases, the surface hydrophobicity becomes more outstanding and presents self-cleaning until the very end. The reflectance of the black silicon is drastically suppressed over a broad spectral range due to the unique geometry, which is effective for the enhancement of absorption. PMID:23941184

  7. The Synthesis and Photoluminescent Properties of CaMoO₄:Eu³⁺ Nanocrystals by a Soft Chemical Route.

    PubMed

    Li, Fuhai; Yu, Lixin; Sun, Jiaju; Li, Songchu; Wei, Shuilin

    2017-04-01

    In this paper, the CaMoO4:Eu3+ phosphors were prepared by a simple hydrothermal method assisted by the citric acid as the surfactant, and characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and fluorescent spectrophotometry. The results of XRD show that the as-prepared samples are single phase. The process of the Ostwald ripening is controlled by the content of the citric acid in the hydrothermal reaction. The pH value of the precursor affects the shift of the charge transition band (CTB) in the excitation spectra. The reaction condition can strongly affect the luminescent intensity of the samples.

  8. A facile route to synthesize nanogels doped with silver nanoparticles

    NASA Astrophysics Data System (ADS)

    Coll Ferrer, M. Carme; Ferrier, Robert C.; Eckmann, David M.; Composto, Russell J.

    2013-01-01

    In this study, we describe a simple method to prepare hybrid nanogels consisting of a biocompatible core-shell polymer host containing silver nanoparticles. First, the nanogels (NG, 160 nm) containing a lysozyme rich core and a dextran rich shell, are prepared via Maillard and heat-gelation reactions. Second, silver nanoparticles (Ag NPs, 5 nm) are synthesized "in situ" in the NG solution without requiring additional reducing agents. This approach leads to stable Ag NPs located in the NG. Furthermore, we demonstrate that the amount of Ag NPs in the NG can be tuned by varying silver precursor concentration. Hybrid nanogels with silver nanoparticles have potential in antimicrobial, optical, and therapeutic applications.

  9. Multifunctional transparent ZnO nanorod films.

    PubMed

    Kwak, Geunjae; Jung, Sungmook; Yong, Kijung

    2011-03-18

    Transparent ZnO nanorod (NR) films that exhibit extreme wetting states (either superhydrophilicity or superhydrophobicity through surface chemical modification), high transmittance, UV protection and antireflection have been prepared via the facile ammonia hydrothermal method. The periodic 1D ZnO NR arrays showed extreme wetting states as well as antireflection properties due to their unique surface structure and prevented the UVA region from penetrating the substrate due to the unique material property of ZnO. Because of the simple, time-efficient and low temperature preparation process, ZnO NR films with useful functionalities are promising for fabrication of highly light transmissive, antireflective, UV protective, antifogging and self-cleaning optical materials to be used for optical devices and photovoltaic energy devices.

  10. Synthesis of highly nanoporous YBO3 architecture via a co-precipitation approach and tunable luminescent properties.

    PubMed

    Liu, Lili; Zhang, Xianwen; Chaudhuri, Jharna

    2015-01-01

    We present a simple co-precipitation method to prepare highly nanoporous YBO(3) architecture using NaBO(3) ·  4H(2)O as a boric source and 600°C as the annealing temperature. The reaction was carried out under an aqueous condition without any organic solvent, surfactant, or catalysts. The prepared samples were characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The photoluminescence of doped-nanoporous YBO(3):Eu(3+) was further investigated. It is expected that highly nanoporous YBO(3) architecture can be an ideal candidate for applications in catalysis, adsorption, and optoelectronic devices. © Wiley Periodicals, Inc.

  11. Touch imprint cytology with massively parallel sequencing (TIC-seq): a simple and rapid method to snapshot genetic alterations in tumors.

    PubMed

    Amemiya, Kenji; Hirotsu, Yosuke; Goto, Taichiro; Nakagomi, Hiroshi; Mochizuki, Hitoshi; Oyama, Toshio; Omata, Masao

    2016-12-01

    Identifying genetic alterations in tumors is critical for molecular targeting of therapy. In the clinical setting, formalin-fixed paraffin-embedded (FFPE) tissue is usually employed for genetic analysis. However, DNA extracted from FFPE tissue is often not suitable for analysis because of its low levels and poor quality. Additionally, FFPE sample preparation is time-consuming. To provide early treatment for cancer patients, a more rapid and robust method is required for precision medicine. We present a simple method for genetic analysis, called touch imprint cytology combined with massively paralleled sequencing (touch imprint cytology [TIC]-seq), to detect somatic mutations in tumors. We prepared FFPE tissues and TIC specimens from tumors in nine lung cancer patients and one patient with breast cancer. We found that the quality and quantity of TIC DNA was higher than that of FFPE DNA, which requires microdissection to enrich DNA from target tissues. Targeted sequencing using a next-generation sequencer obtained sufficient sequence data using TIC DNA. Most (92%) somatic mutations in lung primary tumors were found to be consistent between TIC and FFPE DNA. We also applied TIC DNA to primary and metastatic tumor tissues to analyze tumor heterogeneity in a breast cancer patient, and showed that common and distinct mutations among primary and metastatic sites could be classified into two distinct histological subtypes. TIC-seq is an alternative and feasible method to analyze genomic alterations in tumors by simply touching the cut surface of specimens to slides. © 2016 The Authors. Cancer Medicine published by John Wiley & Sons Ltd.

  12. Adsorption dynamics of methyl violet onto granulated mesoporous carbon: Facile synthesis and adsorption kinetics.

    PubMed

    Kim, Yohan; Bae, Jiyeol; Park, Hosik; Suh, Jeong-Kwon; You, Young-Woo; Choi, Heechul

    2016-09-15

    A new and facile one-step synthesis method for preparing granulated mesoporous carbon (GMC) with three-dimensional spherical mesoporous symmetry is prepared to remove large molecular weight organic compounds in aqueous phase. GMC is synthesized in a single step using as-synthesized mesoporous carbon particles and organic binders through a simple and economical synthesis approach involving a simultaneous calcination and carbonization process. Characterization results obtained from SEM, XRD, as well as surface and porosity analysis indicate that the synthesized GMC has similar physical properties to those of the powdered mesoporous carbon and maintains the Brunauer-Emmett-Teller (BET) surface area and pore volume because the new synthesis method prevents the collapse of the pores during the granulation process. Batch adsorption experiments revealed GMC showed a substantial adsorption capacity (202.8 mg/g) for the removal of methyl violet as a target large molecular contaminant in aqueous phase. The mechanisms and dynamics modeling of GMC adsorption were also fully examined, which revealed that surface diffusion was rate limiting step on adsorption process of GMC. Adsorption kinetics of GMC enables 3 times faster than that of granular activated carbon in terms of surface diffusion coefficient. This is the first study, to the best of our knowledge, to synthesize GMC as an adsorbent for water purification by using facile granulation method and to investigate the adsorption kinetics and characteristics of GMC. This study introduces a new and simple method for the synthesis of GMC and reveals its adsorption characteristics for large molecular compounds in a water treatment. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Raman study of TiO2 coatings modified by UV pulsed laser

    NASA Astrophysics Data System (ADS)

    Belka, Radosław; Keczkowska, Justyna; Sek, Piotr

    2016-12-01

    The TiO2 coatings were prepared by simple sol-gel method and modified by UV pulsed laser. TiO2, also know as titania, is a ceramic compound, existing in numerous polymorphic forms, mainly as tetragonal rutile and anatase, and rhomboidal brookite. Rutile is the most stable form of titanium dioxide, whereas anatase is a metastable form, created in lower temperatures than rutile. Anatase is marked with higher specific surface area, porosity and a higher number of surface hydroxyl groups as compared to rutile. The unique optical and electronic properties of TiO2 results in its use as semiconductors dielectric mirrors, sunscreen and UV-blocking pigments and especially as photocatalyst. In this paper, the tetraisopropoxide was used as Ti precursor according to sol-gel method. An organic base was applied during sol preparation. Prepared gel was coated on glass substrates and calcined in low temperature to obtain amorphous phase of titania. Prepared coatings were modified by UV picosecond pulse laser with different pulse repetition rate and pulse power. Physical modification of the coatings using laser pulses was intended in order change the phase content of the produced material. Raman spectroscopy (RS) method was applied to studies of modified coatings as it is one of the basic analytical techniques, supporting the identification of compounds and obtaining information about the structure. Especially, RS is a useful method for distinguishing the anatase and rutile phases. In these studies, anatase to rutile transformation was observed, depending on laser parameters.

  14. Simple Approach for the Rapid Detection of Alternariol in Pear Fruit by Surface-Enhanced Raman Scattering with Pyridine-Modified Silver Nanoparticles.

    PubMed

    Pan, Ting-Tiao; Sun, Da-Wen; Pu, Hongbin; Wei, Qingyi

    2018-03-07

    A simple method based on surface-enhanced Raman scattering (SERS) was developed for the rapid determination of alternariol (AOH) in pear fruits using an easily prepared silver-nanoparticle (AgNP) substrate. The AgNP substrate was modified by pyridine to circumvent the weak affinity of the AOH molecules to the silver surface and to improve the sensitivity of detection. Quantitative analysis was performed in AOH solutions at concentrations ranging from 3.16 to 316.0 μg/L, and the limit of detection was 1.30 μg/L. The novel method was also applied to the detection of AOH residues in pear fruits purchased from the market and in pear fruits that were artificially inoculated with Alternaria alternata. AOH was not found in any of the fresh fruit, whereas it resided in the rotten and inoculated fruits. Finally, the SERS method was cross validated against HPLC. It was revealed that the SERS method has great potential utility in the rapid detection of AOH in pear fruits and other agricultural products.

  15. A simple and selective method for determination of phthalate biomarkers in vegetable samples by high pressure liquid chromatography-electrospray ionization-tandem mass spectrometry.

    PubMed

    Zhou, Xi; Cui, Kunyan; Zeng, Feng; Li, Shoucong; Zeng, Zunxiang

    2016-06-01

    In the present study, solid-phase extraction cartridges including silica reversed-phase Isolute C18, polymeric reversed-phase Oasis HLB and mixed-mode anion-exchange Oasis MAX, and liquid-liquid extractions with ethyl acetate, n-hexane, dichloromethane and its mixtures were compared for clean-up of phthalate monoesters from vegetable samples. Best recoveries and minimised matrix effects were achieved using ethyl acetate/n-hexane liquid-liquid extraction for these target compounds. A simple and selective method, based on sample preparation by ultrasonic extraction and liquid-liquid extraction clean-up, for the determination of phthalate monoesters in vegetable samples by liquid chromatography/electrospray ionisation-tandem mass spectrometry was developed. The method detection limits for phthalate monoesters ranged from 0.013 to 0.120 ng g(-1). Good linearity (r(2)>0.991) between MQLs and 1000× MQLs was achieved. The intra- and inter-day relative standard deviation values were less than 11.8%. The method was successfully used to determine phthalate monoester metabolites in the vegetable samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

  16. Improved bacterial identification directly from urine samples with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry.

    PubMed

    Kitagawa, Koichi; Shigemura, Katsumi; Onuma, Ken-Ichiro; Nishida, Masako; Fujiwara, Mayu; Kobayashi, Saori; Yamasaki, Mika; Nakamura, Tatsuya; Yamamichi, Fukashi; Shirakawa, Toshiro; Tokimatsu, Issei; Fujisawa, Masato

    2018-03-01

    Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) contributes to rapid identification of pathogens in the clinic but has not yet performed especially well for Gram-positive cocci (GPC) causing complicated urinary tract infection (UTI). The goal of this study was to investigate the possible clinical use of MALDI-TOF MS as a rapid method for bacterial identification directly from urine in complicated UTI. MALDI-TOF MS was applied to urine samples gathered from 142 suspected complicated UTI patients in 2015-2017. We modified the standard procedure (Method 1) for sample preparation by adding an initial 10 minutes of ultrasonication followed by centrifugation at 500 g for 1 minutes to remove debris such as epithelial cells and leukocytes from the urine (Method 2). In 133 urine culture-positive bacteria, the rate of corresponded with urine culture in GPC by MALDI-TOF MS in urine with standard sample preparation (Method 1) was 16.7%, but the modified sample preparation (Method 2) significantly improved that rate to 52.2% (P=.045). Method 2 also improved the identification accuracy for Gram-negative rods (GNR) from 77.1% to 94.2% (P=.022). The modified Method 2 significantly improved the average MALDI score from 1.408±0.153 to 2.166±0.045 (P=.000) for GPC and slightly improved the score from 2.107±0.061 to 2.164±0.037 for GNR. The modified sample preparation for MALDI-TOF MS can improve identification accuracy for complicated UTI causative bacteria. This simple modification offers a rapid and accurate routine diagnosis for UTI, and may possibly be a substitute for urine cultures. © 2017 Wiley Periodicals, Inc.

  17. Portable X-ray fluorescence spectroscopy as a rapid screening technique for analysis of TiO2 and ZnO in sunscreens.

    PubMed

    Bairi, Venu Gopal; Lim, Jin-Hee; Quevedo, Ivan R; Mudalige, Thilak K; Linder, Sean W

    2016-02-01

    This investigation reports a rapid and simple screening technique for the quantification of titanium and zinc in commercial sunscreens using portable X-ray fluorescence spectroscopy (pXRF). A highly evolved technique, inductively coupled plasma-mass spectroscopy (ICP-MS) was chosen as a comparative technique to pXRF, and a good correlation (r 2 > 0.995) with acceptable variations (≤25%) in results between both techniques was observed. Analytical figures of merit such as detection limit, quantitation limit, and linear range of the method are reported for the pXRF technique. This method has a good linearity (r 2 > 0.995) for the analysis of titanium (Ti) in the range of 0.4-14.23 wt%, and zinc (Zn) in the range of 1.0-23.90 wt%. However, most commercial sunscreens contain organic ingredients, and these ingredients are known to cause matrix effects. The development of appropriate matrix matched working standards to obtain the calibration curve was found to be a major challenge for the pXRF measurements. In this study, we have overcome the matrix effect by using metal-free commercial sunscreens as a dispersing media for the preparation of working standards. An easy extension of this unique methodology for preparing working standards in different matrices was also reported. This method is simple, rapid, and cost-effective and, in comparison to conventional techniques (e.g., ICP-MS), did not generate toxic wastes during sample analysis.

