On-cartridge derivatisation using matrix solid phase dispersion for the determination of cyclamate in foods

Energy Technology Data Exchange (ETDEWEB)

Li, Jianjun, E-mail: bootan12@126.com [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, Northwest University, Xi' an 710069 (China); National Engineering Research Center for Miniaturized Detection Systems, Xi' an 710069 (China); Liu, Yun [College of Food Engineering and Nutritional Science, Shaanxi Normal University, Xi' an 710062 (China); Liu, Qianping [National Engineering Research Center for Miniaturized Detection Systems, Xi' an 710069 (China); Hui, Junfeng [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, Northwest University, Xi' an 710069 (China); Liu, Yangzi [National Engineering Research Center for Miniaturized Detection Systems, Xi' an 710069 (China)

2017-06-15

A novel method for determination of sodium cyclamate in foods was developed. In this method, a syringe was loaded with the homogeneous mixture of the sample, KMnO{sub 4} powder and silica dispersant and used as a matrix solid phase dispersion (MSPD) reactor. As the reactor was infiltrated with small amounts of concentrated HCl, cyclamate was converted to 2-chlorocyclohexanone quickly and effectively within 5 min and determined by HPLC on a reversed-phase column using UV detection at a wavelength of 310 nm. Comparing with the traditional derivatisation in solution, the better clean-up was provided using on-cartridge derivatisation of MSPD, and much time, labor, and expense were saved. The results showed good linearity (r{sup 2} = 0.9998) over the concentration range of 1–500 mg/L. The limit of detection (LOD) and limits of quantification (LOQ) of the cyclamate were 0.3 mg/L and 1 mg/L respectively. The recoveries ranged from 91.6% to 101.3% with the relative standard deviations (RSDs) in the range of 2.5%–4.3%. - Highlights: • A novel method was developed for the determination of cyclamate in foods. • On cartridge derivatisation, using matrix solid phase dispersion, was developed. • A new derivatisation reaction for cyclamate conversion to 2-chlorocyclohexanone was developed. • The method was rapid, simple, inexpensive, effective.

Liquid chromatography tandem mass spectrometry method using solid-phase extraction and bead-beating-assisted matrix solid-phase dispersion to quantify the fungicide tebuconazole in controlled frog exposure study: analysis of water and animal tissue

DEFF Research Database (Denmark)

Hansen, Martin; Poulsen, Rikke; Luong, Xuan

2014-01-01

and on tissue from exposed and non-exposed adult X. laevis. Using solid-phase extraction (SPE), the analytical method allows for quantification of tebuconazole at concentrations as low as 3.89 pg mL(-1) in 10 mL water samples. Using bead-beating-assisted matrix solid-phase dispersion (MSPD), it was possible...

Solid KHT tumor dispersal for flow cytometric cell kinetic analysis

International Nuclear Information System (INIS)

Pallavicini, M.G.; Folstad, L.J.; Dunbar, C.

1981-01-01

A bacterial neutral protease was used to disperse KHT solid tumors into single cell suspensions suitable for routine cell kinetic analysis by flow cytometry and for clonogenic cell survival. Neutral protease disaggregation under conditions which would be suitable for routine tumor dispersal was compared with a trypsin/DNase procedure. Cell yield, clonogenic cell survival, DNA distributions of untreated and drug-perturbed tumors, rates of radioactive precursor incorporation during the cell cycle, and preferential cell cycle phase-specific cell loss were investigated. Tumors dispersed with neutral protease yielded approximately four times more cells than those dispersed with trypsin/DNase and approximately a 1.5-fold higher plating efficiency in a semisolid agar system. Quantitative analysis of DNA distributions obtained from untreated and cytosine-arabinoside-perturbed tumors produced similar results with both dispersal procedures. The rates of incorporation of tritiated thymidine during the cell cycle were also similar with neutral protease and trypsin/DNase dispersal. Preferential phase-specific cell loss was not obseved with either technique. We find that neutral protease provides good single cell suspensions of the KHT tumor for cell survival measurements and for cell kinetic analysis of drug-induced perturbations by flow cytometry. In addition, the high cell yields facilitate electronic cell sorting where large numbers of cells are often required

The growth and tensile deformation behavior of the silver solid solution phase with zinc

International Nuclear Information System (INIS)

Wu, Jiaqi; Lee, Chin C.

2016-01-01

The growth of homogeneous silver solid solution phase with zinc are conducted at two different compositions. X-ray diffraction (XRD) and Scanning electron microscope/Energy dispersive X-ray spectroscopy (SEM/EDX) are carried out for phase identification and chemical composition verification. The mechanical properties of silver solid solution phase with zinc are evaluated by tensile test. The engineering and true stress vs. strain curves are presented and analyzed, with those of pure silver in comparison. According to the experimental results, silver solid solution phase with zinc at both compositions show tempered yield strength, high tensile strength and large uniform strain compared to those of pure silver. Fractography further confirmed the superior ductility of silver solid solution phase with zinc at both compositions. Our preliminary but encouraging results may pave the way for the silver based alloys to be applied in industries such as electronic packaging and structure engineering.

Core-shell Fe3O4 polydopamine nanoparticles as sorbent for magnetic dispersive solid-phase extraction of copper from food samples.

Science.gov (United States)

Yavuz, Emre; Tokalıoğlu, Şerife; Patat, Şaban

2018-10-15

In the present study, core-shell Fe 3 O 4 polydopamine nanoparticles were synthesized and used for the first time as an adsorbent for the vortex assisted magnetic dispersive solid phase extraction of copper from food samples. After elution, copper in the solutions was determined by FAAS. The adsorbent was characterized using X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller surface area, and zeta potential measurements. Various parameters affecting the magnetic dispersive solid-phase extraction were evaluated. The optimum pH and magnetic adsorbent amount were found to be 5 and 40 mg, respectively. Elution was made by 3 mL of 2 mol L -1 HNO 3 .The major advantage of the method is the fast equilibration during adsorption without the need for vortexing or shaking. The preconcentration factor and detection limit of the method were found to be 150 and 0.22 mg L -1 , respectively. The precision (as RSD%) and adsorption capacity of the method were 3.7% and 28 mg g -1 , respectively. The method was successfully verified by analyzing four certified reference materials (SPS-WW1 Batch 114 Wastewater, TMDA-53.3 Lake water, BCR-482 Lichen and 1573a Tomato Leaves) and by addition/recovery tests of copper standard solution in organic baby food, muesli, macaroni, honey, and milk samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

Liquid-liquid and liquid-solid phase separation and flocculation for a charged colloidal dispersion

International Nuclear Information System (INIS)

Lai, S.K.; Wu, K.L.

2002-01-01

We model the intercolloidal interaction by a hard-sphere Yukawa repulsion to which is added the long-range van der Waals attraction. In comparison with the Derjaguin-Landau-Verwey-Overbeek repulsion, the Yukawa repulsion explicitly incorporates the spatial correlations between colloids and small ions. As a result, the repulsive part can be expressed analytically and has a coupling strength depending on the colloidal volume fraction. By use of this two-body potential of mean force and in conjunction with a second-order thermodynamic perturbation theory, we construct the colloidal Helmholtz free energy and use it to calculate the thermodynamic quantities, pressure and chemical potential, needed in the determination of the liquid-liquid and liquid-solid phase diagrams. We examine, in an aqueous charged colloidal dispersion, the effects of the Hamaker constant and particle size on the conformation of a stable liquid-liquid phase transition calculated with respect to the liquid-solid coexistence phases. We find that there exists a threshold Hamaker constant or particle size whose value demarcates the stable liquid-liquid coexistence phases from their metastable counterparts. Applying the same technique and using the energetic criterion, we extend our calculations to study the flocculation phenomenon in aqueous charged colloids. Here, we pay due attention to determining the loci of a stability curve stipulated for a given temperature T 0 , and obtain the parametric phase diagram of the Hamaker constant vs the coupling strength or, at given surface potential, the particle size. By imposing T 0 to be the critical temperature T c , i.e., setting k B T 0 (=k B T c ) equal to a reasonable potential barrier, we arrive at the stability curve that marks the irreversible reversible phase transition. The interesting result is that there occurs a minimum size for the colloidal particles below (above) which the colloidal dispersion is driven to an irreversible (reversible) phase

Physicochemical characterization of tacrolimus-loaded solid dispersion with sodium carboxylmethyl cellulose and sodium lauryl sulfate.

Science.gov (United States)

Park, Young-Joon; Ryu, Dong-Sung; Li, Dong Xun; Quan, Qi Zhe; Oh, Dong Hoon; Kim, Jong Oh; Seo, Youn Gee; Lee, Young-Im; Yong, Chul Soon; Woo, Jong Soo; Choi, Han-Gon

2009-06-01

To develop a novel tacrolimus-loaded solid dispersion with improved solubility, various solid dispersions were prepared with various ratios of water, sodium lauryl sulfate, citric acid and carboxylmethylcellulose-Na using spray drying technique. The physicochemical properties of solid dispersions were investigated using scanning electron microscopy, differential scanning calorimetery and powder X-ray diffraction. Furthermore, their solubility and dissolution were evaluated compared to drug powder. The solid dispersion at the tacrolimus/CMC-Na/sodium lauryl sulfate/citric acid ratio of 3/24/3/0.2 significantly improved the drug solubility and dissolution compared to powder. The scanning electron microscopy result suggested that carriers might be attached to the surface of drug in this solid dispersion. Unlike traditional solid dispersion systems, the crystal form of drug in this solid dispersion could not be converted to amorphous form, which was confirmed by the analysis of DSC and powder X-ray diffraction. Thus, the solid dispersion system with water, sodium lauryl sulfate, citric acid and CMC-Na should be a potential candidate for delivering a poorly water-soluble tacrolimus with enhanced solubility and no convertible crystalline.

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction for the determination of sulfonamides in animal tissues using high-performance liquid chromatography.

Science.gov (United States)

Wang, Zhibing; He, Mengyu; Jiang, Chunzhu; Zhang, Fengqing; Du, Shanshan; Feng, Wennan; Zhang, Hanqi

2015-12-01

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction was developed and applied to the extraction of some sulfonamides, including sulfamerazine, sulfamethazine, sulfathiazole, sulfachloropyridazine, sulfadoxine, sulfisoxazole, and sulfaphenazole, in animal tissues. High-performance liquid chromatography was applied to the separation and determination of the target analytes. The solid sample was directly treated by matrix solid-phase dispersion and the eluate obtained was treated by homogeneous ionic liquid microextraction. The ionic liquid was used as the extraction solvent in this method, which may result in the improvement of the recoveries of the target analytes. To avoid using organic solvent and reduce environmental pollution, water was used as the elution solvent of matrix solid-phase dispersion. The effects of the experimental parameters on recoveries, including the type and volume of ionic liquid, type of dispersant, ratio of sample to dispersant, pH value of elution solvent, volume of elution solvent, amount of salt in eluate, amount of ion-pairing agent (NH4 PF6 ), and centrifuging time, were evaluated. When the present method was applied to the analysis of animal tissues, the recoveries of the analytes ranged from 85.4 to 118.0%, and the relative standard deviations were lower than 9.30%. The detection limits for the analytes were 4.3-13.4 μg/kg. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Polypyrrole-magnetite dispersive micro-solid-phase extraction combined with ultraviolet-visible spectrophotometry for the determination of rhodamine 6G and crystal violet in textile wastewater.

Science.gov (United States)

Kamaruddin, Amirah Farhan; Sanagi, Mohd Marsin; Wan Ibrahim, Wan Aini; Md Shukri, Dyia S; Abdul Keyon, Aemi S

2017-11-01

Polypyrrole-magnetite dispersive micro-solid-phase extraction method combined with ultraviolet-visible spectrophotometry was developed for the determination of selected cationic dyes in textile wastewater. Polypyrrole-magnetite was used as adsorbent due to its thermal stability, magnetic properties, and ability to adsorb Rhodamine 6G and crystal violet. Dispersive micro-solid-phase extraction parameters were optimized, including sample pH, adsorbent amount, extraction time, and desorption solvent. The optimum polypyrrole-magnetite dispersive micro-solid phase-extraction conditions were sample pH 8, 60 mg polypyrrole-magnetite adsorbent, 5 min of extraction time, and acetonitrile as the desorption solvent. Under the optimized conditions, the polypyrrole-magnetite dispersive micro-solid-phase extraction with ultraviolet-visible method showed good linearity in the range of 0.05-7 mg/L (R 2  > 0.9980). The method also showed a good limit of detection for the dyes (0.05 mg/L) and good analyte recoveries (97.4-111.3%) with relative standard deviations extraction and determination of dyes at trace concentration levels. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Relating hydrogen-bonding interactions with the phase behavior of naproxen/PVP K 25 solid dispersions: evaluation of solution-cast and quench-cooled films.

