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two liquid phase

Xiyue Xiong, Haiqin He, Yan Shu, Yuxin Li, Zihui Yang, Yingzhuang Chen, Ming Ma, Bo Chen
A facile, flexible process was developed for the preparation of surface-glycosylated porous monolithic columns via aqueous two-phase graft copolymerization of polyethylene glycol diacrylate (PEGDA) and water-soluble dextran (dextran sulfate). The formation of poly(PEGDA) porous skeletons and surface glycosylation were achieved via a one-step process without pre-modification of the dextran. The synthesis conditions were thoroughly optimized. The optimal monolithic column exhibited a large dry state surface area (greater than 400m(2)/g), and it was evaluated as a hydrophilic liquid chromatography (HILIC) stationary phase...
December 1, 2016: Talanta
Félix Zapata, Mª Ángeles Fernández de la Ossa, Elizabeth Gilchrist, Leon Barron, Carmen García-Ruiz
Concerning the dreadful global threat of terrorist attacks, the detection of explosive residues in biological traces and marks is a current need in both forensics and homeland security. This study examines the potential of Raman microscopy in comparison to liquid chromatography (ion chromatography (IC) and reversed-phase high performance liquid chromatography (RP-HPLC)) to detect, identify and quantify residues in human handmarks of explosives and energetic salts commonly used to manufacture Improvised Explosive Devices (IEDs) including dynamite, ammonium nitrate, single- and double-smokeless gunpowders and black powder...
December 1, 2016: Talanta
Pavel Kubáň, Knut Fredrik Seip, Astrid Gjelstad, Stig Pedersen-Bjergaard
This work investigated selective micro-electromembrane extractions (μ-EMEs) of the colored indicators metanil yellow and congo red (visual proof-of-principle) and the small drug substances nortriptyline, papaverine, mianserin, and citalopram (model analytes) based on their acid-base strength. With two free liquid membranes (FLMs), the target analytes were extracted from aqueous donor solution, across FLM 1 (1-pentanol, 1-ethyl-2-nitrobenzene (ENB) or 4-nitrocumene (4-NC)), into aqueous acceptor solution 1, further across FLM 2 (1-pentanol, ENB or 4-NC), and finally into aqueous acceptor solution 2...
November 2, 2016: Analytica Chimica Acta
Donatella Nardiello, Clelia Prattichizzo, Maria Teresa Rocchetti, Loreto Gesualdo, Diego Centonze
A dedicated proteomic approach based on nano-Liquid Chromatography coupled with tandem mass spectrometry in ion trap is proposed for the analysis of proteins trapped in sorbent resin cartridges used to remove inflammatory mediators from blood by coupled plasma filtration adsorption (CPFA). The final purpose of the proposed proteomic approach was to obtain a reference map of plasma proteins trapped in CPFA sorbents used for the extracorporeal blood purification of healthy pigs, with the potential impact to design new bio-filters able to control the inflammatory imbalance under pathological conditions, such as severe sepsis...
October 12, 2016: Journal of Pharmaceutical and Biomedical Analysis
Sushant B Jadhav, Rahul M Mane, Kalyanraman L Narayanan, Popatrao N Bhosale
A novel, stability indicating, reverse phase high-performance liquid chromatography (RP-HPLC) method was developed to determine the S-isomer of linagliptin (LGP) in linagliptin and metformin hydrochloride (MET HCl) tablets (LGP-MET HCl) by implementing design of experiment (DoE), i.e., two-level, full factorial design (2³ + 3 centre points = 11 experiments) to understand the critical method parameters (CMP) and its relation with the critical method attribute (CMA), and to ensure robustness of the method. The separation of the S-isomer, LGP and MET HCl in the presence of their impurities was achieved on Chiralpak(®) IA-3 (Amylose tris (3, 5-dimethylphenylcarbamate), immobilized on 3 µm silica gel) stationary phase (250 × 4...
October 17, 2016: Scientia Pharmaceutica
Suchithra Padmajan Sasikala, Kai Huang, Baptiste Giroire, Prem Prabhakaran, Lucile Henry, Alain Pénicaud, Philippe Poulin, Cyril Aymonier
We report the exfoliation of graphite and simultaneous N doping of graphene by two methods; by supercritical ammonia treatment and by liquid phase exfoliation with NH4OH. While the supercritical ammonia allowed N doping at a level of 6.4 at.% in 2 h, the liquid phase exfoliation with NH4OH allowed N doping at a level of 2.7at.% in 6 h. The N doped graphene obtained via supercritical ammonia route were few layers (<5), showed large lateral flake size (~8µm), low defect density (ID/IG<0.6) in spite of their high level of N doping...