  18. Portable X-ray fluorescence spectroscopy as a rapid screening technique for analysis of TiO2 and ZnO in sunscreens

    NASA Astrophysics Data System (ADS)

    Bairi, Venu Gopal; Lim, Jin-Hee; Quevedo, Ivan R.; Mudalige, Thilak K.; Linder, Sean W.

    2016-02-01

    This investigation reports a rapid and simple screening technique for the quantification of titanium and zinc in commercial sunscreens using portable X-ray fluorescence spectroscopy (pXRF). A highly evolved technique, inductively coupled plasma-mass spectroscopy (ICP-MS) was chosen as a comparative technique to pXRF, and a good correlation (r2 > 0.995) with acceptable variations (≤ 25%) in results between both techniques was observed. Analytical figures of merit such as detection limit, quantitation limit, and linear range of the method are reported for the pXRF technique. This method has a good linearity (r2 > 0.995) for the analysis of titanium (Ti) in the range of 0.4-14.23 wt%, and zinc (Zn) in the range of 1.0-23.90 wt%. However, most commercial sunscreens contain organic ingredients, and these ingredients are known to cause matrix effects. The development of appropriate matrix matched working standards to obtain the calibration curve was found to be a major challenge for the pXRF measurements. In this study, we have overcome the matrix effect by using metal-free commercial sunscreens as a dispersing media for the preparation of working standards. An easy extension of this unique methodology for preparing working standards in different matrices was also reported. This method is simple, rapid, and cost-effective and, in comparison to conventional techniques (e.g., ICP-MS), did not generate toxic wastes during sample analysis.

  19. A synthesis of fluorescent starch based on carbon nanoparticles for fingerprints detection

    NASA Astrophysics Data System (ADS)

    Li, Hongren; Guo, Xingjia; Liu, Jun; Li, Feng

    2016-10-01

    A pyrolysis method for synthesizing carbon nanoparticles (CNPs) were developed by using malic acid and ammonium oxalate as raw materials. The incorporation of a minor amount of carbon nanoparticles into starch powder imparts remarkable color-tunability. Based on this phenomenon, an environment friendly fluorescent starch powder for detecting latent fingerprints in non-porous surfaces was prepared. The fingerprints on different non-porous surfaces developed with this powder showed very good fluorescent images under ultraviolet excitation. The method using fluorescent starch powder as fluorescent marks is simple, rapid and green. Experimental results illustrated the effectiveness of proposed methods, enabling its practical applications in forensic sciences.

  20. Epitaxially Self-Assembled Alkane Layers for Graphene Electronics.

    PubMed

    Yu, Young-Jun; Lee, Gwan-Hyoung; Choi, Ji Il; Shim, Yoon Su; Lee, Chul-Ho; Kang, Seok Ju; Lee, Sunwoo; Rim, Kwang Taeg; Flynn, George W; Hone, James; Kim, Yong-Hoon; Kim, Philip; Nuckolls, Colin; Ahn, Seokhoon

    2017-02-01

    The epitaxially grown alkane layers on graphene are prepared by a simple drop-casting method and greatly reduce the environmentally driven doping and charge impurities in graphene. Multiscale simulation studies show that this enhancement of charge homogeneity in graphene originates from the lifting of graphene from the SiO 2 surface toward the well-ordered and rigid alkane self-assembled layers. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Synthesis of Perfluorinated Ethers by Solution Phase Direct Fluorination: An Adaptation of the La-Mar Technique

    DTIC Science & Technology

    1990-08-22

    Six of the 3 perfluorinated ethers prepared have been previously synthesized by other methods: perfluoro -5,5-bis(ethoxy- f methyl) -3,7-dioxanonane...from partially fluorinated starting material [34]. Third, as with perfluoroalkanes and simple perfluoroethers , Clark’s experimental results indicated 3...a highly branched perfluoroether ) by direct fluorination 3 in solution. Second, since some of these perfluorinated compounds had been previously

  2. Magnetically Recyclable Cufe2o4 Nanoparticles as an Efficient and Reusable Catalyst for the Green Synthesis of 2,4,6,8,10,12-Hexabenzyl-2,4,6,8,10,12-hexaazaisowurtzitane as CL-20 Explosive Precursor

    NASA Astrophysics Data System (ADS)

    Azizkhani, Vahid; Montazeri, Faezeh; Molashahi, Ebrahim; Ramazani, Ali

    2017-07-01

    Magnetic nanoparticles of copper ferrite (CuFe2O4 MNPs) have been simply prepared and applied as an efficient recyclable and reusable catalyst for the green synthesis of 2,4,6,8,10,12-hexabenzyl-2,4,6,8,10,12-hexaazatetracyclo[5.5.0.05,9.03,11]dodecane (HBIW). The structure of the synthesized pure HBIW (recrystallization from ethanol) was confirmed by using various spectral techniques like infrared (IR), 1H-NMR, 13C-NMR and some of its physical properties. The prepared catalyst was characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared (FTIR). In addition, CuFe2O4 MNPs could be reused up to seven runs without any significant loss of activity. Finally, the remarkable advantages of this method are the simple experimental procedure, shorter reaction times, simple workup, and green aspects by avoiding toxic catalysts and high yield of product.

  3. Accelerated Thermal Cycling Test of Microencapsulated Paraffin Wax/Polyaniline Made by Simple Preparation Method for Solar Thermal Energy Storage.

    PubMed

    Silakhori, Mahyar; Naghavi, Mohammad Sajad; Metselaar, Hendrik Simon Cornelis; Mahlia, Teuku Meurah Indra; Fauzi, Hadi; Mehrali, Mohammad

    2013-04-29

    Microencapsulated paraffin wax/polyaniline was prepared using a simple in situ polymerization technique, and its performance characteristics were investigated. Weight losses of samples were determined by Thermal Gravimetry Analysis (TGA). The microencapsulated samples with 23% and 49% paraffin showed less decomposition after 330 °C than with higher percentage of paraffin. These samples were then subjected to a thermal cycling test. Thermal properties of microencapsulated paraffin wax were evaluated by Differential Scanning Calorimeter (DSC). Structure stability and compatibility of core and coating materials were also tested by Fourier transform infrared spectrophotometer (FTIR), and the surface morphology of the samples are shown by Field Emission Scanning Electron Microscopy (FESEM). It has been found that the microencapsulated paraffin waxes show little change in the latent heat of fusion and melting temperature after one thousand thermal recycles. Besides, the chemical characteristics and structural profile remained constant after one thousand thermal cycling tests. Therefore, microencapsulated paraffin wax/polyaniline is a stable material that can be used for thermal energy storage systems.

  4. Simple hydrothermal synthesis of metal oxides coupled nanocomposites: Structural, optical, magnetic and photocatalytic studies

    NASA Astrophysics Data System (ADS)

    Ganeshraja, Ayyakannu Sundaram; Clara, Antoni Samy; Rajkumar, Kanniah; Wang, Yanjie; Wang, Yu; Wang, Junhu; Anbalagan, Krishnamoorthy

    2015-10-01

    The present article is focused on recent developments toward the preparation of room temperature ferromagnetic nanocomposites using better photocatalytic performance. These nanocomposites were successfully prepared by a simple hydrothermal method and their molecular formulas were confirmed as Ti0.90Sn0.10O2 (S1), 0.2CuO-Ti0.73Sn0.06Cu0.21O2-δ (S2), and Ti0.82Sn0.09Fe0.09O2-δ (S3). The ICP, XRD, DRS, FTIR, Raman, XAFS, XPS, EPR, SEM-EDX, HRSEM, HRTEM, photoluminescence and vibrating sample magnetometric measurements were employed to characterize the phase structures, morphologies, optical and magnetic properties of the photocatalysts. The local structures of Sn4+ and Fe3+ were confirmed by 119Sn and 57Fe Mössbauer analysis. The photocatalytic activities of the samples were evaluated by the degradation of methyl orange in water under visible light irradiation. Among the samples, tin doped TiO2 (S1) showed the best photocatalytic performance and stability.

  5. Application of glucose as a green capping agent and reductant to fabricate CuI micro/nanostructures

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

    Tavakoli, Farnosh; Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir; Ghanbari, Davood

    Graphical abstract: - Highlights: • CuI nanostructures were prepared via a simple precipitation method. • Glucose as a green capping agent and reductant was applied. • The effect of glucose concentration on the morphology of CuI was investigated. • According to XRD results, pure cubic phase CuI have been formed by using glucose. - Abstract: In this work, CuI micro/nanostructures have been successfully prepared via a simple precipitation route at room temperature. By using glucose as a clean reducing agent with different concentrations, CuI micro/nanostructures with various morphologies were obtained. Besides glucose, Na{sub 2}SO{sub 3}, KBH{sub 4} and N{sub 2}H{submore » 4}·H{sub 2}O have been applied as reductant. X-ray diffraction (XRD), scanning electron microscopy (SEM), photoluminescence spectroscopy, X-ray energy dispersive spectroscopy (EDS) and Fourier transformed infrared (FT-IR) spectroscopy were used to characterize the as-produced CuI micro/nanostructures. According to the XRD results, it was found that pure cubic phase CuI have been formed by using glucose.« less

  6. Stability of Metronidazole Suspensions.

    PubMed

    Donnelly, Ronald F; Ying, James

    2015-01-01

    Metronidazole is an antiprotozoal agent used in the treatment of bacterial and protozoal anaerobic infections. The objectives of this study were to develop concentrated metronidazole suspensions that are inexpensive and easy to prepare and determine the stability of these suspensions after storage in amber polyvinyl chloride bottles at room temperature (23°C) and under refrigeration (5°C). Metronidazole suspensions (50 mg/mL) were prepared from powder using Ora-Blend or simple syrup as the vehicles. Samples were collected in triplicate from each container on days 0, 7, 14, 28, 56, and 93. Samples were assayed using a high-performance liquid chromatography method that had been validated as stability indicating. Color, change in physical appearance, and pH were also monitored at each time interval. There was no apparent change in color or physical appearance. The pH values changed by less than 0.20 units over the 93 days. The stability of metronidazole suspensions compounded from United States Pharmacopeia powder using Ora-Blend or simple syrup and packaged in amber polyvinyl chloride bottles was determined to be 93 days when stored at either room temperature or under refrigeration.

  7. Accelerated Thermal Cycling Test of Microencapsulated Paraffin Wax/Polyaniline Made by Simple Preparation Method for Solar Thermal Energy Storage

    PubMed Central

    Silakhori, Mahyar; Naghavi, Mohammad Sajad; Metselaar, Hendrik Simon Cornelis; Mahlia, Teuku Meurah Indra; Fauzi, Hadi; Mehrali, Mohammad

    2013-01-01

    Microencapsulated paraffin wax/polyaniline was prepared using a simple in situ polymerization technique, and its performance characteristics were investigated. Weight losses of samples were determined by Thermal Gravimetry Analysis (TGA). The microencapsulated samples with 23% and 49% paraffin showed less decomposition after 330 °C than with higher percentage of paraffin. These samples were then subjected to a thermal cycling test. Thermal properties of microencapsulated paraffin wax were evaluated by Differential Scanning Calorimeter (DSC). Structure stability and compatibility of core and coating materials were also tested by Fourier transform infrared spectrophotometer (FTIR), and the surface morphology of the samples are shown by Field Emission Scanning Electron Microscopy (FESEM). It has been found that the microencapsulated paraffin waxes show little change in the latent heat of fusion and melting temperature after one thousand thermal recycles. Besides, the chemical characteristics and structural profile remained constant after one thousand thermal cycling tests. Therefore, microencapsulated paraffin wax/polyaniline is a stable material that can be used for thermal energy storage systems. PMID:28809232

  8. Real-time fluorescence loop mediated isothermal amplification for the diagnosis of malaria.

    PubMed

    Lucchi, Naomi W; Demas, Allison; Narayanan, Jothikumar; Sumari, Deborah; Kabanywanyi, Abdunoor; Kachur, S Patrick; Barnwell, John W; Udhayakumar, Venkatachalam

    2010-10-29

    Molecular diagnostic methods can complement existing tools to improve the diagnosis of malaria. However, they require good laboratory infrastructure thereby restricting their use to reference laboratories and research studies. Therefore, adopting molecular tools for routine use in malaria endemic countries will require simpler molecular platforms. The recently developed loop-mediated isothermal amplification (LAMP) method is relatively simple and can be improved for better use in endemic countries. In this study, we attempted to improve this method for malaria diagnosis by using a simple and portable device capable of performing both the amplification and detection (by fluorescence) of LAMP in one platform. We refer to this as the RealAmp method. Published genus-specific primers were used to test the utility of this method. DNA derived from different species of malaria parasites was used for the initial characterization. Clinical samples of P. falciparum were used to determine the sensitivity and specificity of this system compared to microscopy and a nested PCR method. Additionally, directly boiled parasite preparations were compared with a conventional DNA isolation method. The RealAmp method was found to be simple and allowed real-time detection of DNA amplification. The time to amplification varied but was generally less than 60 minutes. All human-infecting Plasmodium species were detected. The sensitivity and specificity of RealAmp in detecting P. falciparum was 96.7% and 91.7% respectively, compared to microscopy and 98.9% and 100% respectively, compared to a standard nested PCR method. In addition, this method consistently detected P. falciparum from directly boiled blood samples. This RealAmp method has great potential as a field usable molecular tool for diagnosis of malaria. This tool can provide an alternative to conventional PCR based diagnostic methods for field use in clinical and operational programs.

  9. Mean centering of ratio spectra and concentration augmented classical least squares in a comparative approach for quantitation of spectrally overlapped bands of antihypertensives in formulations

    NASA Astrophysics Data System (ADS)

    Hegazy, Maha Abdel Monem; Fayez, Yasmin Mohammed

    2015-04-01

    Two different methods manipulating spectrophotometric data have been developed, validated and compared. One is capable of removing the signal of any interfering components at the selected wavelength of the component of interest (univariate). The other includes more variables and extracts maximum information to determine the component of interest in the presence of other components (multivariate). The applied methods are smart, simple, accurate, sensitive, precise and capable of determination of spectrally overlapped antihypertensives; hydrochlorothiazide (HCT), irbesartan (IRB) and candesartan (CAN). Mean centering of ratio spectra (MCR) and concentration residual augmented classical least-squares method (CRACLS) were developed and their efficiency was compared. CRACLS is a simple method that is capable of extracting the pure spectral profiles of each component in a mixture. Correlation was calculated between the estimated and pure spectra and was found to be 0.9998, 0.9987 and 0.9992 for HCT, IRB and CAN, respectively. The methods were successfully determined the three components in bulk powder, laboratory-prepared mixtures, and combined dosage forms. The results obtained were compared statistically with each other and to those of the official methods.