Science.gov (United States)

Paudel, Amrit; Nies, Erik; Van den Mooter, Guy

2012-11-05

In this work, we investigated the relationship between various intermolecular hydrogen-bonding (H-bonding) interactions and the miscibility of the model hydrophobic drug naproxen with the hydrophilic polymer polyvinylpyrrolidone (PVP) across an entire composition range of solid dispersions prepared by quasi-equilibrium film casting and nonequilibrium melt quench cooling. The binary phase behavior in solid dispersions exhibited substantial processing method dependence. The solid state solubility of crystalline naproxen in PVP to form amorphous solid dispersions was 35% and 70% w/w naproxen in solution-cast films and quench-cooled films, respectively. However, the presence of a single mixed phase glass transition indicated the amorphous miscibility to be 20% w/w naproxen for the films, beyond which amorphous-amorphous and/or crystalline phase separations were apparent. This was further supported by the solution state interactions data such as PVP globular size distribution and solution infrared spectral profiles. The borderline melt composition showed cooling rate dependence of amorphization. The glass transition and melting point depression profiles of the system were treated with the analytical expressions based on Flory-Huggins mixing theory to interpolate the equilibrium solid solubility. FTIR analysis and subsequent spectral deconvolution revealed composition and miscibility dependent variations in the strength of drug-polymer intermolecular H-bonding. Two types of H-bonded populations were evidenced from 25% w/w and 35% w/w naproxen in solution-cast films and quench-cooled films, respectively, with the higher fraction of strongly H-bonded population in the drug rich domains of phase separated amorphous film compositions and highly drug loaded amorphous quench-cooled dispersions.

Comparison of spray drying, electroblowing and electrospinning for preparation of Eudragit E and itraconazole solid dispersions.

Science.gov (United States)

Sóti, Péter Lajos; Bocz, Katalin; Pataki, Hajnalka; Eke, Zsuzsanna; Farkas, Attila; Verreck, Geert; Kiss, Éva; Fekete, Pál; Vigh, Tamás; Wagner, István; Nagy, Zsombor K; Marosi, György

2015-10-15

Three solvent based methods: spray drying (SD), electrospinning (ES) and air-assisted electrospinning (electroblowing; EB) were used to prepare solid dispersions of itraconazole and Eudragit E. Samples with the same API/polymer ratios were prepared in order to make the three technologies comparable. The structure and morphology of solid dispersions were identified by scanning electron microscopy and solid phase analytical methods such as, X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC) and Raman chemical mapping. Moreover, the residual organic solvents of the solid products were determined by static headspace-gas chromatography/mass spectroscopy measurements and the wettability of samples was characterized by contact angle measurement. The pharmaceutical performance of the three dispersion type, evaluated by dissolution tests, proved to be very similar. According to XRPD and DSC analyses, made after the production, all the solid dispersions were free of any API crystal clusters but about 10 wt% drug crystallinity was observed after three months of storage in the case of the SD samples in contrast to the samples produced by ES and EB in which the polymer matrix preserved the API in amorphous state. Copyright © 2015 Elsevier B.V. All rights reserved.

Structural diversity of solid dispersions of acetylsalicylic acid as seen by solid-state NMR.

Science.gov (United States)

Policianova, Olivia; Brus, Jiri; Hruby, Martin; Urbanova, Martina; Zhigunov, Alexander; Kredatusova, Jana; Kobera, Libor

2014-02-03

Solid dispersions of active pharmaceutical ingredients are of increasing interest due to their versatile use. In the present study polyvinylpyrrolidone (PVP), poly[N-(2-hydroxypropyl)-metacrylamide] (pHPMA), poly(2-ethyl-2-oxazoline) (PEOx), and polyethylene glycol (PEG), each in three Mw, were used to demonstrate structural diversity of solid dispersions. Acetylsalicylic acid (ASA) was used as a model drug. Four distinct types of the solid dispersions of ASA were created using a freeze-drying method: (i) crystalline solid dispersions containing nanocrystalline ASA in a crystalline PEG matrix; (ii) amorphous glass suspensions with large ASA crystallites embedded in amorphous pHPMA; (iii) solid solutions with molecularly dispersed ASA in rigid amorphous PVP; and (iv) nanoheterogeneous solid solutions/suspensions containing nanosized ASA clusters dispersed in a semiflexible matrix of PEOx. The obtained structural data confirmed that the type of solid dispersion can be primarily controlled by the chemical constitutions of the applied polymers, while the molecular weight of the polymers had no detectable impact. The molecular structure of the prepared dispersions was characterized using solid-state NMR, wide-angle X-ray scattering (WAXS), and differential scanning calorimetry (DSC). By applying various (1)H-(13)C and (1)H-(1)H correlation experiments combined with T1((1)H) and T1ρ((1)H) relaxation data, the extent of the molecular mixing was determined over a wide range of distances, from intimate intermolecular contacts (0.1-0.5 nm) up to the phase-separated nanodomains reaching ca. 500 nm. Hydrogen-bond interactions between ASA and polymers were probed by the analysis of (13)C and (15)N CP/MAS NMR spectra combined with the measurements of (1)H-(15)N dipolar profiles. Overall potentialities and limitations of individual experimental techniques were thoroughly evaluated.

Trace and ultratrace determination of heavy metal ions by energy-dispersive X-ray fluorescence spectrometry using graphene as solid sorbent in dispersive micro solid-phase extraction

Energy Technology Data Exchange (ETDEWEB)

Kocot, Karina; Sitko, Rafal, E-mail: rafal.sitko@us.edu.pl

2014-04-01

In this paper, the adsorptive properties of graphene nanosheets were used for simultaneous preconcentration of cobalt, nickel, copper and lead ions from water samples. The developed methodology is based on dispersive micro-solid phase extraction (DMSPE) which is miniaturized and a simplified version of classical solid phase extraction technique. In proposed procedure only 200 μL of suspension containing graphene (0.2 mg), ammonium pyrrolidine dithiocarbamate (APDC) (0.8 mg) and Triton-X-100 (0.1 mg) is rapidly injected to 50 mL of water sample. Then, graphene nanosheets with adsorbed metal-APDC chelates are collected on membrane filter and measured using energy-dispersive X-ray fluorescence (EDXRF) spectrometry. The various parameters including pH, amount of APDC, sample volume, amount of Triton-X-100 and sorption time were optimized in order to obtain the best recoveries. The experiment shows that Co, Ni, Cu and Pb can be simultaneously preconcentrated at pH of 5 with high recoveries (97%, 96%, 99% and 96% for Co, Ni, Cu and Pb, respectively) and very good precision (RSDs within 2.6–3.4%). Due to the excellent enrichment factors ranging from 400 to 2500 the proposed DMSPE–EDXRF procedure offers low detection limits. For optimized measurement conditions (voltage and current of X-ray tube, primary beam filter) the detection limits are even 0.08, 0.07, 0.08 and 0.20 ng mL{sup −1} for Co, Ni, Cu and Pb, respectively. - Highlights: • Excellent detection limits using EDXRF • A new preconcentration procedure combining DMSPE and EDXRF measurement • Graphene as a promising and efficient solid sorbent in DMSPE • Simple, fast, inexpensive and environmental friendly method.

Simultaneous determination of phenolic compounds in Equisetum palustre L. by ultra high performance liquid chromatography with tandem mass spectrometry combined with matrix solid-phase dispersion extraction.

Science.gov (United States)

Wei, Zuofu; Pan, Youzhi; Li, Lu; Huang, Yuyang; Qi, Xiaolin; Luo, Meng; Zu, Yuangang; Fu, Yujie

2014-11-01

A method based on matrix solid-phase dispersion extraction followed by ultra high performance liquid chromatography with tandem mass spectrometry is presented for the extraction and determination of phenolic compounds in Equisetum palustre. This method combines the high efficiency of matrix solid-phase dispersion extraction and the rapidity, sensitivity, and accuracy of ultra high performance liquid chromatography with tandem mass spectrometry. The influential parameters of the matrix solid-phase dispersion extraction were investigated and optimized. The optimized conditions were as follows: silica gel was selected as dispersing sorbent, the ratio of silica gel to sample was selected to be 2:1 (400/200 mg), and 8 mL of 80% methanol was used as elution solvent. Furthermore, a fast and sensitive ultra high performance liquid chromatography with tandem mass spectrometry method was developed for the determination of nine phenolic compounds in E. palustre. This method was carried out within <6 min, and exhibited satisfactory linearity, precision, and recovery. Compared with ultrasound-assisted extraction, the proposed matrix solid-phase dispersion procedure possessed higher extraction efficiency, and was more convenient and time saving with reduced requirements on sample and solvent amounts. All these results suggest that the developed method represents an excellent alternative for the extraction and determination of active components in plant matrices. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development of solid dispersion systems of dapivirine to enhance its solubility.

Science.gov (United States)

Gorajana, Adinarayana; Ying, Chan Chiew; Shuang, Yeen; Fong, Pooi; Tan, Zhi; Gupta, Jyoti; Talekar, Meghna; Sharma, Manisha; Garg, Sanjay

2013-06-01

Dapivirine, formerly known as TMC 120, is a poorly-water soluble anti-HIV drug, currently being developed as a vaginal microbicide. The clinical use of this drug has been limited due to its poor solubility. The aim of this study was to design solid dispersion systems of Dapivirine to improve its solubility. Solid dispersions were prepared by solvent and fusion methods. Dapivirine release from the solid dispersion system was determined by conducting in-vitro dissolution studies. The physicochemical characteristics of the drug and its formulation were studied using Differential Scanning Calorimetry (DSC), powder X-ray Diffraction (XRD), Fourier-transform Infrared Spectroscopy (FTIR) and Scanning Electron Microscopy (SEM). A significant improvement in drug dissolution rate was observed with the solid dispersion systems. XRD, SEM and DSC results indicated the transformation of pure Dapivirine which exists in crystalline form into an amorphous form in selected solid dispersion formulations. FTIR and HPLC analysis confirmed the absence of drug-excipient interactions. Solid dispersion systems can be used to improve the dissolution rate of Dapivirine. This improvement could be attributed to the reduction or absence of drug crystallinity, existence of drug particles in an amorphous form and improved wettability of the drug.

Solubility enhancement of benfotiamine, a lipid derivative of thiamine by solid dispersion technique.

Science.gov (United States)

Patel, S M; Patel, R P; Prajapati, B G

2012-03-01

The present study was aimed to increase the solubility of the poorly water soluble drug benfotiamine using hydrophilic polymers (PVP K-30 and HPMC E4). Solid dispersions were prepared by kneading method. Phase solubility study, in-vitro dissolution of pure drug, physical mixtures and solid dispersions were carried out. PVP and HPMC were found to be effective in increasing the dissolution of Benfotiamine in solid dispersions when compared to pure drug. FT-IR, differential scanning calorimetry and X-ray diffractometry studies were carried out in order to characterize the drug and solid dispersion. To conclude that, the prepared solid dispersion of PVP-30 may to effectively used for the enhancement of solubility of poorly water soluble drugs such as benfotiamine.

Solubility enhancement of benfotiamine, a lipid derivative of thiamine by solid dispersion technique

Directory of Open Access Journals (Sweden)

S M Patel

2012-01-01

Full Text Available The present study was aimed to increase the solubility of the poorly water soluble drug benfotiamine using hydrophilic polymers (PVP K-30 and HPMC E4. Solid dispersions were prepared by kneading method. Phase solubility study, in-vitro dissolution of pure drug, physical mixtures and solid dispersions were carried out. PVP and HPMC were found to be effective in increasing the dissolution of Benfotiamine in solid dispersions when compared to pure drug. FT-IR, differential scanning calorimetry and X-ray diffractometry studies were carried out in order to characterize the drug and solid dispersion. To conclude that, the prepared solid dispersion of PVP-30 may to effectively used for the enhancement of solubility of poorly water soluble drugs such as benfotiamine.

Extraction of acetanilides in rice using ionic liquid-based matrix solid phase dispersion-solvent flotation.

Science.gov (United States)

Zhang, Liyuan; Wang, Changyuan; Li, Zuotong; Zhao, Changjiang; Zhang, Hanqi; Zhang, Dongjie

2018-04-15

Ionic liquid-based matrix solid phase dispersion-solvent flotation coupled with high performance liquid chromatography was developed for the determination of the acetanilide herbicides, including metazachlor, propanil, alachlor, propisochlor, pretilachlor, and butachlor in rice samples. Some experimental parameters, including the type of dispersant, the mass ratio of dispersant to sample, pH of sample solution, the type of extraction solvent, the type of ionic liquid, flotation time, and flow rate of N 2 were optimized. The average recoveries of the acetanilide herbicides at spiked concentrations of 50, 125, and 250 µg/kg ranged from 89.4% to 108.7%, and relative standard deviations were equal to or lower than 7.1%, the limits of quantification were in the range of 38.0 to 84.7 µg/kg. Copyright © 2017 Elsevier Ltd. All rights reserved.

The Stabilization of Amorphous Zopiclone in an Amorphous Solid Dispersion.