October 20, 2016: ACS Applied Materials & Interfaces
Dong-Gue Kang, Minwook Park, Dae-Yoon Kim, Munju Goh, Namil Kim, Kwang-Un Jeong
For the development of advanced heat transfer organic materials (HTOMs) with excellent thermal conductivities, triphenylene-based reactive discogens, 2,3,6,7,10,11-hexakis(but-3-enyloxy) triphenylene (HABET) and 4,4',4'',4''',4'''',4'''''-(triphenylene-2,3,6,7,10,11-hexaylhexakis(oxy)) hexakis(butane-1-thiol) (THBT), were synthesized as discotic liquid crystal (DLC) monomers and crosslinkers, respectively. Temperature-composition phase diagram of HABET-THBT mixtures was first established based on their thermal and microscopic analyses...
October 20, 2016: ACS Applied Materials & Interfaces
Julian A Michely, Sascha K Manier, Achim T Caspar, Simon D Brandt, Jason Wallach, Hans H Maurer
3-Methoxyphencyclidine (3-MeO-PCP) and 3-methoxyrolicyclidine (3-MeO-PCPy) are two new psychoactive substances (NPS). The aims of the present study were the elucidation of their metabolic fate in rat and pooled human liver microsomes (pHLM), the identification of the cytochrome P450 (CYP) isoenzymes involved, and the detectability using standard urine screening approaches (SUSA) after intake of common users' doses using gas chromatography-mass spectrometry (GC-MS), liquid chromatography-multi-stage mass spectrometry (LC-MSn), and liquid chromatography-high-resolution tandem mass spectrometry (LC-HR-MS/MS)...
October 18, 2016: Current Neuropharmacology
Stefan C Weiss, Nicole Egetenmeyer, Wolfgang Schulz
Modern analytical test methods increasingly detect anthropogenic organic substances and their transformation products in water samples and in the environment. The presence of these compounds might pose a risk to the aquatic environment. To determine a possible (eco)toxicological risk, aquatic samples are tested using various bioassays, including sub-organismic assays such as the luminescent bacteria inhibition test, the acetylcholinesterase inhibition test, and the umu-test. The effect-directed analysis (EDA) combines physicochemical separation methods with biological (in vitro) tests...
October 19, 2016: Advances in Biochemical Engineering/biotechnology
Saijie Pan, Niels Boon, Monica Olvera de la Cruz
Epitaxial growth of DNA functionalized nanoparticles is used to grow extended superlattices with a preferred orientation for optimizing the physical properties of meta-materials for real applications. Like any solid in nature, superlattices can contain different kinds of structural defects, which significantly alter their physical properties. Further development of these materials requires a deeper understanding of, as well as precise control over, structural defect formation. Here we use Monte Carlo simulations to conduct a systematic study of the equilibrium structures of the adsorbed nanoparticle monolayers by changing the binding energies of different attachment sites...
October 18, 2016: ACS Nano
Nian Wei, Lili Hu, Lirong Song, Nanqin Gan
Micocystin (MC) exists in Microcystis cells in two different forms, free and protein-bound. We examined the dynamic change in extracellular free MCs, intracellular free MCs and protein-bound MCs in both batch cultures and semi-continuous cultures, using high performance liquid chromatography and Western blot. The results showed that the free MC per cell remained constant, while the quantity of protein-bound MCs increased with the growth of Microcystis cells in both kinds of culture. Significant changes in the dominant MC-bound proteins occurred in the late exponential growth phase of batch cultures, while the dominant MC-bound proteins in semi-continuous cultures remained the same...
October 12, 2016: Toxins
Valentina Franco, Roberto Marchiselli, Cinzia Fattore, Elena Tartara, Giovambattista De Sarro, Emilio Russo, Emilio Perucca
BACKGROUND: Perampanel, a new specific non-competitive AMPA receptor antagonist, has been recently approved in the United States and the European Union for the adjunctive treatment of focal seizures and primary generalized tonic-clonic seizures associated with idiopathic generalized epilepsy. A positive relationship between plasma perampanel concentration and improvement in seizure control has been identified in regulatory trials, suggesting that therapeutic drug monitoring (TDM) could be useful in optimizing clinical response in patients with epilepsy treated with perampanel...
October 6, 2016: Therapeutic Drug Monitoring
Sang Jun Lee, Ji Yoon Kang, Wonjoon Choi, Rhokyun Kwak
Nanofluidic resistive pulse sensing (RPS) has been extensively used to measure the size, concentration, and surface charge of nanoparticles in electrically conducting solutions. Although various methods have been explored for improving detection performances, intrinsic problems including the extremely low particle-to-pore volume ratio (<0.01%) and fast nanoparticle translocation (10-1000 µs) still induce difficulties in detection, such as low signal magnitudes and short translocation times. Herein, we present an aqueous two-phase system (ATPS) in a nanofluidic RPS for amplifying translocation signals and decreasing translocation speeds simultaneously...