  10. Prepare Healthy Foods with Toddlers

    ERIC Educational Resources Information Center

    Izumi-Taylor, Satomi; Rike, Cheryl

    2011-01-01

    Toddlers--from about 16 to 36 months--can learn a variety of skills as they prepare food and follow recipes in developmentally appropriate ways. Early childhood teachers are encouraged to support young children's healthy eating habits by offering simple food preparation experiences. When toddlers--and preschoolers--safely prepare healthy snacks,…

  11. Development and characterization of a mucoadhesive sublingual formulation for pain control: extemporaneous oxycodone films in personalized therapy.

    PubMed

    Parodi, Brunella; Russo, Eleonora; Baldassari, Sara; Zuccari, Guendalina; Pastorino, Sara; Yan, Mengying; Neduri, Karthik; Caviglioli, Gabriele

    2017-06-01

    The aim of this work was the development of mucoadhesive sublingual films, prepared using a casting method, for the administration of oxycodone. A solvent casting method was employed to prepare the mucoadhesive films. A calibrated pipette was used to deposit single aliquots of different polymeric solutions on a polystyrene plate lid. Among the various tested polymers, hydroxypropylcellulose at low and medium molecular weight (HPC) and pectin at two different degrees of esterification (PC) were chosen for preparing solutions with good casting properties, capable of producing films suitable for mucosal application. The obtained films showed excellent drug content uniformity and stability and rapid drug release, which, at 8 min, ranged from 60% to 80%. All films presented satisfactory mucoadhesive and mechanical properties, also confirmed by a test on healthy volunteers, who did not experience irritation or mucosa damages. Pectin films based on pectin at lower degrees of esterification have been further evaluated to study the influence of two different amounts of drug on the physicochemical properties of the formulation. A slight reduction in elasticity has been observed in films containing a higher drug dose; nevertheless, the formulation maintained satisfactory flexibility and resistance to elongation. HPC and PC sublingual films, obtained by a simple casting method, could be proposed to realize personalized hospital pharmacy preparations on a small scale.

  12. Enhanced light extraction of plastic scintillator using large-area photonic crystal structures fabricated by hot embossing.

    PubMed

    Chen, Xueye; Liu, Bo; Wu, Qiang; Zhu, Zhichao; Zhu, Jingtao; Gu, Mu; Chen, Hong; Liu, Jinliang; Chen, Liang; Ouyang, Xiaoping

    2018-04-30

    Plastic scintillators are widely used in various radiation measurement systems. However, detection efficiency and signal-to-noise are limited due to the total internal reflection, especially for weak signal detection situations. In the present investigation, large-area photonic crystals consisting of an array of periodic truncated cone holes were prepared based on hot embossing technology aiming at coupling with the surface of plastic scintillator to improve the light extraction efficiency and directionality control. The experimental results show that a maximum enhancement of 64% at 25° emergence angle along Γ-M orientation and a maximum enhancement of 58% at 20° emergence angle along Γ-K orientation were obtained. The proposed fabrication method of photonic crystal scintillator can avoid complicated pattern transfer processes used in most traditional methods, leading to a simple, economical method for large-area preparation. The photonic crystal scintillator demonstrated in this work is of great value for practical applications of nuclear radiation detection.

  13. Preparation of Multiwalled Carbon Nanotubes/Hydroxyl-Terminated Silicone Oil Fiber and Its Application to Analysis of Crude Oils

    PubMed Central

    Tong, Ting; Zhang, Wanfeng; Dai, Wei; He, Sheng; Chang, Zhenyang; Gao, Xuanbo

    2014-01-01

    A simple and efficient method to analyze the volatile and semivolatile organic compounds in crude oils has been developed based on direct immersion solid-phase microextraction coupled to comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry (DI-SPME-GC × GC/TOFMS). A novel fiber, multiwalled carbon nanotubes/hydroxyl-terminated silicone oil (MWNTs-TSO-OH), was prepared by sol-gel technology. Using standard solutions, the extraction conditions were optimized such as extraction mode, extraction temperature, extraction time, and salts effect. With the optimized conditions, a real crude oil sample was extracted and then analyzed in detail. It shows that the proposed method is very effective in simultaneously analyzing the normal and branched alkanes, cycloalkanes, aromatic hydrocarbons, and biomarkers of crude oil such as steranes and terpanes. Furthermore, the method showed good linearity (r > 0.999), precision (RSD < 8%), and detection limits ranging from 0.2 to 1.6 ng/L. PMID:24578659

  14. Quantification of urinary zwitterionic organic acids using weak-anion exchange chromatography with tandem MS detection.

    PubMed

    Bishop, Michael Jason; Crow, Brian S; Kovalcik, Kasey D; George, Joe; Bralley, James A

    2007-04-01

    A rapid and accurate quantitative method was developed and validated for the analysis of four urinary organic acids with nitrogen containing functional groups, formiminoglutamic acid (FIGLU), pyroglutamic acid (PYRGLU), 5-hydroxyindoleacetic acid (5-HIAA), and 2-methylhippuric acid (2-METHIP) by liquid chromatography tandem mass spectrometry (LC/MS/MS). The chromatography was developed using a weak anion-exchange amino column that provided mixed-mode retention of the analytes. The elution gradient relied on changes in mobile phase pH over a concave gradient, without the use of counter-ions or concentrated salt buffers. A simple sample preparation was used, only requiring the dilution of urine prior to instrumental analysis. The method was validated based on linearity (r2>or=0.995), accuracy (85-115%), precision (C.V.<12%), sample preparation stability (

  15. Micro- and nano-porous surface patterns prepared by surface-confined directional melt crystallization of solvent

    NASA Astrophysics Data System (ADS)

    Kim, Byoung Soo; Kim, Hyun Jin; An, Suyeong; Chi, Sangwon; Kim, Junseok; Lee, Jonghwi

    2017-07-01

    Recently, numerous attempts have been made to engineer micro- and nano-porous surface patterns or to develop convenient preparation methods for the practical applications of self-cleaning surfaces, water-repellent surfaces, novel textures, etc. Herein, we introduce a simple, cheap, and repeatable crystallization-based method to produce porous surface structures, on any surface of already fabricated polymeric materials. Contact of the solvent phase with cooled polymer surfaces enabled the limited dissolution of the surfaces and the subsequent extremely fast melt crystallization of the solvent. After removing the crystals, various micro- and nano-porous patterns were obtained, whose pore sizes ranged over three orders of magnitude. Pore depth was linearly dependent on the dissolution time. Crystal growth was mainly directed normal to the surfaces, but it was also controlled in-plane, resulting in cylindrical or lamellar structures. Superhydrophobic surfaces were successfully prepared on both polystyrene and polycarbonate. This process offers a novel surface engineering tool for a variety of polymer surfaces, whose topology can be conveniently controlled over a wide range by crystal engineering.

  16. Preparation and Thermoelectric Properties of Graphite/Bi0.5Sb1.5Te3 Composites

    NASA Astrophysics Data System (ADS)

    Hu, Wenhua; Zhou, Hongyu; Mu, Xin; He, Danqi; Ji, Pengxia; Hou, Weikang; Wei, Ping; Zhu, Wanting; Nie, Xiaolei; Zhao, Wenyu

    2018-06-01

    Bismuth telluride zone-melting alloys are the most commercially used thermoelectric materials. However, the zone-melting ingots have weak machinability due to the strong preferred orientation. Here, non-textured graphite/Bi0.5Sb1.5Te3 (G/BST) composites were prepared by a powder metallurgy method combined with cold-pressing and annealing treatments. The composition, microstructure, and thermoelectric properties of the G/BST composites with different mass percentages of G were investigated. It was found that G addition could effectively reduce the thermal conductivity and slightly improve the electrical properties of the BST, which resulted in a large enhancement in the figure-of-merit, ZT. The largest ZT for the xG/BST composites with x = 0.05% reached 1.05 at 320 K, which is increased by 35% as compared with that of the G-free BST materials. This work provided an effective method for preparing non-textured Bi2Te3-based TE materials with a simple process, low cost, and large potential in scale production.

  17. Relationship between fabrication method and chemical stability of Ni-BaZr0.8Y0.2O3-δ membrane

    NASA Astrophysics Data System (ADS)

    Fang, Shumin; Wang, Siwei; Brinkman, Kyle S.; Su, Qing; Wang, Haiyan; Chen, Fanglin

    2015-03-01

    NiO effectively promotes the sintering of highly refractory Y-doped BaZrO3 (BZY) through the formation of BaY2NiO5, providing a simple and cost-effective method for the fabrication of dense BZY electrolyte and Ni-BZY hydrogen separation membrane at ∼1400 °C. Unfortunately, insulating BaCO3 and Y2O3 phases formed on the surface of BZY and Ni-BZY prepared by solid state reaction method with NiO after annealing in wet CO2. Ni-BZY membranes prepared from different methods suffered different degree of performance loss in wet H2 at 900 °C. The chemical instability of Ni-BZY is attributed to the formation of a secondary phase (BaY2O4) generated from the reduction of BaY2NiO5 in H2 during the sintering process. Both BaY2O4 and BaY2NiO5 react with H2O, and CO2 at elevated temperatures, generating insulating Ba(OH)2 and BaCO3 phases, respectively. The less BaY2O4 is formed in the fabrication process, the better chemical stability the Ni-BZY membranes possess. Therefore, a new Ni-BZY membrane is prepared through a judicial combination of BZY powders prepared from combined EDTA-citric and solid state reaction methods, and demonstrates exceptional chemical stability in H2O and CO2, enabling stable and even improved hydrogen flux in wet 50% CO2 at 900 °C.

  18. Preparation and Structural Studies on Hybrid Core-Shell Nanoparticles Consisting of Silica Core and Conjugated Block Copolymer Shell Prepared by Surface-Initiated Polymerization

    NASA Astrophysics Data System (ADS)

    Chatterjee, Sourav; Karam, Tony; Rosu, Cornelia; Li, Xin; Do, Changwoo; Youm, Sang Gil; Haber, Louis; Russo, Paul; Nesterov, Evgueni

    Controlled Kumada catalyst-transfer polymerization occurring by chain-growth mechanism was developed for the synthesis of conjugated polymers and block copolymers from the surface of inorganic substrates such as silica nanoparticles. Although synthesis of conjugated polymers via Kumada polymerization became an established method for solution polymerization, carrying out the same reaction in heterogeneous conditions to form monodisperse polymer chains still remains a challenge. We developed and described a simple and efficient approach to the preparation of surface-immobilized layer of catalytic Ni(II) initiator, and demonstrated using it to prepare polymers and block copolymers on silica nanoparticle. The structure of the resulting hybrid nanostructures was thoroughly studied using small-angle neutron and X-ray scattering, thermal analysis, and optical spectroscopy. The photoexcitation energy transfer processes in the conjugated polymer shell were studied via steady-state and time resolved transient absorption spectroscopy. This study uncovered important details of the energy transfer, which will be discussed in this presentation.

  19. Formation of N, S-codoped fluorescent carbon dots from biomass and their application for the selective detection of mercury and iron ion

    NASA Astrophysics Data System (ADS)

    Ye, Qianghua; Yan, Fanyong; Luo, Yunmei; Wang, Yinyin; Zhou, Xuguang; Chen, Li

    2017-02-01

    Biomass is regarded as an excellent candidate for the preparation of heteroatom-doped carbon nanomaterials. We have developed a simple and facile one-pot synthesis of nitrogen and sulfur codoped fluorescent carbon dots from pigeon feathers, egg and manure via the pyrolysis carbonization method. The as-prepared four PCDs have high fluorescence quantum yield about 24.87% (PCDs-f), 17.48% (PCDs-w), 16.34% (PCDs-y), 33.50% (PCDs-m), respectively, which is higher than the other carbon dots preparing from biomass. We found that the preparation of PCDs-m with pigeon manure has no favourable selectively with heavy metal ions. However, other PCDs exhibit highly sensitive and selective detection behavior of Hg2 +/Fe3 + ions with a low detection limit of 10.3 and 60.9 nM. They were applied to imaging of human umbilical vein endothelial cells, showing low cytotoxicity and good biocompatibility.

  20. 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.

  1. Artificial 3D hierarchical and isotropic porous polymeric materials

    PubMed Central

    Musteata, Valentina-Elena; Behzad, Ali Reza

    2018-01-01

    Hierarchical porous materials that replicate complex living structures are attractive for a wide variety of applications, ranging from storage and catalysis to biological and artificial systems. However, the preparation of structures with a high level of complexity and long-range order at the mesoscale and microscale is challenging. We report a simple, nonextractive, and nonreactive method used to prepare three-dimensional porous materials that mimic biological systems such as marine skeletons and honeycombs. This method exploits the concurrent occurrence of the self-assembly of block copolymers in solution and macrophase separation by nucleation and growth. We obtained a long-range order of micrometer-sized compartments. These compartments are interconnected by ordered cylindrical nanochannels. The new approach is demonstrated using polystyrene-b-poly(t-butyl acrylate), which can be further explored for a broad range of applications, such as air purification filters for viruses and pollution particle removal or growth of bioinspired materials for bone regeneration.

  2. Artificial 3D hierarchical and isotropic porous polymeric materials.

    PubMed

    Chisca, Stefan; Musteata, Valentina-Elena; Sougrat, Rachid; Behzad, Ali Reza; Nunes, Suzana P

    2018-05-01

    Hierarchical porous materials that replicate complex living structures are attractive for a wide variety of applications, ranging from storage and catalysis to biological and artificial systems. However, the preparation of structures with a high level of complexity and long-range order at the mesoscale and microscale is challenging. We report a simple, nonextractive, and nonreactive method used to prepare three-dimensional porous materials that mimic biological systems such as marine skeletons and honeycombs. This method exploits the concurrent occurrence of the self-assembly of block copolymers in solution and macrophase separation by nucleation and growth. We obtained a long-range order of micrometer-sized compartments. These compartments are interconnected by ordered cylindrical nanochannels. The new approach is demonstrated using polystyrene- b -poly( t -butyl acrylate), which can be further explored for a broad range of applications, such as air purification filters for viruses and pollution particle removal or growth of bioinspired materials for bone regeneration.