Science.gov (United States)

Milne, Marnus; Liebenberg, Wilna; Aucamp, Marique

2015-10-01

Zopiclone is a poorly soluble psychotherapeutic agent. The aim of this study was to prepare and characterize an amorphous form of zopiclone as well as the characterization and performance of a stable amorphous solid dispersion. The amorphous form was prepared by the well-known method of quench-cooling of the melt. The solid dispersion was prepared by a solvent evaporation method of zopiclone, polyvinylpyrrolidone-25 (PVP-25), and methanol, followed by freeze-drying. The physico-chemical properties and stability of amorphous zopiclone and the solid dispersion was studied using differential scanning calorimetry (DSC), infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), hot-stage microscopy (HSM), X-ray diffractometry (XRD), solubility, and dissolution studies. The zopiclone amorphous solid-state form was determined to be a fragile glass; it was concluded that the stability of the amorphous form is influenced by both temperature and water. Exposure of amorphous zopiclone to moisture results in rapid transformation of the amorphous form to the crystalline dihydrated form. In comparison, the amorphous solid dispersion proved to be more stable with increased aqueous solubility.

Determination of six pesticides in the medicinal herb Cordia salicifolia by matrix solid-phase dispersion and gas chromatography/mass spectrometry.

Science.gov (United States)

de Carvalho, Pedro Henrique Viana; Prata, Vanessa de Menezes; Alves, Péricles Barreto; Navickiene, Sandro

2009-01-01

A simple and effective extraction method based on matrix solid-phase dispersion was developed for acephate, chlorpropham, pyrimicarb, bifenthrin, tetradifon, and phosalone in leaves of the medicinal plant Cordia salicifolia, whose extracts are commercialized in Brazil as diuretic, appetite suppressant, and weight loss products. The determination method was GC/MS with selected-ion monitoring. Different parameters of the method were evaluated, such as type of solid phase (C18, alumina, silica gel, and Florisil) and the amount of solid phase and eluent (dichloromethane, ethyl acetate, chloroform, and cyclohexane). The best results were obtained using 0.5 g herb sample, 0.5 g neutral alumina as the dispersant sorbent, 0.5 g C18 as the cleanup sorbent, and cyclohexane-dichloromethane (3 + 1, v/v) as the eluting solvent. The method was validated using herb samples fortified with pesticides at different concentration levels (0.3, 0.5, and 1.0 mg/kg). Average recoveries (seven replicates) ranged from 67.7 to 129.9%, with relative standard deviations between 6.3 and 26%. Detection and quantitation limits for the herb ranged from 0.10 to 0.15 and 0.15 to 0.25 mg/kg, respectively.

Efficient sample preparation method based on solvent-assisted dispersive solid-phase extraction for the trace detection of butachlor in urine and waste water samples.

Science.gov (United States)

Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

2016-10-01

In this work, an efficient sample preparation method termed solvent-assisted dispersive solid-phase extraction was applied. The used sample preparation method was based on the dispersion of the sorbent (benzophenone) into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was achieved by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the butachlor, the cloudy solution was centrifuged and butachlor in the sediment phase dissolved in ethanol and determined by gas chromatography with flame ionization detection. Under the optimized conditions (solution pH = 7.0, sorbent: benzophenone, 2%, disperser solvent: ethanol, 500 μL, centrifuged at 4000 rpm for 3 min), the method detection limit for butachlor was 2, 3 and 3 μg/L for distilled water, waste water, and urine sample, respectively. Furthermore, the preconcentration factor was 198.8, 175.0, and 174.2 in distilled water, waste water, and urine sample, respectively. Solvent-assisted dispersive solid-phase extraction was successfully used for the trace monitoring of butachlor in urine and waste water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Enhancing the bioavailability of magnolol in rabbits using melting solid dispersion with polyvinylpyrrolidone.

Science.gov (United States)

Lin, Shiuan-Pey; Hou, Yu-Chi; Liao, Tzu-Yun; Tsai, Shang-Yuan

2014-03-01

Preparation of magnolol-loaded amorphous solid dispersion was investigated for improving the bioavailability. A solid dispersion of magnolol was prepared with polyvinylpyrrolidone K-30 (PVP) by melting method, and the physical properties were characterized by using differential scanning calorimetry, powder X-ray diffractometry, Fourier transformation-infrared spectroscopy and scanning electron microscope. In addition, dissolution test was also performed. Subsequently, the bioavailability of magnolol pure compound, its physical mixture and solid dispersion were compared in rabbits. The blood samples withdrawn via marginal ear vein at specific time points were assayed by HPLC method. Oral administration of the solid dispersion of magnolol with PVP significantly increased the systemic exposures of magnolol and magnolol sulfates/glucuronides by 80.1% and 142.8%, respectively, compared to those given with magnolol pure compound. Magnolol-loaded amorphous solid dispersion with PVP has demonstrated enhanced bioavailability of magnolol in rabbits.

Application of zein-modified magnetite nanoparticles in dispersive magnetic micro-solid-phase extraction of synthetic food dyes in foodstuffs.

Science.gov (United States)

Jangju, Azam; Farhadi, Khalil; Hatami, Mehdi; Amani, Samireh; Esma-Ali, Farzan; Moshkabadi, Aisan; Hajilari, Fatemeh

2017-03-01

A simple method for the simultaneous and trace analysis of four synthetic food azo dyes including carmoisine, ponceau 4R, sunset yellow, and allura red from some foodstuff samples was developed by combining dispersive μ-solid-phase extraction and high-performance liquid chromatography with diode array detection. Zein-modified magnetic Fe 3 O 4 nanoparticles were prepared and used for μ-solid-phase extraction of trace amounts of mentioned food dyes. The prepared modified magnetic nanoparticles were characterized by scanning electron microscopy and FTIR spectroscopy. The factors affecting the extraction of the target analytes such as pH, amount of sorbent, extraction time, type and volume of the desorption eluent, and desorption time were investigated. Under the optimized conditions, the method provided good repeatability with relative standard deviations lower than 5.8% (n = 9). Limit of detection values ranged between 0.3 and 0.9 ng/mL with relatively high enrichment factors (224-441). Comparing the obtained results indicated that Fe 3 O 4 nanoparticles modified by zein biopolymer show better analytical application than bare magnetic nanoparticles. The proposed method was also applied for the determination of target synthetic food dyes in foodstuff samples such as carbonated beverage, snack, and candy samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Selective Dispersive Solid Phase Extraction of Ser-traline Using Surface Molecularly Imprinted Polymer Grafted on SiO2/Graphene Oxide

Directory of Open Access Journals (Sweden)

Faezeh Khalilian

2017-01-01

Full Text Available A surface molecularly imprinted dispersive solid phase extraction coupled with liquid chromatography–ultraviolet detection is proposed as a selective and fast clean-up technique for the determination of sertraline in biological sample. Surface sertraline-molecular imprinted polymer was grafted and synthesized on the SiO2/graphene oxide surface. Firstly SiO2 was coated on synthesized graphene oxide sheet using sol-gel technique. Prior to polymerization, the vinyl group was incorporated on to the surface of SiO2/graphene oxide to direct selective polymerization on the surface. Methacrylic acid, ethylene glycol dimethacrylate and ethanol were used as monomer, cross-linker and progen, respectively. Non-imprinted polymer was also prepared for comparing purposes. The properties of the molecular imprinted polymer were characterized using field emission-scanning electron microscopy and Fourier transform infrared spectroscopy methods. The surface molecular imprinted polymer was utilized as an adsorbent of dispersive solid phase extraction for separation and preconcentration of sertraline. The effects of the different parameters influencing the extraction efficiency, such as sample pH were investigated and optimized. The specificity of the molecular imprinted polymer over the non-imprinted polymer was examined in absence and presence of competitive drugs. Sertraline calibration curve showed linearity in the ranges 1–500 µg L-1. The limits of detection and quantification under optimized conditions were obtained 0.2 and 0.5 µg L-1. The within-day and between-day relative standard deviations (n=3 were 4.3 and 7.1%, respectively. Furthermore, the relative recoveries for spiked biological samples were above 92%.

In-line micro-matrix solid-phase dispersion extraction for simultaneous separation and extraction of Sudan dyes in different spices.

Science.gov (United States)

Rajabi, Maryam; Sabzalian, Sedigheh; Barfi, Behruz; Arghavani-Beydokhti, Somayeh; Asghari, Alireza

2015-12-18

A novel, simple, fast, and miniaturized method, termed in-line micro-matrix solid-phase dispersion (in-line MMSPD), coupled with high performance liquid chromatography (HPLC) was developed for the simultaneous extraction and determination of Sudan dyes (i.e. Sudan I-IV, Sudan orange G, Sudan black B, and Sudan red G) with the aid of an experimental design strategy. In this method, a matrix solid-phase dispersion (MSPD) column including a suitable mixture of polar sorbents was inserted in the mobile phase pathway, and while the interfering compounds were retained, the analytes were eluted and entered into the analytical column. In this way, the extraction, elution, and separation of the analytes were performed sequentially. Under the optimal experimental conditions (including the amount of sample, 0.0426g; amount of dispersant phase, 0.0216g of florisil, 0.0227g of silica, 0.0141g of alumina; and blending time, 112s), the limits of detection (LODs), limits of quantification, linear dynamic ranges, and recoveries were obtained to be 0.3-15.3μgkg(-1), 1-50μgkg(-1), 50-28,000μgkg(-1), and 94.5-99.1%, respectively. The results obtained showed that determination of the selected Sudan dyes in food samples using an enough sensitive and a simple analytically validated method like in-line MMSPD may offer a suitable screening method, which could be useful for food analysis and adulteration. Copyright © 2015 Elsevier B.V. All rights reserved.

Picosecond phase-velocity dispersion of hypersonic phonons imaged with ultrafast electron microscopy

International Nuclear Information System (INIS)

Cremons, Daniel R.; Du, Daniel X.; Flannigan, David J.

2017-01-01

We describe the direct imaging—with four-dimensional ultrafast electron microscopy—of the emergence, evolution, dispersion, and decay of photoexcited, hypersonic coherent acoustic phonons in nanoscale germanium wedges. Coherent strain waves generated via ultrafast in situ photoexcitation were imaged propagating with initial phase velocities of up to 35 km/s across discrete micrometer-scale crystal regions. We then observe that, while each wave front travels at a constant velocity, the entire wave train evolves with a time-varying phase-velocity dispersion, displaying a single-exponential decay to the longitudinal speed of sound (5 km/s) and with a mean lifetime of 280 ps. We also find that the wave trains propagate along a single in-plane direction oriented parallel to striations introduced during specimen preparation, independent of crystallographic direction. Elastic-plate modeling indicates the dynamics arise from excitation of a single, symmetric (dilatational) guided acoustic mode. Further, by precisely determining the experiment time-zero position with a plasma-lensing method, we find that wave-front emergence occurs approximately 100 ps after femtosecond photoexcitation, which matches well with Auger recombination times in germanium. We conclude by discussing the similarities between the imaged hypersonic strain-wave dynamics and electron/hole plasma-wave dynamics in strongly photoexcited semiconductors.

Picosecond phase-velocity dispersion of hypersonic phonons imaged with ultrafast electron microscopy

Science.gov (United States)

Cremons, Daniel R.; Du, Daniel X.; Flannigan, David J.

2017-12-01

Here, we describe the direct imaging—with four-dimensional ultrafast electron microscopy—of the emergence, evolution, dispersion, and decay of photoexcited, hypersonic coherent acoustic phonons in nanoscale germanium wedges. Coherent strain waves generated via ultrafast in situ photoexcitation were imaged propagating with initial phase velocities of up to 35 km/s across discrete micrometer-scale crystal regions. We observe that, while each wave front travels at a constant velocity, the entire wave train evolves with a time-varying phase-velocity dispersion, displaying a single-exponential decay to the longitudinal speed of sound (5 km/s) and with a mean lifetime of 280 ps. We also find that the wave trains propagate along a single in-plane direction oriented parallel to striations introduced during specimen preparation, independent of crystallographic direction. Elastic-plate modeling indicates the dynamics arise from excitation of a single, symmetric (dilatational) guided acoustic mode. Further, by precisely determining the experiment time-zero position with a plasma-lensing method, we find that wave-front emergence occurs approximately 100 ps after femtosecond photoexcitation, which matches well with Auger recombination times in germanium. We conclude by discussing the similarities between the imaged hypersonic strain-wave dynamics and electron/hole plasma-wave dynamics in strongly photoexcited semiconductors.

Determination of Iron Species by Combination of Solvent Assisted-Dispersive Solid Phase Extraction and Spectrophotometry

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Zahra Dehghani

2015-06-01

Full Text Available A simple, rapid and sensitive solvent assisted-dispersive solid phase extraction method was developed for the extraction of iron(II prior to its spectrophotometric determination. The Fe(II reacted with 2,4,6-tris(2-pyridyl-1,3,5-triazine, neutralized with sodium dodecyl sulfate and extracted onto the fine particles of benzophenone which were formed upon rapid injection of a mixture of benzophenone as the sorbent and ethanol as the disperser solvent into the aqueous solution. After phase separation, the sedimented phase containing the complex was dissolved in ethanol and the analyte concentration was determined by measuring its absorption at 594 nm. Total iron was determined after the reduction of Fe(III to Fe(II with hydroxylamine hydrochloride. Under the optimized conditions, an enhancement factor of 32, the detection limit of 0.16 µg l-1, and the relative standard deviation of 1.9% (n = 6 at 20 µg l-1 concentration level of Fe(II were achieved. The method was successfully applied to the determination of iron species in water samples and total iron in infant dry formula milk, apple, rice, spinach and parsley samples.