October 18, 2016: Small
Yuli Hu, Shoujun Fan, Xiaobing Liao, Chao Chen, Liang Su, Xuegang Li
Berberine (BBR) is a bioactive plant ingredient derived from the roots and bark of Berberis aristata and Coptis chinensis and has a wide variety of pharmacological effects. 8-cetylberberine (8-BBR-C16) is the berberine (BBR) derivative reconstructed from adding octadecyl at C-8 of BBR to enhance its activity. This study presents a reliable method for the determination of BBR and 8-BBR-C16 in rat plasma, urine and feces. BBR and 8-BBR-C16 were determined by HPLC-UV after liquid-liquid extraction for plasma samples, and solid-phase extraction for urinary and fecal samples...
October 14, 2016: Journal of Pharmaceutical and Biomedical Analysis
Delphine Vincent, Aaron Elkins, Mark R Condina, Vilnis Ezernieks, Simone Rochfort
Cow's milk is an important source of proteins in human nutrition. On average, cow's milk contains 3.5% protein. The most abundant proteins in bovine milk are caseins and some of the whey proteins, namely beta-lactoglobulin, alpha-lactalbumin, and serum albumin. A number of allelic variants and post-translationally modified forms of these proteins have been identified. Their occurrence varies with breed, individuality, stage of lactation, and health and nutritional status of the animal. It is therefore essential to have reliable methods of detection and quantitation of these proteins...
2016: PloS One
ShuLing Wang, Hui Xu
An inorganic-organic hybrid nanocomposite (zinc oxide/polypyrrole) that represents a novel kind of coating for in-tube solid-phase microextraction is reported. The composite coating was prepared by a facile electrochemical polymerization strategy on the inner surface of a stainless steel tube. Based on the coating tube, a novel online in-tube solid-phase microextraction with liquid chromatography and mass spectrometry method was developed and applied for the extraction of three monohydroxy polycyclic aromatic hydrocarbons in human urine...
October 17, 2016: Journal of Separation Science
Mengzhe Guo, Dengyang Yin, Jie Han, Cheng Guo, Xiao Li, Liyan Zhang, Yan Du, Haibo Wang, Daoquan Tang
RATIONALE: Mass spectrometry has been developed as one of the common tools for the analysis of the organometallic systems in the gas phase over decades. The study of the fragmentation of organics-metal complexes has attracted much attention since the interesting dissociation pathways exhibited by these compounds are usually different from the protonated analogues. METHODS: In this work, iohexol complexed with different dications such as Mg(2+) , Cu(2+) , and Zn(2+) have been investigated by ESI tandem mass spectrometry...
October 17, 2016: Rapid Communications in Mass Spectrometry: RCM
Patcharanee Tawasri, Chadarat Ampasavate, Somsak Tharatha, Natthakarn Chiranthanut, Supanimit Teekachunhatean
The objective of this randomized, open-label, single-dose, two-phase crossover study was to determine the effect of ascorbic acid on pharmacokinetics of ganoderic acid A, an important biologically active triterpenoid compound with anticancer activities, following oral administration of water extract of fruiting bodies of Ling Zhi in 12 healthy male subjects. Each subject was randomized to receive either one of the two regimens: (1) a single dose of 3,000 mg of the Ling Zhi preparation or (2) a single dose of 3,000 mg of the Ling Zhi preparation in combination with 2,500 mg of ascorbic acid...
2016: BioMed Research International
Mónica Catalá-Icardo, Carmen Gómez-Benito, Ernesto Francisco Simó-Alfonso, José Manuel Herrero-Martínez
This paper describes a novel and sensitive method for extraction, preconcentration, and determination of two important widely used fungicides, azoxystrobin, and chlorothalonil. The developed methodology is based on solid-phase extraction (SPE) using a polymeric material functionalized with gold nanoparticles (AuNPs) as sorbent followed by high-performance liquid chromatography (HPLC) with diode array detector (DAD). Several experimental variables that affect the extraction efficiency such as the eluent volume, sample flow rate, and salt addition were optimized...
October 15, 2016: Analytical and Bioanalytical Chemistry
David Bouttes, Emmanuelle Gouillart, Damien Vandembroucq
The crucial role of hydrodynamic pinch-off instabilities is evidenced in the coarsening stage of viscous liquids. The phase separation of a barium borosilicate glass melt is studied by in situ synchrotron tomography at high temperature. The high viscosity contrast between the less viscous phase and the more viscous phase induces a topological symmetry breaking: capillary breakups occur preferentially in the less viscous phase. As a result, contrasting morphologies are obtained in the two phases. This symmetry breaking is illustrated on three different glass compositions, corresponding to different volume fractions of the two phases...
September 30, 2016: Physical Review Letters
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