  3. Preparation and characterization of functionalized single walled carbon nanotubes (fSWCNT)/ Hydroxyapatite (HAp)-Nylon hybridized composite biomaterial to study the mechanical properties

    NASA Astrophysics Data System (ADS)

    Khanal, Suraj; Leventouri, Theodora; Mahfuz, Hassan; Rondinone, Adam

    2014-03-01

    Synthetic hydroxyapatite (HAp) bears poor mechanical properties that limit its applicability in orthopedics. We study the possibility of overcoming such limitations by incorporating functionalized single walled carbon nanotubes (fSWCNT) in a biocompatible/bioactive nano-composite. We present results from synthesis and characterization of samples prepared under different processing parameters. Ultra sonication method was to disperse functionalized single walled carbon nanotubes (fSWCNT) in HAp followed by a simple hot assorting method to incorporate with polymerized ɛ-caprolactam. The fracture toughness of the composite materials was tested in compliance with the ASTM D-5045 standard. We have found that while the fracture toughness strongly depends on the processing parameters, a value comparable to the one for cortical bone is achieved. Mechanical properties, electron microscopy and crystal structure properties of the composite materials will be discussed.

  4. Production of morphology-controllable porous hyaluronic acid particles using a spray-drying method.

    PubMed

    Iskandar, Ferry; Nandiyanto, Asep Bayu Dani; Widiyastuti, W; Young, Lee Sin; Okuyama, Kikuo; Gradon, Leon

    2009-05-01

    Hyaluronic acid (HA) porous particles with controllable porosity and pore size, ranging from 100 to 300 nm, were successfully prepared using a colloidal templating and spray-drying method. HA powder and polystyrene latex (PSL) particles, which were used as the precursor and templating agent, respectively, were mixed in aqueous solution and spray-dried using a two-fluid nozzle system to produce HA and PSL composite particles. Water was evaporated during spray-drying using heated air with a temperature of 120 degrees C. This simple process was completed within several seconds. The prepared particles were collected and washed with an organic solvent to dissolve the PSL templating agent. The porosity and pore size of the resulting particles were easily controlled by changing the initial mass ratio of precursor to templating agent, i.e., HA to PSL, and by altering the size of the PSL template particles.

  5. Structural, Optical and Magnetic Properties of Ni-Zn Ferrite Nanoparticles Prepared by a Microwave Assisted Combustion Method.

    PubMed

    Vijaya, J Judith; Bououdina, M

    2016-01-01

    Ni-doped ZnFe₂O₄(Ni(x)Zn₁₋xFe₂O₄; x = 0.0 to 0.5) nanoparticles were synthesized by a simple microwave combustion method. The X-ray diffraction confirms the presence of cubic spinel ZnFe₂O₄for all compositions. The lattice parameter decreases with an increase in Ni content resulting in the reduction of lattice strain. High resolution scanning electron microscope images revealed that the as-prepared samples are crystalline with particle size distribution in 40-50 nm range. Optical properties were determined by UV-Visible diffuse reflectance and photoluminescence spectroscopy respectively. The saturation magnetization (Ms) shows the super paramagnetic nature of the sample for x = 0.0-0.2, whereas for x = 0.3-0.5, it shows ferromagnetic nature. The Ms value is 1.638 emu/g for pure ZnFe₂O₄ sample and it increases with increase in Ni content.

  6. A simple, broad-scope nickel(0) precatalyst system for direct amination of allyl alcohols.

    PubMed

    Sweeney, Joseph B; Ball, Anthony; Lawrence, Philippa; Sinclair, Mackenzie; Smith, Luke

    2018-06-25

    The preparation of allylic amines is traditionally accomplished by reaction of amines with reactive electrophiles, such as allylic halides, sulfonates or oxyphosphonium species; such methods involve hazardous reagents, generate stoichiometric waste streams, and often suffer from side-reactions (such as over-alkylation). We report here the first nickel-catalysed direct amination of allyl alcohols which enables allylation of primary, secondary and electron-deficient amines, using an inexpensive Ni(II)-Zn couple, without need for glove-box techniques. Under mild conditions, primary and secondary aliphatic amines react smoothly with a range of allyl alcohols, giving secondary and tertiary amines efficiently. This 'totally catalytic' method can be also applied to electron-deficient nitrogen nucleophiles with effective results; the practicality of the process has been demonstrated in an efficient, gram-scale preparation of the calcium antagonist drug substance flunarizine (Sibelium®). © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Three-dimensional sulphur/nitrogen co-doped reduced graphene oxide as high-performance supercapacitor binder-free electrodes

    NASA Astrophysics Data System (ADS)

    Huo, Jinghao; Zheng, Peng; Wang, Xiaofei; Guo, Shouwu

    2018-06-01

    Sulphur/nitrogen co-doped reduced graphene oxide (SNG) aerogels were prepared by a simple solvothermal method with l-cysteine-assisted in ethylene glycol. The morphology and composition tests showed that the S/N heteroatoms were evenly distributed on SNG microsheets, and these microsheets were further composed of SNG aerogels with three-dimensional (3D) porous structure. The cyclic voltammetry and galvanostatic charge/discharge tests illustrated the SNG bind-free electrode possessed electric double-layer capacitance and pseudocapacitance, and had a capacitance of 254 F g-1 at a current density of 1 A g-1. After the 5000 cycles tests, the capacitance retained 83.54% at a current density of 2 A g-1. Meanwhile, the electrochemical impedance spectroscopy data shown the electrode materials had excellent capacity and good conductivity. Hence, the SNG aerogel prepared by l-cysteine-assisted solvothermal method is a great material for high-performance supercapacitors.

  8. Room Temperature Gas Sensing Properties of Sn-Substituted Nickel Ferrite (NiFe2O4) Thin Film Sensors Prepared by Chemical Co-Precipitation Method

    NASA Astrophysics Data System (ADS)

    Manikandan, V.; Li, Xiaogan; Mane, R. S.; Chandrasekaran, J.

    2018-04-01

    Tin (Sn) substituted nickel ferrite (NiFe2O4) thin film sensors were prepared by a simple chemical co-precipitation method, which initially characterized their structure and surface morphology with the help of x-ray diffraction and scanning electron microscopy. Surface morphology of the sensing films reveals particles stick together with nearer particles and this formation leads to a large specific area as a large specific area is very useful for easy adsorption of gas molecules. Transmission electron microscopy and selected area electron diffraction pattern images confirm particle size and nanocrystallnity as due to formation of circular rings. Fourier transform infrared analysis has supported the presence of functional groups. The 3.69 eV optical band gap of the film was found which enabled better gas sensing. Gas sensors demonstrate better response and recovery characteristics, and the maximum response was 68.43%.

  9. Biosorbents for Removing Hazardous Metals and Metalloids †

    PubMed Central

    Inoue, Katsutoshi; Parajuli, Durga; Ghimire, Kedar Nath; Biswas, Biplob Kumar; Kawakita, Hidetaka; Oshima, Tatsuya; Ohto, Keisuke

    2017-01-01

    Biosorbents for remediating aquatic environmental media polluted with hazardous heavy metals and metalloids such as Pb(II), Cr(VI), Sb(III and V), and As(III and V) were prepared from lignin waste, orange and apple juice residues, seaweed and persimmon and grape wastes using simple and cheap methods. A lignophenol gel such as lignocatechol gel was prepared by immobilizing the catechol functional groups onto lignin from sawdust, while lignosulfonate gel was prepared directly from waste liquor generated during pulp production. These gels effectively removed Pb(II). Orange and apple juice residues, which are rich in pectic acid, were easily converted using alkali (e.g., calcium hydroxide) into biosorbents that effectively removed Pb(II). These materials also effectively removed Sb(III and V) and As(III and V) when these were preloaded with multi-valent metal ions such as Zr(IV) and Fe(III). Similar biosorbents were prepared from seaweed waste, which is rich in alginic acid. Other biosorbents, which effectively removed Cr(VI), were prepared by simply treating persimmon and grape wastes with concentrated sulfuric acid. PMID:28773217

  10. Development of a Terbium-Sensitized Fluorescence Method for Analysis of Silibinin.

    PubMed

    Ershadi, Saba; Jouyban, Abolghasem; Molavi, Ommoleila; Shayanfar, Ali

    2017-05-01

    Silibinin is a natural flavonoid with potent anticancer properties, as shown in both in vitro and in vivo experiments. Various methods have been used for silibinin analysis. Terbium-sensitized fluorescence methods have been widely used for the determination of drugs in pharmaceutical preparations and biological samples in recent years. The present work is aimed at providing a simple analytical method for the quantitative determination of silibinin in aqueous solutions based on the formation of a fluorescent complex with terbium ion. Terbium concentration, pH, and volume of buffer, the important effective parameters for the determination of silibinin by the proposed method, were optimized using response surface methodology. The fluorescence intensity of silibinin was measured at 545 nm using λex = 334 nm. The developed method was applied for the determination of silibinin in plasma samples after protein precipitation with acetone. Under optimum conditions, the method provided a linear range between 0.10 and 0.50 mg/L, with a coefficient of determination (R2) of 0.997. The LOD and LOQ were 0.034 and 0.112 mg/L, respectively. These results indicate that the developed method is a simple, low-cost, and suitable analytical method for the quantification of silibinin in aqueous solution and plasma samples.

  11. 'The artist's piece is already in the stone': constructing creativity in paleontology laboratories.

    PubMed

    Wylie, Caitlin Donahue

    2015-02-01

    Laboratory technicians are typically portrayed as manual workers following routine procedures to produce scientific data. However, technicians in vertebrate paleontology laboratories often describe their work in terms of creativity and artistry. Fossil specimens undergo extensive preparation--including rock removal, damage repair, and reconstruction of missing parts--to become accessible to researchers. Technicians called 'fossil preparators' choose, apply, and sometimes invent these preparation methods. They have no formal training, no standard protocols, and few publications to consult on techniques. Despite the resulting diversity of people and practices, preparators and their work are usually absent from research publications, making them 'invisible technicians' in Steven Shapin's sense. But preparators reject the view of their work as predictable or simple; in particular, many preparators value art training, the aesthetics of prepared fossils, and the process of creative problem-solving in their work. Based on interviews and participant observation and drawing from literature in science studies, sociology of work, and anthropology of craft, I ask why these technicians compare themselves with artists and how this portrayal affects scientific practice and social order in laboratories. I argue that associating artistry and creativity with their work distances preparators from ideas of unskilled technical work and technicians' low status, thus improving their social role in the laboratory community and preserving their power over laboratory practices.

  12. Magnetron sputtering based direct fabrication of three dimensional CdTe hierarchical nanotrees exhibiting stable superhydrophobic property

    NASA Astrophysics Data System (ADS)

    Luo, Bingwei; Deng, Yuan; Wang, Yao; Shi, Yongming; Cao, Lili; Zhu, Wei

    2013-09-01

    Three dimensional CdTe hierarchical nanotrees are initially prepared by a simple one-step magnetron sputtering method without any templates or additives. The CdTe hierarchical nanotrees are constructed by the spear-like vertical trunks and horizontal branches with the diameters of about 100 nm at bottom and became cuspidal on the top. The particular nanostructure imparts these materials superhydrophobic property, and this property can be preserved after placing in air for 90 days, and is stable even after the ultraviolet light and X-ray irradiation, respectively. This study provides a simple strategy to achieve superhydrophobic properties for CdTe materials at lower temperature, which opens a new potential for CdTe solar cell with self-cleaning property.

  13. Quantification of strontium in human serum by ICP-MS using alternate analyte-free matrix and its application to a pilot bioequivalence study of two strontium ranelate oral formulations in healthy Chinese subjects.

    PubMed

    Zhang, Dan; Wang, Xiaolin; Liu, Man; Zhang, Lina; Deng, Ming; Liu, Huichen

    2015-01-01

    A rapid, sensitive and accurate ICP-MS method using alternate analyte-free matrix for calibration standards preparation and a rapid direct dilution procedure for sample preparation was developed and validated for the quantification of exogenous strontium (Sr) from the drug in human serum. Serum was prepared by direct dilution (1:29, v/v) in an acidic solution consisting of nitric acid (0.1%) and germanium (Ge) added as internal standard (IS), to obtain simple and high-throughput preparation procedure with minimized matrix effect, and good repeatability. ICP-MS analysis was performed using collision cell technology (CCT) mode. Alternate matrix method by using distilled water as an alternate analyte-free matrix for the preparation of calibration standards (CS) was used to avoid the influence of endogenous Sr in serum on the quantification. The method was validated in terms of selectivity, carry-over, matrix effects, lower limit of quantification (LLOQ), linearity, precision and accuracy, and stability. Instrumental linearity was verified in the range of 1.00-500ng/mL, corresponding to a concentration range of 0.0300-15.0μg/mL in 50μL sample of serum matrix and alternate matrix. Intra- and inter-day precision as relative standard deviation (RSD) were less than 8.0% and accuracy as relative error (RE) was within ±3.0%. The method allowed a high sample throughput, and was sensitive and accurate enough for a pilot bioequivalence study in healthy male Chinese subjects following single oral administration of two strontium ranelate formulations containing 2g strontium ranelate. Copyright © 2014 Elsevier GmbH. All rights reserved.

  14. Chem Ed Compacts

    ERIC Educational Resources Information Center

    Wolf, Walter A., Ed.