Mathematical modeling of disperse two-phase flows

CERN Document Server

Morel, Christophe

2015-01-01

This book develops the theoretical foundations of disperse two-phase flows, which are characterized by the existence of bubbles, droplets or solid particles finely dispersed in a carrier fluid, which can be a liquid or a gas. Chapters clarify many difficult subjects, including modeling of the interfacial area concentration. Basic knowledge of the subjects treated in this book is essential to practitioners of Computational Fluid Dynamics for two-phase flows in a variety of industrial and environmental settings. The author provides a complete derivation of the basic equations, followed by more advanced subjects like turbulence equations for the two phases (continuous and disperse) and multi-size particulate flow modeling. As well as theoretical material, readers will discover chapters concerned with closure relations and numerical issues. Many physical models are presented, covering key subjects including heat and mass transfers between phases, interfacial forces and fluid particles coalescence and breakup, a...

Dissolution and precipitation behavior of ternary solid dispersions of ezetimibe in biorelevant media.

Science.gov (United States)

Alhayali, Amani; Tavellin, Staffan; Velaga, Sitaram

2017-01-01

The effects of different formulations and processes on inducing and maintaining the supersaturation of ternary solid dispersions of ezetimibe (EZ) in two biorelevant media fasted-state simulated intestinal fluid (FaSSIF) and fasted-state simulated gastric fluid (FaSSGF) at different temperatures (25 °C and 37 °C) were investigated in this work. Ternary solid dispersions of EZ were prepared by adding polymer PVP-K30 and surfactant poloxamer 188 using melt-quenching and spray-drying methods. The resulting solid dispersions were characterized using scanning electron microscopy, differential scanning calorimetry (DSC), modulated DSC, powder X-ray diffraction and Fourier transformation infrared spectroscopy. The dissolution of all the ternary solid dispersions was tested in vitro under non-sink conditions. All the prepared solid dispersions were amorphous in nature. In FaSSIF at 25 °C, the melt-quenched (MQ) solid dispersions of EZ were more soluble than the spray-dried (SD) solid dispersions and supersaturation was maintained. However, at 37 °C, rapid and variable precipitation behavior was observed for all the MQ and SD formulations. In FaSSGF, the melting method resulted in better solubility than the spray-drying method at both temperatures. Ternary solid dispersions show potential for improving solubility and supersaturation. However, powder dissolution experiments of these solid dispersions of EZ at 25 °C may not predict the supersaturation behavior at physiologically relevant temperatures.

Evaluation of Antibacterial Enrofloxacin in Eggs by Matrix Solid Phase Dispersion-Flow Injection Chemiluminescence

Directory of Open Access Journals (Sweden)

Xiaocui Duan

2014-01-01

Full Text Available The study based on the chemiluminescence (CL reaction of potassium ferricyanide and luminol in sodium hydroxide medium, enrofloxacin (ENRO could dramatically enhance CL intensities and incorporated with matrix solid-phase dispersion (MSPD technique (Florisil used as dispersant, dichloromethane eluted the target compounds. A simple flow injection chemiluminescence (FL-CL method with MSPD technique for determination of ENRO in eggs was described. Under optimal conditions, the CL intensities were linearly related to ENRO concentration ranging from 4.0×10-8 g.L−1 to 5.0×10-5 g.L−1, with a correlation coefficient of 0.9989 and detection limit of 5.0×10-9 g.L−1. The relative standard deviation was 3.6% at an ENRO concentration of 2.0×10-6 g.L−1. Our testing technique can help ensure food safety, and thus, protect public health.

Overview of the phase diagram of ionic magnetic colloidal dispersions

International Nuclear Information System (INIS)

Cousin, F.; Dubois, E.; Cabuil, V.; Boue, F.; Perzynski, R.

2001-01-01

We study ionic magnetic colloidal dispersions, which are constituted of γ-Fe 2 O 3 nanoparticles dispersed in water, and stabilized with electrostatic interparticle repulsion. The phase diagram PV versus Φ (P: osmotic pressure, V: particle volume, Φ: particle volume fraction) is explored, especially in the range of high Π and high Φ. The osmotic pressure P of the colloidal dispersion is known either by a measurement either because it is imposed during the sample preparation by osmotic compression. The structure of the colloidal dispersion is determined from Small Angle Neutron Scattering. Two regimes can be distinguished. At high pressure, fluid and solid phases can exist. Their structure is governed by strong electrostatic repulsion, the range of which is here evaluated. At low pressure, gas, liquid and glassy solids can exist. Their structure results from a sticky hard sphere potential. (author)

Sensitive determination of three aconitum alkaloids and their metabolites in human plasma by matrix solid-phase dispersion with vortex-assisted dispersive liquid-liquid microextraction and HPLC with diode array detection.

Science.gov (United States)

Wang, Xiaozhong; Li, Xuwen; Li, Lanjie; Li, Min; Liu, Ying; Wu, Qian; Li, Peng; Jin, Yongri

2016-05-01

A simple and sensitive method for determination of three aconitum alkaloids and their metabolites in human plasma was developed using matrix solid-phase dispersion combined with vortex-assisted dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection. The plasma sample was directly purified by matrix solid-phase dispersion and the eluate obtained was concentrated and further clarified by vortex-assisted dispersive liquid-liquid microextraction. Some important parameters affecting the extraction efficiency, such as type and amount of dispersing sorbent, type and volume of elution solvent, type and volume of extraction solvent, salt concentration as well as sample solution pH, were investigated in detail. Under optimal conditions, the proposed method has good repeatability and reproducibility with intraday and interday relative standard deviations lower than 5.44 and 5.75%, respectively. The recoveries of the aconitum alkaloids ranged from 73.81 to 101.82%, and the detection limits were achieved within the range of 1.6-2.1 ng/mL. The proposed method offered the advantages of good applicability, sensitivity, simplicity, and feasibility, which makes it suitable for the determination of trace amounts of aconitum alkaloids in human plasma samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid Phase Characterization of Tank 241-AY-102 Annulus Space Particulate

Energy Technology Data Exchange (ETDEWEB)

Cooke, G. A.

2013-01-30

The Special Analytical Studies Group at the 222-S Laboratory (222-S) examined the particulate recovered from a series of samples from the annular space of tank 241-AY-102 (AY-102) using solid phase characterization (SPC) methods. These include scanning electron microscopy (SEM) using the ASPEX®1 scanning electron microscope, X-ray diffraction (XRD) using the Rigaku®2 MiniFlex X-ray diffractometer, and polarized light microscopy (PLM) using the Nikon®3 Eclipse Pol optical microscope. The SEM is equipped with an energy dispersive X-ray spectrometer (EDS) to provide chemical information.

Development and characterization of nifedipine-amino methacrylate copolymer solid dispersion powders with various adsorbents

Directory of Open Access Journals (Sweden)

Yotsanan Weerapol

2017-07-01

Full Text Available Solid dispersions of nifedipine (NDP, a poorly water-soluble drug, and amino methacrylate copolymer (AMCP with aid of adsorbent, that is, fumed silica, talcum, calcium carbonate, titanium dioxide, and mesoporous silica from rice husks (SRH, were prepared by solvent method. The physicochemical properties of solid dispersions, compared to their physical mixtures, were determined using powder X-ray diffractometry (PXRD and differential scanning calorimetry (DSC. The surface morphology of the prepared solid dispersions was examined by scanning electron microscopy (SEM. The dissolution of NDP from solid dispersions was compared to NDP powders. The effect of adsorbent type on NDP dissolution was also examined. The dissolution of NDP increased with the ratio of NDP:AMCP:adsorbent of 1:4:1 when compared to the other formulations. As indicated from PXRD patterns, DSC thermograms and SEM images, NDP was molecularly dispersed within polymer carrier or in an amorphous form, which confirmed the better dissolution of solid dispersions. Solid dispersions containing SRH provided the highest NDP dissolution, due to a porous nature of SRH, allowing dissolved drug to fill in the pores and consequently dissolve in the medium. The results suggested that solid dispersions containing adsorbents (SRH in particular demonstrated improved dissolution of poorly water-soluble drug when compared to NDP powder.

Electron drift in a large scale solid xenon

International Nuclear Information System (INIS)

Yoo, J.; Jaskierny, W.F.

2015-01-01

A study of charge drift in a large scale optically transparent solid xenon is reported. A pulsed high power xenon light source is used to liberate electrons from a photocathode. The drift speeds of the electrons are measured using a 8.7 cm long electrode in both the liquid and solid phase of xenon. In the liquid phase (163 K), the drift speed is 0.193 ± 0.003 cm/μs while the drift speed in the solid phase (157 K) is 0.397 ± 0.006 cm/μs at 900 V/cm over 8.0 cm of uniform electric fields. Therefore, it is demonstrated that a factor two faster electron drift speed in solid phase xenon compared to that in liquid in a large scale solid xenon

High-throughput multipesticides residue analysis in earthworms by the improvement of purification method: Development and application of magnetic Fe3 O4 -SiO2 nanoparticles based dispersive solid-phase extraction.

Science.gov (United States)

Sun, Yuhan; Qi, Peipei; Cang, Tao; Wang, Zhiwei; Wang, Xiangyun; Yang, Xuewei; Wang, Lidong; Xu, Xiahong; Wang, Qiang; Wang, Xinquan; Zhao, Changshan

2018-06-01

As a key representative organism, earthworms can directly illustrate the influence of pesticides on environmental organisms in soil ecosystems. The present work aimed to develop a high-throughput multipesticides residue analytical method for earthworms using solid-liquid extraction with acetonitrile as the solvent and magnetic material-based dispersive solid-phase extraction for purification. Magnetic Fe 3 O 4 nanoparticles were modified with a thin silica layer to form Fe 3 O 4 -SiO 2 nanoparticles, which were fully characterized by field-emission scanning electron microscopy, transmission electron microscopy, Fourier-transform infrared spectroscopy, X-ray diffractometry, and vibrating sample magnetometry. The Fe 3 O 4 -SiO 2 nanoparticles were used as the separation media in dispersive solid-phase extraction with primary secondary amine and ZrO 2 as the cleanup adsorbents to eliminate matrix interferences. The amounts of nanoparticles and adsorbents were optimized for the simultaneous determination of 44 pesticides and six metabolites in earthworms by liquid chromatography with tandem mass spectrometry. The method performance was systematically validated with satisfactory results. The limits of quantification were 20 μg/kg for all analytes studied, while the recoveries of the target analytes ranged from 65.1 to 127% with relative standard deviation values lower than 15.0%. The developed method was subsequently utilized to explore the bioaccumulation of bitertanol in earthworms exposed to contaminated soil, verifying its feasibility for real sample analysis. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Response surface method optimize of nano-silica solid dispersion technology assistant enzymatic hydrolysis preparation genistein].

Science.gov (United States)

Jin, Xin; Zhang, Zhen-Hai; Zhu, Jing; Sun, E; Yu, Dan-Hong; Chen, Xiao-Yun; Liu, Qi-Yuan; Ning, Qing; Jia, Xiao-Bin

2012-04-01

This article reports that nano-silica solid dispersion technology was used to raise genistein efficiency through increasing the enzymatic hydrolysis rate. Firstly, genistin-nano-silica solid dispersion was prepared by solvent method. And differential scanning calorimetry (DSC) and transmission electron microscopy (TEM) were used to verify the formation of solid dispersion, then enzymatic hydrolysis of solid dispersion was done by snailase to get genistein. With the conversion of genistein as criteria, single factor experiments were used to study the different factors affecting enzymatic hydrolysis of genistin and its solid dispersion. And then, response surface method was used to optimize of nano-silica solid dispersion technology assistant enzymatic hydrolysis. The optimum condition to get genistein through enzymatic hydrolysis of genistin-nano-silica solid dispersion was pH 7.1, temperature 52.2 degrees C, enzyme concentration 5.0 mg x mL(-1) and reaction time 7 h. Under this condition, the conversion of genistein was (93.47 +/- 2.40)%. Comparing with that without forming the genistin-nano-silica solid dispersion, the conversion increased 2.62 fold. At the same time, the product of hydrolysis was purified to get pure genistein. The method of enzymatic hydrolysis of genistin-nano-silica solid dispersion by snailase to obtain genistein is simple, efficiency and suitable for the modern scale production.

Determination of five pyrethroids in tea drinks by dispersive solid phase extraction with polyaniline-coated magnetic particles.

Science.gov (United States)

Wang, Yuanpeng; Sun, Ying; Gao, Yan; Xu, Bo; Wu, Qiong; Zhang, Hanqi; Song, Daqian

2014-02-01

The polyaniline-coated magnetic particles with bowl-shaped morphology (Fe3O4/C/PANI microbowls) were successfully prepared and characterized by scanning electron microscopy, transmission electron microscopy and vibrating sample magnetometry. The prepared microbowls were used as the magnetic adsorbent in dispersive solid phase extraction of five pyrethroids, including cyhalothrin, beta-cypermethrin, esfenvalerate, permethrin and bifenthrin in plain tea drinks. The effects of experiment factors, including amount of Fe3O4/C/PANI microbowls, pH value, ultrasound extraction time and desorption conditions, were investigated. The extraction recoveries obtained with 8 mg of magnetic microbowls were satisfactory, and the microbowls can be reused after easy washing. Thus, a simple, selective and effective method for the determination of the pyrethroids was established successfully. The results showed that the method had good linearity (r=0.9992-0.9998), and the limits of detections (LODs) were from 0.025 to 0.032 ng mL(-1). The intra-day and inter-day relative standard deviations (RSDs) were in the range of 2.4-6.1% and 3.5-8.8%, respectively. Recoveries obtained by analyzing the real tea drinks were in the range of 72.1-118.4%. © 2013 Published by Elsevier B.V.

Solid Phase Characterization of Tank 241-AY-102 Annulus Space Particulate

International Nuclear Information System (INIS)

Cooke, G. A.

2013-01-01

The Special Analytical Studies Group at the 222-S Laboratory (222-S) examined the particulate recovered from a series of samples from the annular space of tank 241-AY-102 (AY-102) using solid phase characterization (SPC) methods. These include scanning electron microscopy (SEM) using the ASPEX(R)1 scanning electron microscope, X-ray diffraction (XRD) using the Rigaku(R)2 MiniFlex X-ray diffractometer, and polarized light microscopy (PLM) using the Nikon(R)3 Eclipse Pol optical microscope. The SEM is equipped with an energy dispersive X-ray spectrometer (EDS) to provide chemical information

Trace determination of five triazole fungicide residues in traditional Chinese medicine samples by dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction and UHPLC-MS/MS.

Science.gov (United States)

Ma, Shuping; Yuan, Xucan; Zhao, Pengfei; Sun, Hong; Ye, Xiu; Liang, Ning; Zhao, Longshan

2017-08-01

A novel and reliable method for determination of five triazole fungicide residues (triadimenol, tebuconazole, diniconazole, flutriafol, and hexaconazol) in traditional Chinese medicine samples was developed using dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction before ultra-high performance liquid chromatography with tandem mass spectrometry. The clean up of the extract was conducted using dispersive solid-phase extraction by directly adding sorbents into the extraction solution, followed by shaking and centrifugation. After that, a mixture of 400 μL trichloromethane (extraction solvent) and 0.5 mL of the above supernatant was injected rapidly into water for the dispersive liquid-liquid microextraction procedure. The factors affecting the extraction efficiency were optimized. Under the optimum conditions, the calibration curves showed good linearity in the range of 2.0-400 (tebuconazole, diniconazole, and hexaconazole) and 4.0-800 ng/g (triadimenol and flutriafol) with the regression coefficients higher than 0.9958. The limit of detection and limit of quantification for the present method were 0.5-1.1 and 1.8-4.0 ng/g, respectively. The recoveries of the target analytes ranged from 80.2 to 103.2%. The proposed method has been successfully applied to the analysis of five triazole fungicides in traditional Chinese medicine samples, and satisfactory results were obtained. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A combination of solid-phase extraction and dispersive solid-phase extraction effectively reduces the matrix interference in liquid chromatography-ultraviolet detection during pyraclostrobin analysis in perilla leaves.

Science.gov (United States)

Farha, Waziha; Rahman, Md Musfiqur; Abd El-Aty, A M; Jung, Da-I; Kabir, Md Humayun; Choi, Jeong-Heui; Kim, Sung-Woo; Im, So Jeong; Lee, Young-Jun; Shin, Ho-Chul; Kwon, Chan-Hyeok; Son, Young-Wook; Lee, Kang-Bong; Shim, Jae-Han

2015-12-01

Perilla leaves contain many interfering substances; thus, it is difficult to protect the analytes during identification and integration. Furthermore, increasing the amount of sample to lower the detection limit worsens the situation. To overcome this problem, we established a new method using a combination of solid-phase extraction and dispersive solid-phase extraction to analyze pyraclostrobin in perilla leaves by liquid chromatography with ultraviolet absorbance detection. The target compound was quantitated by external calibration with a good determination coefficient (R(2) = 0.997). The method was validated (in triplicate) with three fortification levels, and 79.06- 89.10% of the target compound was recovered with a relative standard deviation <4. The limits of detection and quantification were 0.0033 and 0.01 mg/kg, respectively. The method was successfully applied to field samples collected from two different areas at Gwangju and Muan. The decline in the resiudue concentrations was best ascribed to a first-order kinetic model with half-lives of 5.7 and 4.6 days. The variation between the patterns was attributed to humidity. Copyright © 2015 John Wiley & Sons, Ltd.

Determination of haloacetic acids in water using layered double hydroxides as a sorbent in dispersive solid-phase extraction followed by liquid chromatography with tandem mass spectrometry.

Science.gov (United States)

Alsharaa, Abdulnaser; Sajid, Muhammad; Basheer, Chanbasha; Alhooshani, Khalid; Lee, Hian Kee

2016-09-01

In the present study, highly efficient and simple dispersive solid-phase extraction procedure for the determination of haloacetic acids in water samples has been established. Three different types of layered double hydroxides were synthesized and used as a sorbent in dispersive solid-phase extraction. Due to the interesting behavior of layered double hydroxides in an acidic medium (pH˂4), the analyte elution step was not needed; the layered double hydroxides are simply dissolved in acid immediately after extraction to release the analytes which are then directly introduced into a liquid chromatography with tandem mass spectrometry system for analysis. Several dispersive solid-phase extraction parameters were optimized to increase the extraction efficiency of haloacetic acids such as temperature, extraction time and pH. Under optimum conditions, good linearity was achieved over the concentration range of 0.05-100 μg/L with detection limits in the range of 0.006-0.05 μg/L. The relative standard deviations were 0.33-3.64% (n = 6). The proposed method was applied to different water samples collected from a drinking water plant to determine the concentrations of haloacetic acids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Innovative separation and preconcentration technique of coagulating homogenous dispersive micro solid phase extraction exploiting graphene oxide nanosheets

Energy Technology Data Exchange (ETDEWEB)

Ghazaghi, Mehri [Department of Chemistry, College of Science, Semnan University, P.O. Box: 35131-19111, Semnan (Iran, Islamic Republic of); Mousavi, Hassan Zavvar, E-mail: hzmousavi@semnan.ac.ir [Department of Chemistry, College of Science, Semnan University, P.O. Box: 35131-19111, Semnan (Iran, Islamic Republic of); Rashidi, Ali Morad [Nanotechnology Research Center, Research Institute of Petroleum Industry (RIPI), West Entrance Blvd., Olympic Village, P.O. Box: 14857-33111, Tehran (Iran, Islamic Republic of); Shirkhanloo, Hamid [Occupational and Environmental Health Research Center (OEHRC), Iranian Petroleum Industry Health Research Institute (IPIHRI), Tehran (Iran, Islamic Republic of); Rahighi, Reza [Nanotechnology Research Center, Research Institute of Petroleum Industry (RIPI), West Entrance Blvd., Olympic Village, P.O. Box: 14857-33111, Tehran (Iran, Islamic Republic of); Department of Research and Development, Sharif Ultrahigh Nanotechnologists (SUN) Company, P.O. Box: 13488-96394, Tehran (Iran, Islamic Republic of)

2016-01-01

A uniquely novel, fast, and facile technique is introduced for the first time in which a scant amount of graphene oxide (GO), without modification, has been utilized in dispersive mode of solid phase extraction (SPE) for an efficient yet simple separation. The proposed method of coagulating homogenous dispersive micro solid phase extraction (CHD-µSPE) is based on coagulation of homogeneous GO solution with the aid of polyetheneimine (PEI). CHD-µSPE use full adsorption capacity of GO because in this method was used GO solution obtained from synthesis process without drying step and stacking nanosheets. In optimized condition, 30 µL GO solution (7 mg mL{sup −1}), obtained in synthesis process, was injected into 1.5 mL the sample solution followed by immediate injection of 53 µL PEI solution (1 mg mL{sup −1}). After inserting PEI, GO sheets aggregate and can be readily separated by centrifugation. PEI not only cause aggregation of GO, but also form three-dimensional network of GO with easy handling in following separation steps. Lead, cadmium, and chromium were selected as model analytes and the effecting parameters including the amount of GO, concentration of PEI, sample pH, extraction time, and type of desorption solvent were investigated and optimized. The results indicate that the proposed CHD-µSPE method can be successfully applied GO in dispersive mode of SPE without effecting on good capability adsorption of GO. The novel method was applied in determination of lead, cadmium, and chromium in water, human saliva, and urine samples by electrothermal atomic absorption spectrometry. The detection limits are as low as 0.035, 0.005, and 0.012 µg L{sup −1} for Pb, Cd, and Cr respectively. The intra-day precisions (RSDs) were lower than 3.8%. CHD-µSPE method showed a good linear ranges of 0.24–15.6, 0.015–0.95 and 0.039–2.33 µg L{sup −1} for Pb, Cd and Cr respectively. Method performance was investigated by determination of mentioned

Influence of pressure on the solid state phase transformation of Cu–Al–Bi alloy

International Nuclear Information System (INIS)

Gong, Li; Jian-Hua, Liu; Wen-Kui, Wang; Ri-Ping, Liu

2010-01-01

The solid state phase transformation of Cu-Al-Bi alloy under high pressure was investigated by x-ray diffraction, energy dispersive spectroscopy and transmission electron microscopy. Experimental results show that the initial crystalline phase in the Cu-Al-Bi alloy annealed at 750 °C under the pressures in the range of 0–6 GPa is α-Cu solid solution (named as α-Cu phase below), and high pressure has a great influence on the crystallisation process of the Cu-Al-Bi alloy. The grain size of the α-Cu phase decreases with increasing pressure as the pressure is below about 3 GPa, and then increases (P > 3 GPa). The mechanism for the effects of high pressure on the crystallisation process of the alloy has been discussed. (condensed matter: structure, thermal and mechanical properties)

Micro-matrix solid-phase dispersion coupled with MEEKC for quantitative analysis of lignans in Schisandrae Chinensis Fructus using molecular sieve TS-1 as a sorbent.

Science.gov (United States)

Chu, Chu; Wei, Mengmeng; Wang, Shan; Zheng, Liqiong; He, Zheng; Cao, Jun; Yan, Jizhong

2017-09-15

A simple and effective method was developed for determining lignans in Schisandrae Chinensis Fructus by using a micro-matrix solid phase dispersion (MSPD) technique coupled with microemulsion electrokinetic chromatography (MEEKC). Molecular sieve, TS-1, was applied as a solid supporting material in micro MSPD extraction for the first time. Parameters that affect extraction efficiency, such as type of dispersant, mass ratio of the sample to the dispersant, grinding time, elution solvent and volume were optimized. The optimal extraction conditions involve dispersing 25mg of powdered Schisandrae samples with 50mg of TS-1 by a mortar and pestle. A grinding time of 150s was adopted. The blend was then transferred to a solid-phase extraction cartridge and the target analytes were eluted with 500μL of methanol. Moreover, several parameters affecting MEEKC separation were studied, including the type of oil, SDS concentration, type and concentration of cosurfactant, and concentration of organic modifier. A satisfactory linearity (R>0.9998) was obtained, and the calculated limits of quantitation were less than 2.77μg/mL. Finally, the micro MSPD-MEEKC method was successfully applied to the analysis of lignans in complex Schisandrae fructus samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Measurement of phase interaction in dispersed gas-particle two-phase flow by phase-doppler anemometry

OpenAIRE

Mergheni Ali Mohamed; Ben Ticha Hmaied; Sautet Jen-Charles; Godard Gille; Ben Nasrallah Sassi

2008-01-01

For simultaneous measurement of size and velocity distributions of continuous and dispersed phases in a two-phase flow a technique phase-Doppler anemometry was used. Spherical glass particles with a particle diameter range from 102 up to 212 µm were used. In this two-phase flow an experimental results are presented which indicate a significant influence of the solid particles on the flow characteristics. The height of influence of these effects depends on the local position in the jet. Near t...

Drop Printing of Pharmaceuticals: Effect of Molecular Weight on PEG Coated-Naproxen/PEG3350 Solid Dispersions.

Science.gov (United States)

Hsu, Hsin-Yun; Toth, Scott; Simpson, Garth J; Harris, Michael T

2015-12-01

Solid dispersions have been used to enhance the bioavailability of poorly water-soluble active pharmaceutical ingredients (APIs). However, the solid state phase, compositional uniformity, and scale-up problems are issues that need to be addressed. To allow for highly controllable products, the Drop Printing (DP) technique can provide precise dosages and predictable compositional uniformity of APIs in two/three dimensional structures. In this study, DP was used to prepare naproxen (NAP)/polyethylene glycol 3350 (PEG3350) solid dispersions with PEG coatings of different molecular weights (MW). A comparison of moisture-accelerated crystallization inhibition by different PEG coatings was assessed. Scanning electron microscopy (SEM), second harmonic generation (SHG) microscopy, and differential scanning calorimetry (DSC) analysis were performed to characterize the morphology and quantify the apparent crystallinity of NAP within the solid dispersions. Thermogravimetric analysis (TGA) was employed to measure the water content within each sample. The results suggest that the moisture-accelerated crystallization inhibition capability of the PEG coatings increased with increasing MW of the PEG coating. Besides, to demonstrate the flexibility of DP technology on manufacturing formulation, multilayer tablets with different PEG serving as barrier layers were also constructed, and their dissolution behavior was examined. By applying DP and appropriate materials, it is possible to design various carrier devices used to control the release dynamics of the API.