    1978-01-01

    Presents four simple laboratory procedures for: preparation of organometallic compounds, a realistic qualitative organic analysis project, a computer program to plot potentiometric titration curves, and preparation of stereoscopic transparencies. (SL)

  15. Advanced transition metal phosphide materials from single-source molecular precursors

    NASA Astrophysics Data System (ADS)

    Colson, Adam Caleb

    In this thesis, the feasibility of employing organometallic single-source precursors in the preparation of advanced transition metal pnictide materials such as colloidal nanoparticles and films has been investigated. In particular, the ternary FeMnP phase was targeted as a model for preparing advanced heterobimetallic phosphide materials, and the iron-rich Fe3P phase was targeted due to its favorable ferromagnetic properties as well as the fact that the preparation of advanced Fe3P materials has been elusive by commonly used methods. Progress towards the synthesis of advanced Fe2--xMn xP nanomaterials and films was facilitated by the synthesis of the novel heterobimetallic complexes FeMn(CO)8(mu-PR1R 2) (R1 = H, R2 = H or R1 = H, R2 = Ph), which contain the relatively rare mu-PH2 and mu-PPhH functionalities. Iron rich Fe2--xMnxP nanoparticles were obtained by thermal decomposition of FeMn(CO)8(mu-PH 2) using solution-based synthetic methods, and empirical evidence suggested that oleic acid was responsible for manganese depletion. Films containing Fe, Mn, and P with the desired stoichiometric ratio of 1:1:1 were prepared using FeMn(CO)8(mu-PH2) in a simple low-pressure metal-organic chemical vapor deposition (MOCVD) apparatus. Although the elemental composition of the precursor was conserved in the deposited film material, spectroscopic evidence indicated that the films were not composed of pure-phase FeMnP, but were actually mixtures of crystalline FeMnP and amorphous FeP and Mn xOy. A new method for the preparation of phase-pure ferromagnetic Fe 3P films on quartz substrates has also been developed. This approach involved the thermal decomposition of the single-source precursors H 2Fe3(CO)9PR (R = tBu or Ph) at 400 °C. The films were deposited using a simple home-built MOCVD apparatus and were characterized using a variety of analytical methods. The films exhibited excellent phase purity, as evidenced by X-ray diffraction, X-ray photoelectron spectroscopy, and field-dependent magnetization measurements, the results of which were all in good agreement with measurements obtained from bulk Fe3P. As-deposited Fe3P films were found to be amorphous, and little or no magnetic hysteresis was observed in plots of magnetization versus applied field. Annealing the Fe3P films at 550 °C resulted in improved crystallinity as well as the observation of magnetic hysteresis.

  16. Standardizing Descemet Membrane Endothelial Keratoplasty Graft Preparation Method in the Eye Bank-Experience of 527 Descemet Membrane Endothelial Keratoplasty Tissues.

    PubMed

    Parekh, Mohit; Baruzzo, Mattia; Favaro, Elisa; Borroni, Davide; Ferrari, Stefano; Ponzin, Diego; Ruzza, Alessandro

    2017-12-01

    To share the experience and provide a standardized protocol for Descemet membrane endothelial keratoplasty (DMEK) graft preparation. A retrospective study based on 527 prestripped DMEK tissues that were prepared between 2014 and 2017. The experience of using different instruments and techniques has been described, and a standardized technique for preparing DMEK grafts has been identified. The tissues in general were prepared by superficially tapping the endothelial side with a Moria trephine (9.5 mm diameter). The plane of cleavage was identified using a cleavage hook, and the DMEK graft was deadhered from the trephined site throughout the circumference for ease of excising the graft. The DMEK graft was peeled using either one or multiple quadrant methods depending on the challenges faced during excision. The graft was finally marked with the letter "F" to identify the orientation during surgery. Data on endothelial cell loss (ECL) and challenging cases were observed, monitored, and recorded during this period. Less than 1 percent trypan blue-positive cells with tissue wastage of <6% was observed during the study period. Our standardized stripping technique has resulted in an overall ECL of 4.6%. Marking Descemet membrane showed 0.5% cell mortality. Standardizing DMEK technique using specific tools and simple techniques would help new surgeons to decide the instruments and improve their tissue preparation skills also in challenging cases such as previous cataract incisions or horseshoe-shaped tears, further reducing ECL or tissue wastage.

  17. A Simple and Rapid Method for Standard Preparation of Gas Phase Extract of Cigarette Smoke

    PubMed Central

    Higashi, Tsunehito; Mai, Yosuke; Noya, Yoichi; Horinouchi, Takahiro; Terada, Koji; Hoshi, Akimasa; Nepal, Prabha; Harada, Takuya; Horiguchi, Mika; Hatate, Chizuru; Kuge, Yuji; Miwa, Soichi

    2014-01-01

    Cigarette smoke consists of tar and gas phase: the latter is toxicologically important because it can pass through lung alveolar epithelium to enter the circulation. Here we attempt to establish a standard method for preparation of gas phase extract of cigarette smoke (CSE). CSE was prepared by continuously sucking cigarette smoke through a Cambridge filter to remove tar, followed by bubbling it into phosphate-buffered saline (PBS). An increase in dry weight of the filter was defined as tar weight. Characteristically, concentrations of CSEs were represented as virtual tar concentrations, assuming that tar on the filter was dissolved in PBS. CSEs prepared from smaller numbers of cigarettes (original tar concentrations ≤15 mg/ml) showed similar concentration-response curves for cytotoxicity versus virtual tar concentrations, but with CSEs from larger numbers (tar ≥20 mg/ml), the curves were shifted rightward. Accordingly, the cytotoxic activity was detected in PBS of the second reservoir downstream of the first one with larger numbers of cigarettes. CSEs prepared from various cigarette brands showed comparable concentration-response curves for cytotoxicity. Two types of CSEs prepared by continuous and puff smoking protocols were similar regarding concentration-response curves for cytotoxicity, pharmacology of their cytotoxicity, and concentrations of cytotoxic compounds. These data show that concentrations of CSEs expressed by virtual tar concentrations can be a reference value to normalize their cytotoxicity, irrespective of numbers of combusted cigarettes, cigarette brands and smoking protocols, if original tar concentrations are ≤15 mg/ml. PMID:25229830

  18. Poly(vinyl Alcohol) Borate Gel Polymer Electrolytes Prepared by Electrodeposition and Their Application in Electrochemical Supercapacitors.

    PubMed

    Jiang, Mengjin; Zhu, Jiadeng; Chen, Chen; Lu, Yao; Ge, Yeqian; Zhang, Xiangwu

    2016-02-10

    Gel polymer electrolytes (GPEs) have been studied for preparing flexible and compact electrochemical energy storage devices. However, the preparation and use of GPEs are complex, and most GPEs prepared through traditional methods do not have good wettability with the electrodes, which retard them from achieving their performance potential. In this study, these problems are addressed by conceiving and implementing a simple, but effective, method of electrodepositing poly(vinyl alcohol) potassium borate (PVAPB) GPEs directly onto the surfaces of active carbon electrodes for electrochemical supercapacitors. PVAPB GPEs serve as both the electrolyte and the separator in the assembled supercapacitors, and their scale and shape are determined solely by the geometry of the electrodes. PVAPB GPEs have good bonding to the active electrode materials, leading to excellent and stable electrochemical performance of the supercapacitors. The electrochemical performance of PVAPB GPEs and supercapacitors can be manipulated simply by adjusting the concentration of KCl salt used during the electrodeposition process. With a 0.9 M KCl concentration, the as-prepared supercapacitors deliver a specific capacitance of 65.9 F g(-1) at a current density of 0.1 A g(-1) and retain more than 95% capacitance after 2000 charge/discharge cycles at a current density of 1 A g(-1). These supercapacitors also exhibit intelligent high voltage self-protection function due to the electrolysis-induced cross-linking effect of PVAPB GPEs.

  19. Quantitative Method for Simultaneous Analysis of Acetaminophen and 6 Metabolites.

    PubMed

    Lammers, Laureen A; Achterbergh, Roos; Pistorius, Marcel C M; Romijn, Johannes A; Mathôt, Ron A A

    2017-04-01

    Hepatotoxicity after ingestion of high-dose acetaminophen [N-acetyl-para-aminophenol (APAP)] is caused by the metabolites of the drug. To gain more insight into factors influencing susceptibility to APAP hepatotoxicity, quantification of APAP and metabolites is important. A few methods have been developed to simultaneously quantify APAP and its most important metabolites. However, these methods require a comprehensive sample preparation and long run times. The aim of this study was to develop and validate a simplified, but sensitive method for the simultaneous quantification of acetaminophen, the main metabolites acetaminophen glucuronide and acetaminophen sulfate, and 4 Cytochrome P450-mediated metabolites by using liquid chromatography with mass spectrometric (LC-MS) detection. The method was developed and validated for the human plasma, and it entailed a single method for sample preparation, enabling quick processing of the samples followed by an LC-MS method with a chromatographic run time of 9 minutes. The method was validated for selectivity, linearity, accuracy, imprecision, dilution integrity, recovery, process efficiency, ionization efficiency, and carryover effect. The method showed good selectivity without matrix interferences. For all analytes, the mean process efficiency was >86%, and the mean ionization efficiency was >94%. Furthermore, the accuracy was between 90.3% and 112% for all analytes, and the within- and between-run imprecision were <20% for the lower limit of quantification and <14.3% for the middle level and upper limit of quantification. The method presented here enables the simultaneous quantification of APAP and 6 of its metabolites. It is less time consuming than previously reported methods because it requires only a single and simple method for the sample preparation followed by an LC-MS method with a short run time. Therefore, this analytical method provides a useful method for both clinical and research purposes.

  20. Boehmite nanostructures preparation by hydrothermal method from anodic aluminium oxide membrane.

    PubMed

    Yang, X; Wang, J Y; Pan, H Y

    2009-02-01

    Boehmite nanostructures were successfully synthesized from porous anodic aluminium oxide (AAO) membrane by a simple and efficient hydro-thermal method. The experiment used high purity alumina as raw material, and the whole reaction process avoided superfluous impurities to be introduced. Thus, the purity of Boehmite products was ensured. The examinations of the morphology and structure were carried out by atomic force microscope (AFM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Composition of the specimens was analyzed using energy dispersive X-ray spectroscope (EDX) and X-ray diffraction (XRD). Based on these observations the growth process was analyzed.

  1. Hydrazine-Assisted Liquid Exfoliation of MoS2 for Catalytic Hydrodeoxygenation of 4-Methylphenol.

    PubMed

    Liu, Guoliang; Ma, Hualong; Teixeira, Ivo; Sun, Zhenyu; Xia, Qineng; Hong, Xinlin; Tsang, Shik Chi Edman

    2016-02-24

    A simple but effective method to exfoliate bulk MoS2 in a range of solvents is presented for the preparation of colloid flakes consisted of one to a few molecular layers by application of ultrasonic treatment in N2 H4 . Their high yield in solution and exposure of more active surface sites allows the synthesis of corresponding solid catalysts with remarkably high activity in hydrodeoxygenation of 4-methylphenol and this method can also be applied to other two dimensional materials. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. A facile approach toward transition metal oxide hierarchical structures and their lithium storage properties.

    PubMed

    Zhang, Cuimiao; Chen, Jing; Zeng, Yi; Rui, Xianhong; Zhu, Jixin; Zhang, Wenyu; Xu, Chen; Lim, Tuti Mariana; Hng, Huey Hoon; Yan, Qingyu

    2012-06-21

    A simple, non-template, non-surfactant and environmentally friendly hydrothermal method is presented based on the controlled release of the reactants into the reaction solvents to induce slow nucleation and growth of three-dimensional hierarchical nanostructures of transition metal oxides. This method is a general approach, which can be used to prepare Co(3)O(4), CuO, and Ni(OH)(2)/NiO. These metal oxides with hierarchical nanostructures can be used as anode materials for lithium-ion batteries with good Li storage performance, e.g. high specific capacities and stable cyclability.

  3. Stable isotope dimethyl labelling for quantitative proteomics and beyond

    PubMed Central

    Hsu, Jue-Liang; Chen, Shu-Hui

    2016-01-01

    Stable-isotope reductive dimethylation, a cost-effective, simple, robust, reliable and easy-to- multiplex labelling method, is widely applied to quantitative proteomics using liquid chromatography-mass spectrometry. This review focuses on biological applications of stable-isotope dimethyl labelling for a large-scale comparative analysis of protein expression and post-translational modifications based on its unique properties of the labelling chemistry. Some other applications of the labelling method for sample preparation and mass spectrometry-based protein identification and characterization are also summarized. This article is part of the themed issue ‘Quantitative mass spectrometry’. PMID:27644970

  4. Sol Gel-Derived SBA-16 Mesoporous Material

    PubMed Central

    Rivera-Muñoz, Eric M.; Huirache-Acuña, Rafael

    2010-01-01

    The aim of this article is to review current knowledge related to the synthesis and characterization of sol gel-derived SBA-16 mesoporous silicas, as well as a review of the state of the art in this issue, to take stock of knowledge about current and future applications. The ease of the method of preparation, the orderly structure, size and shape of their pores and control, all these achievable through simple changes in the method of synthesis, makes SBA-16 a very versatile material, potentially applicable in many areas of science and molecular engineering of materials. PMID:20957080

  5. Development and optimization of a novel sample preparation method cored on functionalized nanofibers mat-solid-phase extraction for the simultaneous efficient extraction of illegal anionic and cationic dyes in foods.

    PubMed

    Qi, Feifei; Jian, Ningge; Qian, Liangliang; Cao, Weixin; Xu, Qian; Li, Jian

    2017-09-01

    A simple and efficient three-step sample preparation method was developed and optimized for the simultaneous analysis of illegal anionic and cationic dyes (acid orange 7, metanil yellow, auramine-O, and chrysoidine) in food samples. A novel solid-phase extraction (SPE) procedure based on nanofibers mat (NFsM) was proposed after solvent extraction and freeze-salting out purification. The preferred SPE sorbent was selected from five functionalized NFsMs by orthogonal experimental design, and the optimization of SPE parameters was achieved through response surface methodology (RSM) based on the Box-Behnken design (BBD). Under the optimal conditions, the target analytes could be completely adsorbed by polypyrrole-functionalized polyacrylonitrile NFsM (PPy/PAN NFsM), and the eluent was directly analyzed by high-performance liquid chromatography-diode array detection (HPLC-DAD). The limits of detection (LODs) were between 0.002 and 0.01 mg kg -1 , and satisfactory linearity with correlation coefficients (R > 0.99) for each dye in all samples was achieved. Compared with the Chinese standard method and the published methods, the proposed method was simplified greatly with much lower requirement of sorbent (5.0 mg) and organic solvent (2.8 mL) and higher sample preparation speed (10 min/sample), while higher recovery (83.6-116.5%) and precision (RSDs < 7.1%) were obtained. With this developed method, we have successfully detected illegal ionic dyes in three common representative foods: yellow croaker, soybean products, and chili seasonings. Graphical abstract Schematic representation of the process of the three-step sample preparation.

  6. Extraction Optimization for Phenolic- and Withanolide-Rich Fractions from Withania somnifera Roots: Identification and Quantification of Withaferin A, 12-Deoxywithastromonolide, and Withanolide A in Plant Materials and Marketed Formulations Using a Reversed-Phase HPLC-Photodiode Array Detection Method.