Synthesis and application of mesoporous molecular sieve for miniaturized matrix solid-phase dispersion extraction of bioactive flavonoids from toothpaste, plant, and saliva.

Science.gov (United States)

Cao, Wan; Cao, Jun; Ye, Li-Hong; Xu, Jing-Jing; Hu, Shuai-Shuai; Peng, Li-Qing

2015-12-01

This article describes the use of the mesoporous molecular sieve KIT-6 as a sorbent in miniaturized matrix solid-phase dispersion (MSPD) in combination with ultra-performance LC for the determination of bioactive flavonoids in toothpaste, Scutellariae Radix, and saliva. In this study, for the first time, KIT-6 was used as a sorbent material for this mode of extraction. Compared with common silica-based sorbents (C18 and activated silica gel), the proposed KIT-6 dispersant with a three-dimensional cubic Ia3d structure and highly ordered arrays of mesoporous channels exhibits excellent adsorption capability of the tested compounds. In addition, several experimental variables, such as the mass ratio of sample to dispersant, grinding time, and elution solvent, were optimized to maximize the extraction efficiency. The proposed analytical method is simple, fast, and entails low consumption of samples, dispersants and elution solvents, thereby meeting "green chemistry" requirements. Under the optimized conditions, the recoveries of three bioactive flavonoids obtained by analyzing the spiked samples were from 89.22 to 101.17%. Also, the LODs and LOQs for determining the analytes were in the range of 0.02-0.04 μg/mL and 0.07-0.13 μg/mL, respectively. Finally, the miniaturized matrix solid-phase dispersion method was successfully applied to the analysis of target solutes in real samples, and satisfactory results were obtained. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Dispersive solid-phase extraction followed by vortex-assisted dispersive liquid-liquid microextraction based on the solidification of a floating organic droplet for the determination of benzoylurea insecticides in soil and sewage sludge.

Science.gov (United States)

Peng, Guilong; He, Qiang; Mmereki, Daniel; Lu, Ying; Zhong, Zhihui; Liu, Hanyang; Pan, Weiliang; Zhou, Guangming; Chen, Junhua

2016-04-01

A novel dispersive solid-phase extraction combined with vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet was developed for the determination of eight benzoylurea insecticides in soil and sewage sludge samples before high-performance liquid chromatography with ultraviolet detection. The analytes were first extracted from the soil and sludge samples into acetone under optimized pretreatment conditions. Clean-up of the extract was conducted by dispersive solid-phase extraction using activated carbon as the sorbent. The vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet procedure was performed by using 1-undecanol with lower density than water as the extraction solvent, and the acetone contained in the solution also acted as dispersive solvent. Under the optimum conditions, the linearity of the method was in the range 2-500 ng/g with correlation coefficients (r) of 0.9993-0.9999. The limits of detection were in the range of 0.08-0.56 ng/g. The relative standard deviations varied from 2.16 to 6.26% (n = 5). The enrichment factors ranged from 104 to 118. The extraction recoveries ranged from 81.05 to 97.82% for all of the analytes. The good performance has demonstrated that the proposed methodology has a strong potential for application in the multiresidue analysis of complex matrices. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Temperature sensitive molecularly imprinted microspheres for solid-phase dispersion extraction of malachite green, crystal violet and their leuko metabolites

International Nuclear Information System (INIS)

Tan, Lei; Chen, Kuncai; He, Rong; Peng, Rongfei; Huang, Cong

2016-01-01

This article demonstrates the feasibility of an alternative strategy for producing temperature sensitive molecularly imprinted microspheres (MIMs) for solid-phase dispersion extraction of malachite green, crystal violet and their leuko metabolites. Thermo-sensitive MIMs can change their structure following temperature stimulation. This allows capture and release of target molecules to be controlled by temperature. The fabrication technique provides surface molecular imprinting in acetonitrile using vinyl modified silica microspheres as solid supports, methacrylic acid and N-isopropyl acrylamide as the functional monomers, ethyleneglycol dimethacrylate as the cross-linker, and malachite green as the template. After elution of the template, the MIMs can be used for fairly group-selective solid phase dispersion extraction of malachite green, crystal violet, leucomalachite green, and leucocrystal violet from homogenized fish samples at a certain temperature. Following centrifugal separation of the microspheres, the analytes were eluted with a 95:5 mixture of acetonitrile and formic acid, and then quantified by ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) with isotope internal calibration. The detection limits for malachite green, crystal violet and their metabolites typically are 30 ng·kg −1 . Positive samples were identified by UHPLC-MS/MS in the positive ionization mode with multiple reaction monitoring. The method was applied to the determination of the dyes and the respective leuko dyes in fish samples, and accuracy and precision were validated by comparative analysis of the samples by using aluminum neutral columns. (author)

Enhanced solubility and bioavailability of sibutramine base by solid dispersion system with aqueous medium.

Science.gov (United States)

Li, Dong Xun; Jang, Ki-Young; Kang, Wonku; Bae, Kyoungjin; Lee, Mann Hyung; Oh, Yu-Kyoung; Jee, Jun-Pil; Park, Young-Joon; Oh, Dong Hoon; Seo, Youn Gee; Kim, Young Ran; Kim, Jong Oh; Woo, Jong Soo; Yong, Chul Soon; Choi, Han-Gon

2010-01-01

To develop a novel sibutramine base-loaded solid dispersion with improved solubility bioavailability, various solid dispersions were prepared with water, hydroxypropylmethyl cellulose (HPMC), poloxamer and citric acid using spray-drying technique. The effect of HPMC, poloxamer and citric acid on the aqueous solubility of sibutramine was investigated. The physicochemical properties of solid dispersion were investigated using scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and X-ray powder diffraction. The dissolution and pharmacokinetics in rats of solid dispersion were evaluated compared to the sibutramine hydrochloride monohydrate-loaded commercial product (Reductil). The sibutramine base-loaded solid dispersion gave two type forms. Like conventional solid dispersion system, one type appeared as a spherical shape with smooth surface, as the carriers and drug with relatively low melting point were soluble in water and formed it. The other appeared as an irregular form with relatively rough surface. Unlike conventional solid dispersion system, this type changed no crystalline form of drug. Our results suggested that this type was formed by attaching hydrophilic carriers to the surface of drug without crystal change, resulting from changing the hydrophobic drug to hydrophilic form. The sibutramine-loaded solid dispersion at the weight ratio of sibutramine base/HPMC/poloxamer/citric acid of 5/3/3/0.2 gave the maximum drug solubility of about 3 mg/ml. Furthermore, it showed the similar plasma concentration, area under the curve (AUC) and C(max) of parent drug, metabolite I and II to the commercial product, indicating that it might give the similar drug efficacy compared to the sibutramine hydrochloride monohydrate-loaded commercial product in rats. Thus, this solid dispersion system would be useful to deliver poorly water-soluble sibutramine base with enhanced bioavailability.

Optimization of matrix solid-phase dispersion for the rapid determination of salicylate and benzophenone-type UV absorbing substances in marketed fish.

Science.gov (United States)

Tsai, Dung-Ying; Chen, Chien-Liang; Ding, Wang-Hsien

2014-07-01

A simple and effective method for the rapid determination of five salicylate and benzophenone-type UV absorbing substances in marketed fish is described. The method involves the use of matrix solid-phase dispersion (MSPD) prior to their determination by on-line silylation gas chromatography tandem mass spectrometry (GC-MS/MS). The parameters that affect the extraction efficiency were optimized using a Box-Behnken design method. The optimal extraction conditions involved dispersing 0.5g of freeze-dried powdered fish with 1.0g of Florisil using a mortar and pestle. This blend was then transferred to a solid-phase extraction (SPE) cartridge containing 1.0g of octadecyl bonded silica (C18), as the clean-up co-sorbent. The target analytes were then eluted with 7mL of acetonitrile. The extract was derivatized on-line in the GC injection-port by reaction with a trimethylsilylating (TMS) reagent. The TMS-derivatives were then identified and quantitated by GC-MS/MS. The limits of quantitation (LOQs) were less than 0.1ng/g. Copyright © 2014 Elsevier Ltd. All rights reserved.

Random phase approximation applied to solids, molecules, and graphene-metal interfaces

DEFF Research Database (Denmark)

Olsen, Thomas; Thygesen, Kristian S.

2013-01-01

The random phase approximation (RPA) is attracting renewed interest as a universal and accurate method for first-principles total energy calculations. The RPA naturally accounts for long-range dispersive forces without compromising accuracy for short-range interactions making the RPA superior...... to semilocal and hybrid functionals in systems dominated by weak van der Waals or mixed covalent-dispersive interactions. In this work, we present plane-wave-based RPA calculations for a broad collection of systems with bond types ranging from strong covalent to van der Waals. Our main result is the RPA...... the RPA captures both the weak covalent and dispersive forces, which are equally important for these systems. We benchmark our implementation in the GPAW electronic structure code by calculating cohesive energies of graphite and a range of covalently bonded solids and molecules as well as the dissociation...

Electronic phase transitions

CERN Document Server

Kopaev, YuV

1992-01-01

Electronic Phase Transitions deals with topics, which are presently at the forefront of scientific research in modern solid-state theory. Anderson localization, which has fundamental implications in many areas of solid-state physics as well as spin glasses, with its influence on quite different research activities such as neural networks, are two examples that are reviewed in this book. The ab initio statistical mechanics of structural phase transitions is another prime example, where the interplay and connection of two unrelated disciplines of solid-state theory - first principle ele

Solid Phase Characterization Of Heel Samples From Tank 241-C-110

International Nuclear Information System (INIS)

Page, J.S.; Cooke, G.A.; Pestovich, J.A.; Huber, H.J.

2011-01-01

During sluicing operations of tank 241-C-110, a significant amount of solids were unable to be retrieved. These solids (often referred to as the tank 'heel') were sampled in 2010 and chemically and mineralogically analyzed in the 222-S Laboratory. Additionally, dissolution tests were performed to identify the amount of undissolvable material after using multiple water contacts. This report covers the solid phase characterization of six samples from these tests using scanning electron microscopy, polarized light microscopy, and X-ray diffraction. The chemical analyses, particle size distribution analysis, and dissolution test results are reported separately. Two of the samples were from composites created from as-received material - Composite A and Composite B. The main phase in these samples was sodium-fluoride-phosphate hydrate (natrophosphate) - in the X-ray diffraction spectra, this phase was the only phase identifiable. Polarized light microscopy showed the presence of minor amounts of gibbsite and other phases. These phases were identified by scanning electron microscopy - energy dispersive X-ray spectroscopy as sodium aluminosilicates, sodium diuranate, and sodium strontium phosphate hydrate (nastrophite) crystals. The natrophosphate crystals in the scanning electron microscopy analysis showed a variety of erosive and dissolution features from perfectly shaped octahedral to well-rounded appearance. Two samples were from water-washed Composites A and B, with no change in mineralogy compared to the as-received samples. This is not surprising, since the water wash had only a short period of water contact with the material as opposed to the water dissolution tests. The last two samples were residual solids from the water dissolution tests. These tests included multiple additions of water at 15 C and 45 C. The samples were sieved to separate a coarser fraction of > 710 μm and a finer fraction of < 710 μm. These two fractions were analyzed separately. The coarser

Strongly coupled dispersed two-phase flows; Ecoulements diphasiques disperses fortement couples

Energy Technology Data Exchange (ETDEWEB)

Zun, I.; Lance, M.; Ekiel-Jezewska, M.L.; Petrosyan, A.; Lecoq, N.; Anthore, R.; Bostel, F.; Feuillebois, F.; Nott, P.; Zenit, R.; Hunt, M.L.; Brennen, C.E.; Campbell, C.S.; Tong, P.; Lei, X.; Ackerson, B.J.; Asmolov, E.S.; Abade, G.; da Cunha, F.R.; Lhuillier, D.; Cartellier, A.; Ruzicka, M.C.; Drahos, J.; Thomas, N.H.; Talini, L.; Leblond, J.; Leshansky, A.M.; Lavrenteva, O.M.; Nir, A.; Teshukov, V.; Risso, F.; Ellinsen, K.; Crispel, S.; Dahlkild, A.; Vynnycky, M.; Davila, J.; Matas, J.P.; Guazelli, L.; Morris, J.; Ooms, G.; Poelma, C.; van Wijngaarden, L.; de Vries, A.; Elghobashi, S.; Huilier, D.; Peirano, E.; Minier, J.P.; Gavrilyuk, S.; Saurel, R.; Kashinsky, O.; Randin, V.; Colin, C.; Larue de Tournemine, A.; Roig, V.; Suzanne, C.; Bounhoure, C.; Brunet, Y.; Tanaka, A.T.; Noma, K.; Tsuji, Y.; Pascal-Ribot, S.; Le Gall, F.; Aliseda, A.; Hainaux, F.; Lasheras, J.; Didwania, A.; Costa, A.; Vallerin, W.; Mudde, R.F.; Van Den Akker, H.E.A.; Jaumouillie, P.; Larrarte, F.; Burgisser, A.; Bergantz, G.; Necker, F.; Hartel, C.; Kleiser, L.; Meiburg, E.; Michallet, H.; Mory, M.; Hutter, M.; Markov, A.A.; Dumoulin, F.X.; Suard, S.; Borghi, R.; Hong, M.; Hopfinger, E.; Laforgia, A.; Lawrence, C.J.; Hewitt, G.F.; Osiptsov, A.N.; Tsirkunov, Yu. M.; Volkov, A.N.