    PubMed

    Kumar, Satyanshu; Singh, Raghuraj; Gajbhiye, Narendra; Dhanani, Tushar

    2018-06-26

    Background : Both the roots and leaves of Withania somnifera are products of commerce. They contain active compounds of therapeutic value and mostly different withanolides. Several pharmacological activities of W. somnifera have links to one or more withanolides. The presence of phenolic compounds in extracts could play a vital role in the reduction of blood glucose levels in diabetic subjects. Objective : The present study was carried out for the selection of a solvent to prepare extracts rich in phenolics, withaferin A (WA), 12-deoxywithastromonolide (12WD), and withanolide A (WDA). A simple, rapid HPLC method was also developed for the identification and quantification of WA, 12WD, and WDA. Methods : The extraction efficiency of aqueous alcoholic solvents including hexane, chloroform, ethyl acetate, and methanol were compared for three selected withanolides and total phenolic content. The contents of WA, 12WD, and WDA and total phenolics were determined in the extracts. The quality of nine formulations containing W. sominfera were also compared in terms of the content of WA, 12WD, and WDA and total phenolics. Results : The maximum extract yield and the total withanolide and phenolic content were obtained from aqueous alcoholic compositions at 50:50 (v/v), 70:30 (v/v), and 100:0 (v/v), respectively. In the case of organic solvents, chloroform and ethyl acetate yielded the highest concentrations of phenolics and three withanolides, respectively. The total phenolic content in formulations was in the range of 1.84-3.13%, and total withanolide content showed wide variability. Conclusions : The outcome of the present investigation could be utilized for the selection of extraction solvents to prepare W. somnifera -enriched extracts and their quality monitoring by using the developed and validated HPLC-Photodiode array detection method. Highlights : A process for preparation of phenolics and withanolides (withaferin A, 12-deoxywithastramonolide and withanolide A) enriched extracts of Withania somnifera . Simple and rapid HPLC method was also developed and validated as per the ICH guidelines for identification and quantification of three major withanolides. The developed HPLC method was applied to analyze the quality of extracts and marketed herbal products (mono, as well as poly constituents). Optimized extraction process could be utilized for upscaling process development in preparation of enriched extracts from Withania somnifera , crop improvement, bio-prospection studies and quality control.

  7. Hydrothermal Synthesis and Electrochemical Properties of CoS2-Reduced Graphene Oxide Nanocomposite for Supercapacitor Application

    NASA Astrophysics Data System (ADS)

    Venkateshalu, Sandhya; Rangappa, Dinesh; Grace, Andrews Nirmala

    A Cobalt disulfide-reduced graphene oxide (CoS2-RGO) nanocomposite was prepared by a simple hydrothermal method and the prepared nanocomposite was characterized using various techniques like XRD, SEM and FTIR. The results of these techniques indicated the uniform deposition of CoS2 nanoparticles on Graphene sheets. Further, the prepared nanocomposites were tested for its activity towards energy storage and the test results showed a specific capacitance of 28F/g in an aqueous 20% KOH electrolyte at a current density of 0.5A/g. All these materials showed highly reversible charge-discharge cycles. The overall electrochemical performance of this composite is shown to be drastically improved when compared to bare CoS2 nanoparticles. Thus with the good electrochemical properties, CoS2-RGO nanocomposites could be effectively used as an electrode material for supercapacitors.

  8. Template-Free Solvothermal Synthesis of Flower-Like BiOBr Microspheres in Ethanol Medium for Photocatalytic Applications

    NASA Astrophysics Data System (ADS)

    Hong, Shaoming; Ren, Huijun; Fang, Yanfeng; Huang, Yingping; Li, Ruiping

    2018-05-01

    Three-dimensionally (3D) BiOBr microflowers were prepared by a simple solvothermal method, employing Bi(NO3)3 · 5H2O and NaBr as starting reagents in ethanol. The structural, light absorption and morphological properties of as-prepared BiOBr microspheres were determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), and UV-Vis diffuse reflectance spectroscopy (DRS), etc. The results showed that ethanol acted not only as a solvent but also as a template in 3D BiOBr preparation. The BiOBr microspheres exhibited superior photocatalytic activity compared with 2D BiOBr nanosheets, far exceeding that of TiO2 (Degussa, P25). It was found that both superoxide radical (O2 •-) and holes (h+) played a key role in the degradation of RhB by BiOBr microflowers.

  9. Recent advances in polymer supporting layered double hydroxides nanocomposite for electrochemical biosensors

    NASA Astrophysics Data System (ADS)

    Dhanasekaran, T.; Padmanaban, A.; Gnanamoorthy, G.; Manigandan, R.; Praveen Kumar, S.; Stephen, A.; Narayanan, V.

    2018-01-01

    In recent years, layered double hydroxides (LDHs) materials having emerging due to their ability of intercalate a variety of anions, either organic or inorganic molecules. The most significance of the LDHs has been found potential applications in catalysis, wastewater treatment, and electrochemical sensors. The Mg-Al LDHs (MAL) and Poly-o-phenylenediamine @ Mg-Al LDHs (P-MAL) was prepared via simple one step hydrothermal method. As prepared material was characterized using many techniques such as, the structural and crystal phase was determined from XRD and Raman analyses. The functional groups were depicted using FT-IR spectroscopy. The optical propertied studied using diffuse reflectance spectroscopy UV-vis spectroscopy and the emission property were analyzed from Photoluminescence spectroscopy. The surface morphology and average particle size was analyzed using FESEM microscopy. The prepared polymer composite material P-MAL was further used for highly sensitive electrochemical detection towards dopamine (DA).

  10. Sustained release of simvastatin from hollow carbonated hydroxyapatite microspheres prepared by aspartic acid and sodium dodecyl sulfate.

    PubMed

    Wang, Ke; Wang, Yinjing; Zhao, Xu; Li, Yi; Yang, Tao; Zhang, Xue; Wu, Xiaoguang

    2017-06-01

    Hollow carbonated hydroxyapatite (HCHAp) microspheres as simvastatin (SV) sustained-release vehicles were fabricated through a novel and simple one-step biomimetic strategy. Firstly, hollow CaCO 3 microspheres were precipitated through the reaction of CaCl 2 with Na 2 CO 3 in the presence of aspartic acid and sodium dodecyl sulfate. Then, the as-prepared hollow CaCO 3 microspheres were transformed into HCHAp microspheres with a controlled anion-exchange method. The HCHAp microspheres were 3-5μm with a shell thickness of 0.5-1μm and were constructed of short needle nanoparticles. The HCHAp microspheres were then loaded with SV, exhibiting excellent drug-loading capacity and sustained release properties. These results present a new material synthesis strategy for HCHAp microspheres and suggest that the as-prepared HCHAp microspheres are promising for applications in drug delivery. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Spectrofluorimetric analysis of famotidine in pharmaceutical preparations and biological fluids by derivatization with benzoin

    NASA Astrophysics Data System (ADS)

    Alamgir, Malik; Khuhawar, Muhammad Yar; Memon, Saima Q.; Hayat, Amir; Zounr, Rizwan Ali

    2015-01-01

    A sensitive and simple spectrofluorimetric method has been developed for the analysis of famotidine, from pharmaceutical preparations and biological fluids after derivatization with benzoin. The reaction was carried out in alkaline medium with measurement of fluorescence intensity at 446 nm with excitation wavelength at 286 nm. Linear calibration was obtained with 0.5-15 μg/ml with coefficient of determination (r2) 0.997. The factors affecting the fluorescence intensity were optimized. The pharmaceutical additives and amino acid did not interfere in the determination. The mean percentage recovery (n = 4) calculated by standard addition from pharmaceutical preparation was 94.8-98.2% with relative standard deviation (RSD) 1.56-3.34% and recovery from deproteinized spiked serum and urine of healthy volunteers was 98.6-98.9% and 98.0-98.4% with RSD 0.34-0.84% and 0.29-0.87% respectively.

  12. Synthesis of new, highly luminescent bis(2,2’-bithiophen-5-yl) substituted 1,3,4-oxadiazole, 1,3,4-thiadiazole and 1,2,4-triazole

    PubMed Central

    Kostyuchenko, Anastasia S; L.Yurpalov, Vyacheslav; Kurowska, Aleksandra; Domagala, Wojciech; Pron, Adam

    2014-01-01

    Summary A new synthetic approach towards the preparation of functionalised, soluble, donor–acceptor (DA) alkylbithiophene derivatives of oxadiazole, thiadiazole and triazole is reported. Taking advantage of the Fiesselmann reaction, reactive bithiophene synthons having alkyl or alkoxy substituents at designated positions are prepared. Following a synthetic strategy, featuring the bottom-up approach, sequential structural elements are built, starting from a simple thiophene compound, until the target molecule is obtained, all in good yield. Supplementing the well established methods of oxadiazole and thiadiazole synthesis, efficient ring closure reaction affording a 4H-1,2,4-triazole unit is presented. All target ambipolar compounds display strong photoluminescence with measured quantum yields up to 0.59. Modification of the demonstrated synthetic routes may be exploited for the preparation of longer, specifically functionalised oligothiophenes, coupled to other heteroaromatic cores. PMID:25161716

  13. Synthesis of new, highly luminescent bis(2,2'-bithiophen-5-yl) substituted 1,3,4-oxadiazole, 1,3,4-thiadiazole and 1,2,4-triazole.

    PubMed

    Kostyuchenko, Anastasia S; L Yurpalov, Vyacheslav; Kurowska, Aleksandra; Domagala, Wojciech; Pron, Adam; Fisyuk, Alexander S

    2014-01-01

    A new synthetic approach towards the preparation of functionalised, soluble, donor-acceptor (DA) alkylbithiophene derivatives of oxadiazole, thiadiazole and triazole is reported. Taking advantage of the Fiesselmann reaction, reactive bithiophene synthons having alkyl or alkoxy substituents at designated positions are prepared. Following a synthetic strategy, featuring the bottom-up approach, sequential structural elements are built, starting from a simple thiophene compound, until the target molecule is obtained, all in good yield. Supplementing the well established methods of oxadiazole and thiadiazole synthesis, efficient ring closure reaction affording a 4H-1,2,4-triazole unit is presented. All target ambipolar compounds display strong photoluminescence with measured quantum yields up to 0.59. Modification of the demonstrated synthetic routes may be exploited for the preparation of longer, specifically functionalised oligothiophenes, coupled to other heteroaromatic cores.

  14. A highly selective and simple fluorescent sensor for mercury (II) ion detection based on cysteamine-capped CdTe quantum dots synthesized by the reflux method.

    PubMed

    Ding, Xiaojie; Qu, Lingbo; Yang, Ran; Zhou, Yuchen; Li, Jianjun

    2015-06-01

    Cysteamine (CA)-capped CdTe quantum dots (QDs) (CA-CdTe QDs) were prepared by the reflux method and utilized as an efficient nano-sized fluorescent sensor to detect mercury (II) ions (Hg(2+) ). Under optimum conditions, the fluorescence quenching effect of CA-CdTe QDs was linear at Hg(2+) concentrations in the range of 6.0-450 nmol/L. The detection limit was calculated to be 4.0 nmol/L according to the 3σ IUPAC criteria. The influence of 10-fold Pb(2+) , Cu(2+) and Ag(+) on the determination of Hg(2+) was < 7% (superior to other reports based on crude QDs). Furthermore, the detection sensitivity and selectivity were much improved relative to a sensor based on the CA-CdTe QDs probe, which was prepared using a one-pot synthetic method. This CA-CdTe QDs sensor system represents a new feasibility to improve the detection performance of a QDs sensor by changing the synthesis method. Copyright © 2014 John Wiley & Sons, Ltd.

  15. Direct analysis of psychoactive tryptamine and harmala alkaloids in the Amazonian botanical medicine ayahuasca by liquid chromatography-electrospray ionization-tandem mass spectrometry.

    PubMed

    McIlhenny, Ethan H; Pipkin, Kelly E; Standish, Leanna J; Wechkin, Hope A; Strassman, Rick; Barker, Steven A

    2009-12-18

    A direct injection/liquid chromatography-electrospray ionization-tandem mass spectrometry procedure has been developed for the simultaneous quantitation of 11 compounds potentially found in the increasingly popular Amazonian botanical medicine and religious sacrament ayahuasca. The method utilizes a deuterated internal standard for quantitation and affords rapid detection of the alkaloids by a simple dilution assay, requiring no extraction procedures. Further, the method demonstrates a high degree of specificity for the compounds in question, as well as low limits of detection and quantitation despite using samples for analysis that had been diluted up to 200:1. This approach also appears to eliminate potential matrix effects. Method bias for each compound, examined over a range of concentrations, was also determined as was inter- and intra-assay variation. Its application to the analysis of three different ayahuasca preparations is also described. This method should prove useful in the study of ayahuasca in clinical and ethnobotanical research as well as in forensic examinations of ayahuasca preparations.

  16. Application of a Stir Bar Sorptive Extraction sample preparation method with HPLC for soil fungal biomass determination in soils from a detrital manipulation study.