2003-07-01

flow, current distribution and mass transfer along a vertical gas evolving electrode; a two-way coupled model for dilute multiphase flows. Topic 3: turbulence modulation by particles, droplets or bubbles in dense systems: influence of particles on the transition to turbulence in pipe flow; comparison between a point particle model and a finite-diameter-model for the particle turbulence interaction in a suspension; the effect on turbulence by bubbles rising through it under buoyancy; the physical mechanisms of modifying the structure of turbulent homogeneous shear flows by dispersed particles; influence of hydrodynamic interactions between particles on the turbulent flow in a suspension; review of relationships between Lagrangian and Eulerian scales; a two-point PDF for modelling turbulent dispersed two-phase flows and derivation of a two field model; mathematical and numerical modeling of two-phase compressible flows with micro-inertia. Topic 4: collective effects in dispersed two-phase flows clustering and phase distribution: hydrodynamic structure of downward bubbly flow; influence of gravity on the dynamics of a turbulent bubbly pipe flow; experimental study of two-phase flows; particle clusters formed in dispersed gas-solid flows: simulations and experiments; experimental study of the turbulence in bubbly flows at high void fraction; first step in the study of the correlation between air/water flow fluctuations and random buffering forces; clustering and settling velocity of micro-droplets in a grid turbulence. Topic 5: large scale instabilities and gravity driven dispersed flows: new 'non-isothermal' linear instability modes in fluidized beds and bubbly flows; large scale instability in a confined buoyant shear layer; convective instability in uniform dispersed layers; structures in gravity driven bubbly flows; effects of concentration profiles on velocity profiles in sewer; pyroclastic density currents viewed as mammoth scale two-phase flows; mixing and

Streamlined sample cleanup using combined dispersive solid-phase extraction and in-vial filtration for analysis of pesticides and environmental pollutants in shrimp

Science.gov (United States)

A new method of sample preparation was developed and is reported for the first time. The approach combines in-vial filtration with dispersive solid-phase extraction (d-SPE) in a fast and convenient cleanup of QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts. The method was appli...

Development of matrix solid-phase dispersion method for the extraction of short-chain chlorinated paraffins in human placenta.

Science.gov (United States)

Wang, Ying; Gao, Wei; Wu, Jing; Liu, Huijin; Wang, Yingjun; Wang, Yawei; Jiang, Guibin

2017-12-01

Chlorinated paraffins (SCCPs) are widely used worldwide, and they can be released into the environment during their production, transport, usage and disposal, which pose potential risks for human health. In this work, an efficient, reliable and rapid pretreatment method based on matrix solid-phase dispersion (MSPD) was developed for the analysis of short-chain CPs (SCCPs) in human placenta by gas chromatograph-electron capture negative ion low-resolution mass spectrometry (GC-ECNI-LRMS) and gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF-HRMS). The MSPD-relevant parameters including dispersing sorbent, sample-to-sorbent mass ratio, and elution solvent were optimized using the orthogonal test. Silica gel was found to be the optimal dispersing sorbent among the selected matrices. Under the optimal conditions, 44% acidic silica gel can be used as the co-sorbent to remove lipid and eluted by the mixture of hexane and dichloromethane (7:3, V/V). The spiked recoveries of the optimized method were 77.4% and 91.4% for analyzing SCCPs in human placenta by GC-ECNI-LRMS and GC-QTOF-HRMS, and the corresponding relative standard deviations were 10.2% and 5.6%, respectively. The method detection limit for the total SCCPs was 36.8ng/g (dry weight, dw) and 19.2ng/g (dw) as measured by GC-ECNI-LRMS and GC-QTOF-HRMS, respectively. The concentrations of SCCPs in four human placentas were in the range of

Primary secondary amine as a sorbent material in dispersive solid-phase extraction clean-up for the determination of indicator polychlorinated biphenyls in environmental water samples by gas chromatography with electron capture detection.

Science.gov (United States)

Guo, Yuanming; Hu, Hongmei; Li, Tiejun; Xue, Lijian; Zhang, Xiaoning; Zhong, Zhi; Zhang, Yurong; Jin, Yanjian

2017-08-01

A simple, rapid, and novel method has been developed and validated for determination of seven indicator polychlorinated biphenyls in water samples by gas chromatography with electron capture detection. 1 L of water samples containing 30 g of anhydrous sodium sulfate was first liquid-liquid extracted with an automated Jipad-6XB vertical oscillator using n-hexane/dichloromethane (1:1, v/v). The concentrated extract was cleaned up by dispersive solid-phase extraction with 100 mg of primary secondary amine as sorbent material. The linearity of this method ranged from 1.25 to 100 μg/L, with regression coefficients ranging between 0.9994 and 0.9999. The limits of detection were in the ng/L level, ranging between 0.2 and 0.3 ng/L. The recoveries of seven spiked polychlorinated biphenyls with external calibration method at different concentration levels in tap water, lake water, and sea water were in the ranges of 85-112, 76-116, and 72-108%, respectively, and with relative standard deviations of 3.3-4.5, 3.4-5.6, and 3.1-4.8% (n = 5), respectively. The performance of the proposed method was compared with traditional liquid-liquid extraction and solid-phase extraction clean-up methods, and comparable efficiencies were obtained. It is concluded that this method can be successfully applied for the determination of polychlorinated biphenyls in different water samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid-state phase equilibria in the Fe-Pt-Pr ternary system at 1173 K

International Nuclear Information System (INIS)

Ren Jing; Gu Zhengfei; Cheng Gang; Zhou Huaiying

2005-01-01

The solid-state phase equilibria in the Fe-Pt-Pr ternary system at 1173 K (Pr ≤ 70%) were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersion spectroscopy (EDS) techniques. The 1173 K isothermal section consists of 13 single-phase regions, 22 two-phase regions and 10 three-phase regions. At 1173 K, we have observed that the maximum solid solubility of Pt in α-Fe is below 1.5 at.% and the solid solution region of Pt in γ-Fe is from 2 to 35 at.%; the maximum solid solubility of Fe in Pt is 18 at.%. The maximum solubility of Fe in PrPt 5 , PrPt 3 , PrPt 2 , Pr 3 Pt 4 , PrPt, Pr 3 Pt 2 and Pr 7 Pt 3 is below 1 at.%. The maximum solubility of Pr in α-(Fe, Pt), γ-(Fe, Pt), FePt, FePt 3 and (Pt, Fe) (the solid solution of Fe in Pt) is 6, 2, 4, 4.5 and 1.5 at.%, respectively. In this work, it is found that the phase Pr 3 Pt 4 does not exist in the ternary system. The binary compounds Fe 7 Pr and Fe 2 Pr and any new ternary compounds were not observed

Modification of polydopamine-coated Fe3O4 nanoparticles with multi-walled carbon nanotubes for magnetic-μ-dispersive solid-phase extraction of antiepileptic drugs in biological matrices.

Science.gov (United States)

Zhang, Ruiqi; Wang, Siming; Yang, Ye; Deng, Yulan; Li, Di; Su, Ping; Yang, Yi

2018-06-01

In this study, multi-walled carbon nanotubes were coated on the surface of magnetic nanoparticles modified by polydopamine. The synthesized composite was characterized and applied to magnetic-μ-dispersive solid-phase extraction of oxcarbazepine (OXC), phenytoin (PHT), and carbamazepine (CBZ) from human plasma, urine, and cerebrospinal fluid samples prior to analysis by a high-performance liquid chromatography-photodiode array detector. The extraction parameters were investigated and the optimum condition was obtained when the variables were set to the following: sorbent type, Fe 3 O 4 @polyDA-MWCNTs (length Graphical abstract Magnetic multi-walled carbon nanotube core-shell composites were applied as magnetic-μ-dispersive solid-phase extraction adsorbents for determination of antiepileptic drugs in biological matrices.

Surface Solid Dispersion and Solid Dispersion of Meloxicam: Comparison and Product Development.

Science.gov (United States)

Chaturvedi, Mayank; Kumar, Manish; Pathak, Kamla; Bhatt, Shailendra; Saini, Vipin

2017-12-01

Purpose: A comparative study was carried out between surface solid dispersion (SSD) and solid dispersion (SD) of meloxicam (MLX) to assess the solubility and dissolution enhancement approach and thereafter develop as patient friendly orodispersible tablet. Methods: Crospovidone (CPV), a hydrophilic carrier was selected for SSD preparation on the basis of 89% in- vitro MLX adsorption, 19% hydration capacity and high swelling index. SD on the other hand was made with PEG4000. Both were prepared by co-grinding and solvent evaporation method using drug: carrier ratios of 1:1, 1:4, and 1:8. Formulation SSDS3 (MLX: CPV in 1:8 ratio) made by solvent evaporation method showed t 50% of 28 min and 80.9% DE 50min which was higher in comparison to the corresponding solid dispersion, SDS3 (t 50% of 35min and 76.4% DE 50min ). Both SSDS3 and SDS3 were developed as orodispersible tablets and evaluated. Results: Tablet formulation F3 made with SSD3 with a disintegration time of 11 secs, by wetting time= 6 sec, high water absorption of 78%by wt and cumulative drug release of 97% proved to be superior than the tablet made with SD3. Conclusion: Conclusively, the SSD of meloxicam has the potential to be developed as fast acing formulation that can ensure almost complete release of drug.

Surface Solid Dispersion and Solid Dispersion of Meloxicam: Comparison and Product Development

Directory of Open Access Journals (Sweden)

Mayank Chaturvedi

2017-12-01

Full Text Available Purpose: A comparative study was carried out between surface solid dispersion (SSD and solid dispersion (SD of meloxicam (MLX to assess the solubility and dissolution enhancement approach and thereafter develop as patient friendly orodispersible tablet. Methods: Crospovidone (CPV, a hydrophilic carrier was selected for SSD preparation on the basis of 89% in- vitro MLX adsorption, 19% hydration capacity and high swelling index. SD on the other hand was made with PEG4000. Both were prepared by co-grinding and solvent evaporation method using drug: carrier ratios of 1:1, 1:4, and 1:8. Formulation SSDS3 (MLX: CPV in 1:8 ratio made by solvent evaporation method showed t50% of 28 min and 80.9% DE50min which was higher in comparison to the corresponding solid dispersion, SDS3 (t50% of 35min and 76.4% DE50min. Both SSDS3 and SDS3 were developed as orodispersible tablets and evaluated. Results: Tablet formulation F3 made with SSD3 with a disintegration time of 11 secs, by wetting time= 6 sec, high water absorption of 78%by wt and cumulative drug release of 97% proved to be superior than the tablet made with SD3. Conclusion: Conclusively, the SSD of meloxicam has the potential to be developed as fast acing formulation that can ensure almost complete release of drug.

A computer model for dispersed fluid-solid turbulent flows

International Nuclear Information System (INIS)

Liu, C.H.; Tulig, T.J.

1985-01-01

A computer model is being developed to simulate two-phase turbulent flow phenomena in fluids containing finely dispersed solids. The model is based on a dual-continuum picture of the individual phases and an extension of a two-equation turbulence closure theory. The resulting set of nonlinear partial differential equations are solved using a finite difference procedure with special treatment to promote convergence. The model has been checked against a number of idealized flow problems with known solutions. The authors are currently comparing model predictions with measurements to determine a proper set of turbulence parameters needed for simulating two-phase turbulent flows

Novel solid – solid phase change material based on polyethylene glycol and cellulose used for temperature stabilisation

Directory of Open Access Journals (Sweden)

Wojda Marta

2014-01-01

Full Text Available Thermal management is one of crucial issues in the development of modern electronic devices. In the recent years interest in phase change materials (PCMs as alternative cooling possibility has increased significantly. Preliminary results concerning the research into possibility of the use of solid-solid phase change materials (S-S PCMs for stabilisation temperature of electronic devices has been presented in the paper. Novel solid-solid phase change material based on polyethylene glycol and cellulose has been synthesized. Attempt to improve its thermal conductivity has been taken. Material has been synthesized for the purpose of stabilisation of temperature of electronic devices.