    PubMed

    Beni, Áron; Lajtha, Kate; Kozma, János; Fekete, István

    2017-05-01

    Ergosterol is a sterol found ubiquitously in cell membranes of filamentous fungi. Although concentrations in different fungal species span the range of 2.6 to 42μg/mL of dry mass, many studies have shown a strong correlation between soil ergosterol content and fungal biomass. The analysis of ergosterol in soil therefore could be an effective tool for monitoring changes in fungal biomass under different environmental conditions. Stir Bar Sorptive Extraction (SBSE) is a new sample preparation method to extract and concentrate organic analytes from liquid samples. SBSE was here demonstrated to be a simple, fast, and cost effective method for the quantitative analysis of ergosterol from field-collected soils. Using this method we observed that soil ergosterol as a measure of fungal biomass proved to be a sensitive indicator of soil microbial dynamics that were altered by changes in plant detrital inputs to soils in a long-term field experiment. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. A convenient method for synthesis of glyconanoparticles for colorimetric measuring carbohydrate-protein interactions

    PubMed Central

    Chuang, Yen-Jun; Zhou, Xichun; Pan, Zhengwei; Turchi, Craig

    2009-01-01

    Carbohydrate functionalized nanoparticles, i.e., the glyconanoparticles, have wide application ranging from studies of carbohydrate-protein interactions, in vivo cell imaging, biolabeling, etc. Currently reported methods for preparation of glyconanoaprticles require multi-step modifications of carbohydrates moieties to conjugate to nanoparticle surface. However, the required synthetic manipulations are difficult and time consuming. We report herewith a simple and versatile method for preparing glyconanoparticles. This method is based on the utilization of clean and convenient microwave irradiation energy for one-step, site-specific conjugation of unmodified carbohydrates onto hydrazide-functionalized Au nanoparticles. A colorimetric assay that utilizes the ensemble of gold glyconanoparticles and Concanavalin A (ConA) was also presented. This feasible assay system was developed to analyze multivalent interactions and to determine the dissociation constant (Kd) for five kind of Au glyconanoparticles with lectin. Surface plasmon changes of the Au glyconanparticles as a function of lectin-carbohydrate interactions were measured and the dissociation constants were determined based on non-linear curve fitting. The strength of the interaction of carbohydrates with ConA was found to be as follows: Maltose > Mannose > Glucose > Lactose > MAN5. PMID:19698698

  18. Eco-friendly aqueous core surface-modified nanocapsules.

    PubMed

    Carbone, C; Musumeci, T; Lauro, M R; Puglisi, G

    2015-01-01

    In this work, positively charged nanocapsules have been developed for potential ocular delivery exploiting the deposition of PLA onto the droplet surface of a W/O nanoemulsion prepared by the reversed procedure of the PIT method. PLA in combination with different amounts of various oils and surfactants have been studied in order to select the best formulation for polymeric nanocapsule preparation. The traditional visual observation together with the Turbiscan(®) technology were exploited in order to identify the best combination of polymer/oil for nanocapsule preparation. Two different primary surfactants (Span(®) 60 and Span(®) 80) have been tested to select their influence on the field of existence of the nanoemulsion by the construction of the pseudoternary phase diagrams. Cationic hybrid NC have been prepared by the addition of a coating layer of DDAB. The physico-chemical and morphological properties of all the prepared nanocapsules have been evaluated and compared by PCS, DSC and AFM. Therefore, positively charged nanocapsules can be easily prepared by a simple eco-friendly technique that exploits biocompatible materials avoiding a large input of mechanical energy as a potential ocular delivery systems for hydrophilic compounds or gene materials. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Simultaneous determination of potassium guaiacolsulfonate, guaifenesin, diphenhydramine HCl and carbetapentane citrate in syrups by using HPLC-DAD coupled with partial least squares multivariate calibration.

    PubMed

    Dönmez, Ozlem Aksu; Aşçi, Bürge; Bozdoğan, Abdürrezzak; Sungur, Sidika

    2011-02-15

    A simple and rapid analytical procedure was proposed for the determination of chromatographic peaks by means of partial least squares multivariate calibration (PLS) of high-performance liquid chromatography with diode array detection (HPLC-DAD). The method is exemplified with analysis of quaternary mixtures of potassium guaiacolsulfonate (PG), guaifenesin (GU), diphenhydramine HCI (DP) and carbetapentane citrate (CP) in syrup preparations. In this method, the area does not need to be directly measured and predictions are more accurate. Though the chromatographic and spectral peaks of the analytes were heavily overlapped and interferents coeluted with the compounds studied, good recoveries of analytes could be obtained with HPLC-DAD coupled with PLS calibration. This method was tested by analyzing the synthetic mixture of PG, GU, DP and CP. As a comparison method, a classsical HPLC method was used. The proposed methods were applied to syrups samples containing four drugs and the obtained results were statistically compared with each other. Finally, the main advantage of HPLC-PLS method over the classical HPLC method tried to emphasized as the using of simple mobile phase, shorter analysis time and no use of internal standard and gradient elution. Copyright © 2010 Elsevier B.V. All rights reserved.

  20. Development and validation of a simple and robust method for arsenic speciation in human urine using HPLC/ICP-MS.

    PubMed

    Sen, Indranil; Zou, Wei; Alvaran, Josephine; Nguyen, Linda; Gajek, Ryszard; She, Jianwen

    2015-01-01

    In order to better distinguish the different toxic inorganic and organic forms of arsenic (As) exposure in individuals, we have developed and validated a simple and robust analytical method for determining the following six As species in human urine: arsenous (III) acid (As-III), As (V) acid, monomethylarsonic acid, dimethylarsinic acid, arsenobetaine (AsB), and arsenocholine. In this method, human urine is diluted using a pH 5.8 buffer, separation is performed using an anion exchange column with isocratic HPLC, and detection is achieved using inductively coupled plasma-MS. The method uses a single mobile phase consisting of low concentrations of both phosphate buffer (5 mM) and ammonium nitrate salt (5 mM) at pH 9.0; this minimizes the column equilibration time and overcomes challenges with separation between AsB and As-III. In addition, As-III oxidation is prevented by degassing the sample preparation buffer at pH 5.8, degassing the mobile phase online at pH 9.0, and by the use of low temperature (-70 °C) and flip-cap airtight tubes for long term storage of samples. The method was validated using externally provided reference samples. Results were in agreement with target values at varying concentrations and successfully passed external performance test criteria. Internal QC samples were prepared and repeatedly analyzed to assess the method's long-term precision, and further analyses were completed on anonymous donor urine to assess the quality of the method's baseline separation. Results from analyses of external reference samples agreed with target values at varying concentrations, and results from precision studies yielded absolute CV values of 3-14% and recovery from 82 to 115% for the six As species. Analysis of anonymous donor urine confirmed the well-resolved baseline separation capabilities of the method for real participant samples.

  1. Microfluidic systems with embedded materials and structures and method thereof

    DOEpatents

    Morse, Jeffrey D [Martinez, CA; Rose, Klint A [Boston, MA; Maghribi, Mariam [Livermore, CA; Benett, William [Livermore, CA; Krulevitch, Peter [Pleasanton, CA; Hamilton, Julie [Tracy, CA; Graff, Robert T [Modesto, CA; Jankowski, Alan [Livermore, CA

    2007-03-06

    Described herein is a process for fabricating microfluidic systems with embedded components in which micron-scale features are molded into the polymeric material polydimethylsiloxane (PDMS). Micromachining is used to create a mold master and the liquid precursors for PDMS are poured over the mold and allowed to cure. The PDMS is then removed form the mold and bonded to another material such as PDMS, glass, or silicon after a simple surface preparation step to form sealed microchannels.

  2. Protocol for the use of light upon extension real-time PCR for the determination of viral load in HBV infection.

    PubMed

    Li, Guimin; Li, Wangfeng; Liu, Lixia

    2012-01-01

    Real-time PCR has engendered wide acceptance for quantitation of hepatitis B virus (HBV) DNA in the blood due to its improved rapidity, sensitivity, reproducibility, and reduced contamination. Here we describe a cost-effective and highly sensitive HBV real-time quantitative assay based on the light upon extension real-time PCR platform and a simple and reliable HBV DNA preparation method using silica-coated magnetic beads.

  3. Thermolysis of Geminal Diazides: Reagent-Free Synthesis of 3-Hydroxypyridines.

    PubMed

    Erhardt, Hellmuth; Kunz, Kevin A; Kirsch, Stefan F

    2017-01-06

    An operationally simple protocol for the rapid and efficient construction of highly substituted 3-hydroxypyridines is presented. The thermally induced cyclization of easily constructed geminal diazides derived from β-ketoesters having an additional olefin moiety affords the title compounds in yields up to 97% under reagent-free conditions. The new method allows for the synthesis of preparative quantities of material. Additionally, the synthetic utility of the pyridine products for the synthesis of valuable heterocycles is described.

  4. Double-Immunodiffusion Assay for Detecting Specific Antibodies (Ouchterlony).

    PubMed

    Hornbeck, Peter

    2017-02-02

    The method first described by Ouchterlony in 1948 is a classic and simple technique that permits evaluation and comparison of antibodies in animal or human sera directed against protein or complex carbohydrate antigens. It is a low-tech procedure that may provide information on the relative quantity of antibody activity and the nature of the antigenic epitopes in different preparations. © 2017 by John Wiley & Sons, Inc. Copyright © 2017 John Wiley & Sons, Inc. All rights reserved.

  5. Synthesis of chitosan supported palladium nanoparticles and its catalytic activity towards 2-nitrophenol reduction

    NASA Astrophysics Data System (ADS)

    Dhanavel, S.; Nivethaa, E. A. K.; Esther, G.; Narayanan, V.; Stephen, A.

    2016-05-01

    Chitosan supported Palladium nanoparticles were synthesized by a simple cost effective chemical reduction method using NaBH4. The prepared nanocomposite was characterized by X-Ray diffraction analysis, FESEM and Energy dispersive spectroscopy analysis of X-rays (EDAX). The catalytic performance of the nanocomposite was evaluated on the reduction of 2-Nitrophenol to the 2-Amino phenol with rate constant 1.08 × 10-3 S-1 by NaBH4 using Spectrophotometer.

  6. Virus templated metallic nanoparticles

    NASA Astrophysics Data System (ADS)

    Aljabali, Alaa A. A.; Barclay, J. Elaine; Lomonossoff, George P.; Evans, David J.

    2010-12-01

    Plant viruses are considered as nanobuilding blocks that can be used as synthons or templates for novel materials. Cowpea mosaic virus (CPMV) particles have been shown to template the fabrication of metallic nanoparticles by an electroless deposition metallization process. Palladium ions were electrostatically bound to the virus capsid and, when reduced, acted as nucleation sites for the subsequent metal deposition from solution. The method, although simple, produced highly monodisperse metallic nanoparticles with a diameter of ca. <=35 nm. CPMV-templated particles were prepared with cobalt, nickel, iron, platinum, cobalt-platinum and nickel-iron.Plant viruses are considered as nanobuilding blocks that can be used as synthons or templates for novel materials. Cowpea mosaic virus (CPMV) particles have been shown to template the fabrication of metallic nanoparticles by an electroless deposition metallization process. Palladium ions were electrostatically bound to the virus capsid and, when reduced, acted as nucleation sites for the subsequent metal deposition from solution. The method, although simple, produced highly monodisperse metallic nanoparticles with a diameter of ca. <=35 nm. CPMV-templated particles were prepared with cobalt, nickel, iron, platinum, cobalt-platinum and nickel-iron. Electronic supplementary information (ESI) available: Additional experimental detail, agarose gel electrophoresis results, energy dispersive X-ray spectra, ζ-potential measurements, dynamic light scattering data, nanoparticle tracking analysis and an atomic force microscopy image of Ni-CPMV. See DOI: 10.1039/c0nr00525h

  7. Ratiometric near infrared luminescent thermometer based on lanthanide metal-organic frameworks

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

    Yue, Dan; Zhang, Jun; Zhao, Dian

    2016-09-15

    A near infrared luminescent MOFs thermometer (Nd{sub 0.676}Yb{sub 0.324}BTC) was prepared via a simple solvothermal method using Ln{sup 3+} (Ln=Nd, Yb) ions and 1, 3, 5-benznenetricarboxylic acid (H{sub 3}BTC), and characterized by PXRD, TGA, ICP, and photoluminescence (PL) spectrum. These results indicate that the Nd{sub 0.676}Yb{sub 0.324}BTC displays high relative sensitivity and excellent repeatability in the physiological temperature range (288–323 K), and the maximum relative sensitivity is determined to be 1.187% K{sup −1} at 323 K. These NIR luminescent MOFs may have potential applications in physiological temperature sensing. - Graphical abstract: A near infrared luminescent MOFs thermometer (Nd{sub 0.054}Yb{sub 0.946}BTCmore » ) displays high relative sensitivity and excellent repeatability in the physiological temperature range (288–323 K). Display Omitted - Highlights: • A ratiometric near infrared luminescent MOFs thermometer (Nd{sub 0.676}Yb{sub 0.324}BTC) was prepared via a simple solvothermal method. • The maximum relative sensitivity of Nd{sub 0.676}Yb{sub 0.324}BTC is determined to be 1.187% K{sup −1} at 323 K. • Nd{sub 0.676}Yb{sub 0.324}BTC showed excellent repeatability in the physiological temperature range (288–323 K).« less

  8. 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

  9. Chemically stable and mechanically durable superamphiphobic aluminum surface with a micro/nanoscale binary structure.

    PubMed

    Peng, Shan; Yang, Xiaojun; Tian, Dong; Deng, Wenli

    2014-09-10

    We developed a simple fabrication method to prepare a superamphiphobic aluminum surface. On the basis of a low-energy surface and the combination of micro- and nanoscale roughness, the resultant surface became super-repellent toward a wide range of liquids with surface tensions of 25.3-72.1 mN m(-1). The applied approach involved (1) the formation of an irregular microplateau structure on an aluminum surface, (2) the fabrication of a nanoplatelet structure, and (3) fluorination treatment. The chemical stability and mechanical durability of the superamphiphobic surface were evaluated in detail. The results demonstrated that the surface presented an excellent chemical stability toward cool corrosive liquids (HCl/NaOH solutions, 25 °C) and 98% concentrated sulfuric acid, hot liquids (water, HCl/NaOH solutions, 30-100 °C), solvent immersion, high temperature, and a long-term period. More importantly, the surface also exhibited robust mechanical durability and could withstand multiple-fold, finger-touch, intensive scratching by a sharp blade, ultrasonication treatment, boiling treatment in water and coffee, repeated peeling by adhesive tape, and even multiple abrasion tests under 500 g of force without losing superamphiphobicity. The as-prepared superamphiphobic surface was also demonstrated to have excellent corrosion resistance. This work provides a simple, cost-effective, and highly efficient method to fabricate a chemically stable and mechanically robust superamphiphobic aluminum surface, which can find important outdoor applications.

  10. Influence of surfactants on the morphology of SnO{sub 2} nanocrystals prepared via a hydrothermal method

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

    Wang Mi; Shanghai Institute of Ceramics; Gao Yanfeng, E-mail: yfgao@mail.sic.ac.cn

    2012-05-15

    Nanoscaled SnO{sub 2} with different morphologies has been synthesized via a simple hydrothermal process at 180 Degree-Sign C using polyvinylpyrrolidone (PVP), sodium dodecyl sulfonate (SDS), cetyl trimethyl ammonium bromide (CTAB) or tetrapropyl ammonium bromide (TPAB) as surfactant. All the prepared SnO{sub 2} are of a tetragonal crystal structure. Nanocubes, nanorods, nanosheets, nanobelts and nanoparticles were prepared when changing the type and dosage of organic surfactants. It is shown that anionic surfactant (SDS) and cationic surfactant (CTAB or TPAB) at their suitable addition amounts can largely influence the morphologies of SnO{sub 2} nanocrystals. The effect is significantly dependent on the solventmore » types: water or ethanol. The non-ionic surfactant (PVP) can also change the morphologies like SDS but the impacts are less obvious. The effect of surfactants on the shape and size of SnO{sub 2} nanoparticles was discussed in detail. The particle growth mechanism is described based on the electrostatic interactions and Van der Waals' forces. - Graphical abstract: SnO{sub 2} nanocrystals with controllable morphologies were prepared via a hydrothermal method with surfactants. Highlights: Black-Right-Pointing-Pointer SnO{sub 2} nanocrystals were prepared via a hydrothermal method with surfactants. Black-Right-Pointing-Pointer SnO{sub 2} morphologies changed with the type and the dosage of surfactants. Black-Right-Pointing-Pointer The effect of surfactants on the growth of crystal planes was studied. Black-Right-Pointing-Pointer The controlling mechanisms of surfactants on SnO{sub 2} morphologies were discussed.« less

  11. Rubber-like Quasi-thermosetting Polyetheramine-cured Epoxy Asphalt Composites Capable of Being Opened to Traffic Immediately

    NASA Astrophysics Data System (ADS)

    Kang, Yang; Wu, Qiang; Jin, Rui; Yu, Pengfei; Cheng, Jixiang

    2016-01-01

    This paper reports the facile preparation, mechanical performance and linear viscoelasticity of polyetheramine-cured rubber-like epoxy asphalt composites (EACs) with different asphalt contents. Compared with previous EACs prepared via complex chemical reactions and time-consuming high-temperature curing, the EACs reported here were obtained by using a compatible, bi-functional polyetheramine and a simple physical co-blend process, which make the EACs feasibly scalable for production at a lower cost. The EACs were cured for 1 h at 160 °C and 3 d at 60 °C therefore, these composites can be opened to traffic immediately. The EACs have a much greater temperature stability than common thermoplastic polymer-modified asphalt composites from -30 °C to 120 °C, but their complex shear moduli at higher temperatures slightly decrease instead of remaining constant when temperatures are greater than 80 °C, especially for the higher asphalt content composites; that is, these composites are quasi-thermosetting. Wicket plots illustrate that the EACs reported here are thermorheological simple materials, and the master curves are constructed and well-fitted by generalized logistic sigmoidal model functions. This research provides a facile, low-cost method for the preparation of polyetheramine-cured EACs that can be opened to traffic immediately, and the concept of quasi-thermosetting may facilitate the development of cheaper EACs for advanced applications.

  12. Functionalized graphene oxide quantum dot-PVA hydrogel: a colorimetric sensor for Fe2+, Co2+ and Cu2+ ions

    NASA Astrophysics Data System (ADS)

    Baruah, Upama; Chowdhury, Devasish

    2016-04-01

    Functionalized graphene oxide quantum dots (GOQDs)-poly(vinyl alcohol) (PVA) hybrid hydrogels were prepared using a simple, facile and cost-effective strategy. GOQDs bearing different surface functional groups were introduced as the cross-linking agent into the PVA matrix thereby resulting in gelation. The four different types of hybrid hydrogels were prepared using graphene oxide, reduced graphene oxide, ester functionalized graphene oxide and amine functionalized GOQDs as cross-linking agents. It was observed that the hybrid hydrogel prepared with amine functionalized GOQDs was the most stable. The potential applicability of using this solid sensing platform has been subsequently explored in an easy, simple, effective and sensitive method for optical detection of M2+ (Fe2+, Co2+ and Cu2+) in aqueous media involving colorimetric detection. Amine functionalized GOQDs-PVA hybrid hydrogel when put into the corresponding solution of Fe2+, Co2+ and Cu2+ renders brown, orange and blue coloration respectively of the solution detecting the presence of Fe2+, Co2+ and Cu2+ ions in the solution. The minimum detection limit observed was 1 × 10-7 M using UV-visible spectroscopy. Further, the applicability of the sensing material was also tested for a mixture of co-existing ions in solution to demonstrate the practical applicability of the system. Insight into the probable mechanistic pathway involved in the detection process is also being discussed.

  13. Easy preparation of a large-size random gene mutagenesis library in Escherichia coli.

    PubMed

    You, Chun; Percival Zhang, Y-H

    2012-09-01

    A simple and fast protocol for the preparation of a large-size mutant library for directed evolution in Escherichia coli was developed based on the DNA multimers generated by prolonged overlap extension polymerase chain reaction (POE-PCR). This protocol comprised the following: (i) a linear DNA mutant library was generated by error-prone PCR or shuffling, and a linear vector backbone was prepared by regular PCR; (ii) the DNA multimers were generated based on these two DNA templates by POE-PCR; and (iii) the one restriction enzyme-digested DNA multimers were ligated to circular plasmids, followed by transformation to E. coli. Because the ligation efficiency of one DNA fragment was several orders of magnitude higher than that of two DNA fragments for typical mutant library construction, it was very easy to generate a mutant library with a size of more than 10(7) protein mutants per 50 μl of the POE-PCR product. Via this method, four new fluorescent protein mutants were obtained based on monomeric cherry fluorescent protein. This new protocol was simple and fast because it did not require labor-intensive optimizations in restriction enzyme digestion and ligation, did not involve special plasmid design, and enabled constructing a large-size mutant library for directed enzyme evolution within 1 day. Copyright © 2012 Elsevier Inc. All rights reserved.

  14. Rubber-like Quasi-thermosetting Polyetheramine-cured Epoxy Asphalt Composites Capable of Being Opened to Traffic Immediately.

    PubMed

    Kang, Yang; Wu, Qiang; Jin, Rui; Yu, Pengfei; Cheng, Jixiang

    2016-01-06

    This paper reports the facile preparation, mechanical performance and linear viscoelasticity of polyetheramine-cured rubber-like epoxy asphalt composites (EACs) with different asphalt contents. Compared with previous EACs prepared via complex chemical reactions and time-consuming high-temperature curing, the EACs reported here were obtained by using a compatible, bi-functional polyetheramine and a simple physical co-blend process, which make the EACs feasibly scalable for production at a lower cost. The EACs were cured for 1 h at 160 °C and 3 d at 60 °C; therefore, these composites can be opened to traffic immediately. The EACs have a much greater temperature stability than common thermoplastic polymer-modified asphalt composites from -30 °C to 120 °C, but their complex shear moduli at higher temperatures slightly decrease instead of remaining constant when temperatures are greater than 80 °C, especially for the higher asphalt content composites; that is, these composites are quasi-thermosetting. Wicket plots illustrate that the EACs reported here are thermorheological simple materials, and the master curves are constructed and well-fitted by generalized logistic sigmoidal model functions. This research provides a facile, low-cost method for the preparation of polyetheramine-cured EACs that can be opened to traffic immediately, and the concept of quasi-thermosetting may facilitate the development of cheaper EACs for advanced applications.

  15. Characterization and immobilization of arylsulfatase on modified magnetic nanoparticles for desulfation of agar.

    PubMed

    Xiao, Qiong; Yin, Qin; Ni, Hui; Cai, Huinong; Wu, Changzheng; Xiao, Anfeng

    2017-01-01

    Carboxyl functioned magnetic nanoparticles (CMNPs) were prepared by a simple co-precipitation method and characterized by Fourier transform infrared spedtroscopy and scanning electron microscope. The prepared CMNPs were used for covalent immobilization of the arylsulfatase which could be applied in desulfation of agar. The optimal immobilizaion conditions were obtained as follows: glutaraldehyde concentration 1.0% (v/v), cross-linking time 3h, immobilization time 3h, immobilization temperature 5°C and enzyme dose 0.62U. Increase in properties of the arylsulfatase such as optimum temperature and pH was observed after immobilization. Immobilization led to increased tolerance of enzyme to some metal ions, inhibitors and detergents. The K m and k cat of the immobilized enzyme for hydrolysis of p-NPS at pH 7.5 and at 50°C were determined to be 0.89mmol/L and 256.91s -1 , respectively. The relative desulfuration rates of immobilized arylsulfatase maintained 61.7% of its initial desulfuration rates after seven cycles. After the reaction of agar with immobilized arylsulfatase for 90min at 50°C, 46% of the sulfate in the agar was removed. These results showed that the immobilization of arylsulfatase onto CMNPs is an efficient and simple way for preparation of stable arylsulfatase and have a great potential for application in enzymatic desulfation of agar. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Towards the development of multifunctional molecular indicators combining soil biogeochemical and microbiological variables to predict the ecological integrity of silvicultural practices.

    PubMed

    Peck, Vincent; Quiza, Liliana; Buffet, Jean-Philippe; Khdhiri, Mondher; Durand, Audrey-Anne; Paquette, Alain; Thiffault, Nelson; Messier, Christian; Beaulieu, Nadyre; Guertin, Claude; Constant, Philippe

    2016-05-01

    The impact of mechanical site preparation (MSP) on soil biogeochemical structure in young larch plantations was investigated. Soil samples were collected in replicated plots comprising simple trenching, double trenching, mounding and inverting site preparation. Unlogged natural mixed forest areas were used as a reference. Analysis of soil nutrients, abundance of bacteria and gas exchanges unveiled no significant difference among the plots. However, inverting site preparation resulted in higher variations of gas exchanges when compared with trenching, mounding and unlogged natural forest. A combination of the biological and physicochemical variables was used to define a multifunctional classification of the soil samples into four distinct groups categorized as a function of their deviation from baseline ecological conditions. According to this classification model, simple trenching was the approach that represented the lowest ecological risk potential at the microsite level. No relationship was observed between MSP method and soil bacterial community structure as assessed by high-throughput sequencing of bacterial 16S rRNA gene; however, indicator genotypes were identified for each multifunctional soil class. This is the first identification of multifunctional molecular indicators for baseline and disturbed ecological conditions in soil, demonstrating the potential of applied microbial ecology to guide silvicultural practices and ecological risk assessment. © 2016 The Authors. Microbial Biotechnology published by John Wiley & Sons Ltd and Society for Applied Microbiology.

  17. Ethanol gas sensor based upon ZnO nanoparticles prepared by different techniques

    NASA Astrophysics Data System (ADS)

    Bhatia, Sonik; Verma, Neha; Bedi, R. K.

    Nowadays, applications of nanosized materials have been an important issue in basic and applied sciences. In this investigation, Zinc Oxide (ZnO) nanoparticles were prepared by two different techniques (simple heat treatment, thermal evaporation-two zone furnaces). In order to control shape and size - ZnO nanoparticles prepared from heat treatment were used as a source for thermal evaporation method by using two zone split furnace by varying zone temperature (Zone 1-800 °C and Zone 2-400 °C). For both techniques 0.17 M of Zn acetate dihydrate is used as main precursor and film is deposited on glass substrate. Synthesized ZnO were characterized for XRD, FESEM, FTIR and UV-Vis spectrophotometer and LCR meter. XRD revealed hexagonal wurtzite structure with preferential orientation along (1 0 1) plane. FESEM observed that grain size in the range of range of ∼50 ± 5 nm. FTIR spectra showed that the peaks between 400 and 500 cm-1 for ZnO stretching modes. Optical properties has been studied and found that the observed band gap lies in the range of 3.32-3.36 eV. The higher value of capacitance is observed at lower frequency. Gas sensing properties showed the higher response in case of thermal evaporation as compared to simple heat treatment at an operating temperature of 250 °C.

  18. Rubber-like Quasi-thermosetting Polyetheramine-cured Epoxy Asphalt Composites Capable of Being Opened to Traffic Immediately

    PubMed Central

    Kang, Yang; Wu, Qiang; Jin, Rui; Yu, Pengfei; Cheng, Jixiang

    2016-01-01

    This paper reports the facile preparation, mechanical performance and linear viscoelasticity of polyetheramine-cured rubber-like epoxy asphalt composites (EACs) with different asphalt contents. Compared with previous EACs prepared via complex chemical reactions and time-consuming high-temperature curing, the EACs reported here were obtained by using a compatible, bi-functional polyetheramine and a simple physical co-blend process, which make the EACs feasibly scalable for production at a lower cost. The EACs were cured for 1 h at 160 °C and 3 d at 60 °C; therefore, these composites can be opened to traffic immediately. The EACs have a much greater temperature stability than common thermoplastic polymer-modified asphalt composites from −30 °C to 120 °C, but their complex shear moduli at higher temperatures slightly decrease instead of remaining constant when temperatures are greater than 80 °C, especially for the higher asphalt content composites; that is, these composites are quasi-thermosetting. Wicket plots illustrate that the EACs reported here are thermorheological simple materials, and the master curves are constructed and well-fitted by generalized logistic sigmoidal model functions. This research provides a facile, low-cost method for the preparation of polyetheramine-cured EACs that can be opened to traffic immediately, and the concept of quasi-thermosetting may facilitate the development of cheaper EACs for advanced applications. PMID:26733315

  19. [Application of penthrox preparation in patients with traumatic disease].

    PubMed

    Boĭko, V V; Sushkov, S V; Zamiatin, P N; Krut'ko, E N

    2011-06-01

    Indications for preparation Pentrox application in injured persons, suffering traumatic disease, were substantiated. The pain syndrome dynamics while conducting analgesia, was investigated, using simple verbal scale.

  20. Precise micropatterning of silver nanoparticles on plastic substrates

    NASA Astrophysics Data System (ADS)

    Ammosova, Lena; Jiang, Yu; Suvanto, Mika; Pakkanen, Tapani A.

    2017-04-01

    Conventional fabrication methods to obtain metal patterns on polymer substrates are restricted by high operating temperature and complex preparation steps. The present study demonstrates a simple yet versatile method for preparation of silver nanoparticle micropatterns on polymer substrates with various surface geometry. With the microworking robot technique, we were able not only to directly structure the surface, but also precisely deposit silver nanoparticle ink on the desired surface location with the minimum usage of ink material. The prepared silver nanoparticle ink, containing silver cations and polyethylene glycol (PEG) as a reducing agent, yields silver nanoparticle micropatterns on plastic substrates at low sintering temperature without any contamination. The influence of the ink behaviour was studied, such as substrate wettability, ink volume, and sintering temperature. The ultraviolet visible (UV-vis), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS) measurements revealed the formation of micropatterns with uniformly distributed silver nanoparticles. The prepared patterns are expected to have a broad range of applications in optics, medicine, and sensor devices owing to the unique properties of silver. Furthermore, the deposition of a chemical compound, which is different from the substrate material, not only adds a fourth dimension to the prestructured three-dimensional (3D) surfaces, but also opens new application areas to the conventional surface structures.

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