Analysis of malachite green in aquatic products by carbon nanotube-based molecularly imprinted - matrix solid phase dispersion.

Science.gov (United States)

Wang, Yu; Chen, Ligang

2015-10-01

A simple method based on matrix solid phase dispersion (MSPD) using molecularly imprinted polymers (MIPs) as sorbents for selective extraction of malachite green (MG) from aquatic products was developed. The MIPs were prepared by using carbon nanotube as support, MG as template, methacrylic acid as functional monomer, ethyleneglycol dimethacrylate as crosslinker and methylene chloride as solvent. The MIPs were characterized by Fourier transform infrared spectrometry and transmission electron microscopy. The isothermal adsorption, kinetics absorption and selective adsorption experiments were carried out. We optimized the extraction conditions as follows: the ratio of MIPs to sample was 2:3, the dispersion time was 15min, washing solvent was 4mL 50% aqueous methanol and elution solvent was 3mL methanol-acetic acid (98: 2, v/v). Once the MSPD process was completed, the MG extracted from aquatic products was determined by high performance liquid chromatography. The detection limit of MG was 0.7μgkg(-1). The relative standard deviations of intra-day and inter-day were obtained in the range of 0.9%-4.7% and 3.4%-9.8%, respectively. In order to evaluate the applicability and reliability of the proposed method, it was applied to determine MG in different aquatic products samples including fish, shrimp, squid and crabs. The satisfied recoveries were in the range of 89.2%-104.6%. The results showed that this method is faster, simpler and makes extraction and purification in the same system. Copyright © 2015 Elsevier B.V. All rights reserved.

Contribution to the study of second phases particles dispersion in polycrystalline uranium dioxide

International Nuclear Information System (INIS)

Peres, V.

1994-06-01

To reduce fission gas release of irradiated polycrystalline uranium dioxide, the dispersion of intragranular nanometric particles of second phase necessary to pin gas bubbles may complete the advantage of a large-grained fuel microstructure. Moreover, intergranular glass films may improve high temperatures mechanical properties of UO 2 . In this study, mixtures of additives composed of ''corindon'' structure oxides that enhance the fuel grain growth and composed of different oxides with variable solid solubilities in the UO 2 matrix were achieved. Additives with a negligible solubility inhibit grain boundaries motion except those, such as silica, that involve a liquid phase at the sintering temperature. Rare earth oxides that form stable solid solutions with UO 2 cannot lead to precipitation, but have no effect on the fuel grain growth doped with ''corindon'' type oxides. A chromium oxide excess allows the creation of a fuel microstructure described by large grains and intragranular spherical Cr 2 O 3 inclusions observed by scanning electron microscopy. Values for the bulk lattice diffusion coefficient of Cr 3+ cations in UO 2 can be deduced from the experimental growth of those dispersed particles by an Ostwald ripening mechanism. The formation of small precipitated metal particles inside the uranium dioxide matrix induced by the internal reduction of a solid solution has not been performed. However, direct reduction of insoluble chromium oxide particles is easy and produces metallic intragranular precipitates. (author). 119 refs., 112 figs., 33 tabs., 5 annexes

Core-shell indium (III) sulfide@metal-organic framework nanocomposite as an adsorbent for the dispersive solid-phase extraction of nitro-polycyclic aromatic hydrocarbons.

Science.gov (United States)

Jia, Yuqian; Zhao, Yanfang; Zhao, Mei; Wang, Zhenhua; Chen, Xiangfeng; Wang, Minglin

2018-05-25

A core-shell discoid shaped indium (III) sulfide@metal-organic framework (MIL-125(Ti)) nanocomposite was synthesized by a solvothermal method and explored as an adsorbent material for dispersive solid-phase extraction (d-SPE). The as-synthesized sorbent was characterized by scanning electron microscopy, energy-dispersive spectroscopy, transmission electron microscopy, powder X-ray diffraction, N 2 adsorption-desorption analysis, and Fourier transform infrared spectroscopy. The extraction performance was evaluated by the d-SPE of 16 nitro-polycyclic aromatic hydrocarbons (NPAHs) from water samples. The analysis was carried out by gas chromatography (GC) coupled with triple quadruple mass spectrometer in negative chemical ionization (NCI) mode. The selected ion monitoring (SIM) was used in the quantification of the target NPAHs. Extraction factors affecting the d-SPE, including the ionic strength, extraction temperature, and extraction time were optimized by the response surface methodology. The developed d-SPE method showed good linear correlations from 10 to 1000 ng L -1 (r > 0.99), low detection limits (2.9-83.0 ng L -1 ), satisfactory repeatability (relative standard deviation of <10%, n = 6), and acceptable recoveries (71.3%-112.2%) for water samples. The developed method was used for the food and environmental sample analysis. The results demonstrated that the method could be used for sample preparation of trace NPAHs in real samples. Copyright © 2018. Published by Elsevier B.V.

Solvent-assisted dispersive solid-phase extraction: A sample preparation method for trace detection of diazinon in urine and environmental water samples.

Science.gov (United States)

Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

2016-09-02

In this research, a sample preparation method termed solvent-assisted dispersive solid-phase extraction (SA-DSPE) was applied. The used sample preparation method was based on the dispersion of the sorbent into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was received by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the diazinon, the cloudy solution was centrifuged and diazinon in the sediment phase dissolved in ethanol and determined by gas chromatography-flame ionization detector. Under the optimized conditions (pH of solution=7.0, Sorbent: benzophenone, 2%, Disperser solvent: ethanol, 500μL, Centrifuge: centrifuged at 4000rpm for 3min), the method detection limit for diazinon was 0.2, 0.3, 0.3 and 0.3μgL(-1) for distilled water, lake water, waste water and urine sample, respectively. Furthermore, the pre-concentration factor was 363.8, 356.1, 360.7 and 353.38 in distilled water, waste water, lake water and urine sample, respectively. SA-DSPE was successfully used for trace monitoring of diazinon in urine, lake and waste water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Influence of solvent composition on the miscibility and physical stability of naproxen/PVP K 25 solid dispersions prepared by cosolvent spray-drying.

Science.gov (United States)

Paudel, Amrit; Van den Mooter, Guy

2012-01-01

To investigate the influence of solvent properties on the phase behavior and physical stability of spray-dried solid dispersions containing naproxen and PVP K 25 prepared from binary cosolvent systems containing methanol, acetone and dichloromethane. The viscosity, polymer globular size and evaporation rate of the spray-drying feed solutions were characterized. The solid dispersions were prepared by spray-drying drug-polymer solutions in binary solvent blends containing different proportions of each solvent. The phase behavior was investigated with mDSC, pXRD, FT-IR and TGA. Further, physical stability of solid dispersions was assessed by analyzing after storage at 75% RH. The solid dispersions prepared from solvent/anti-solvent mixture showed better miscibility and physical stability over those prepared from the mixtures of good solvents. Thus, solid dispersions prepared from dichloromethane-acetone exhibited the best physicochemical attributes followed by those prepared from methanol-acetone. FT-IR analysis revealed differential drug-polymer interaction in solid dispersions prepared from various solvent blends, upon the exposure to elevated humidity. Spray-drying from a cocktail of good solvent and anti-solvent with narrower volatility difference produces solid dispersions with better miscibility and physical stability resulting from the simultaneous effect on the polymer conformation and better dispersivity of drug.

DEVELOPMENT OF SUSTAINED RELEASE TABLETS CONTAINING SOLID DISPERSIONS OF BACLOFEN

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K. H. Janardhana

2015-07-01

Full Text Available Sustained release tablets containing solid dispersions granules of a poorly water soluble drug were prepared to investigate the controlled release of the drug. Baclofen was chosen because of its poor water solubility and short elimination half-life. Poloxamer 188 and PEG 6000 were used as solid dispersion carrier. Free flowing solid dispersion granules were prepared by adsorbing the melt of the drug and carriers onto the surface of an adsorbent, Carbopol 934P followed by direct compression with HPMC K4M and HPMC K100 to obtain an solid dispersion loaded sustained release tablets. FTIR studies confirmed that the compatibility of drug and carriers. Differential scanning calorimetry (DSC and X-ray diffraction (XRD revealed partially amorphous structures of the drug in solid dispersion granules. The solid dispersion granules dissolved completely within 30 min, which was much faster than that of pure drug baclofen. The sustained release of baclofen from the solid dispersion containing tablet was achieved for 2 h in gastric fluid (pH 1.2 and for up to 10 h in intestinal fluid (pH 6.8. A combination of solid dispersion techniques using adsorption and sustained release concepts is a promising approach to control the release rate of poorly water-soluble drugs.

DEVELOPMENT OF SUSTAINED RELEASE TABLETS CONTAINING SOLID DISPERSIONS OF BACLOFEN

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K. H. Janardhana

2013-12-01

Full Text Available Sustained release tablets containing solid dispersions granules of a poorly water soluble drug were prepared to investigate the controlled release of the drug. Baclofen was chosen because of its poor water solubility and short elimination half-life. Poloxamer 188 and PEG 6000 were used as solid dispersion carrier. Free flowing solid dispersion granules were prepared by adsorbing the melt of the drug and carriers onto the surface of an adsorbent, Carbopol 934P followed by direct compression with HPMC K4M and HPMC K100 to obtain an solid dispersion loaded sustained release tablets. FTIR studies confirmed that the compatibility of drug and carriers. Differential scanning calorimetry (DSC and X-ray diffraction (XRD revealed partially amorphous structures of the drug in solid dispersion granules. The solid dispersion granules dissolved completely within 30 min, which was much faster than that of pure drug baclofen. The sustained release of baclofen from the solid dispersion containing tablet was achieved for 2 h in gastric fluid (pH 1.2 and for up to 10 h in intestinal fluid (pH 6.8. A combination of solid dispersion techniques using adsorption and sustained release concepts is a promising approach to control the release rate of poorly water-soluble drugs.

Development of megestrol acetate solid dispersion nanoparticles for enhanced oral delivery by using a supercritical antisolvent process.

Science.gov (United States)

Ha, Eun-Sol; Kim, Jeong-Soo; Baek, In-Hwan; Yoo, Jin-Wook; Jung, Yunjin; Moon, Hyung Ryong; Kim, Min-Soo

2015-01-01

In the present study, solid dispersion nanoparticles with a hydrophilic polymer and surfactant were developed using the supercritical antisolvent (SAS) process to improve the dissolution and oral absorption of megestrol acetate. The physicochemical properties of the megestrol acetate solid dispersion nanoparticles were characterized using scanning electron microscopy, differential scanning calorimetry, powder X-ray diffraction, and a particle-size analyzer. The dissolution and oral bioavailability of the nanoparticles were also evaluated in rats. The mean particle size of all solid dispersion nanoparticles that were prepared was nanoparticles. Hydroxypropylmethyl cellulose (HPMC) solid dispersion nanoparticles significantly increased the maximum dissolution when compared with polyvinylpyrrolidone K30 solid dispersion nanoparticles. The extent and rate of dissolution of megestrol acetate increased after the addition of a surfactant into the HPMC solid dispersion nanoparticles. The most effective surfactant was Ryoto sugar ester L1695, followed by D-α-tocopheryl polyethylene glycol 1000 succinate. In this study, the solid dispersion nanoparticles with a drug:HPMC:Ryoto sugar ester L1695 ratio of 1:2:1 showed >95% rapid dissolution within 30 minutes, in addition to good oral bioavailability, with approximately 4.0- and 5.5-fold higher area under the curve (0-24 hours) and maximum concentration, respectively, than raw megestrol acetate powder. These results suggest that the preparation of megestrol acetate solid dispersion nanoparticles using the supercritical antisolvent process is a promising approach to improve the dissolution and absorption properties of megestrol acetate.

Influence of waste solid on nuclide dispersal

International Nuclear Information System (INIS)

Seitz, M.G.; Steindler, M.J.

1981-01-01

The method most often considered for permanent disposal of radioactive waste is to incorporate the waste into a solid, which is then placed in a geologic formation. The solid is made of waste and nonradioactive additives, with the formulation selected to produce a durable solid that will minimize the potential for dispersal of the radionuclides. Leach rates of radionuclides incorporated in the solid waste indicate the quantity of radioactivity available for dispersal at any time; but leach rates of stable constituents can be just as important to radionuclide dispersal by groundwater. The constituents of the solid will perturb the chemical character of the groundwater and, thereby, profoundly affect the interaction of radionuclides with the geologic medium. An explicit example of how the solid waste can affect radionuclide dispersal is illustrated by the results of experiments that measure cesium adsorption in the presence of rubidium. The experiments were performed with granulated oolitic limestone that absorbed cesium from groundwater solutions to which various concentrations of stable rubidium chloride had been added. The results are expressed as partition coefficients. Large coefficients indicate strong adsorption by the rock and, hence, slow migration. The partition coefficient for cesium decreases as the rubidium concentration in solution is increased. Because the coeficient for cesium depends on the amount of rubidium in solution, it will depend on the leach rate of rubidium from the solid. Rubidium has no radionuclides of concern for long-term isolation of nuclear waste, so its leach rate from a waste solid is rarely ever reported

Liquid-solid phase transition of Ge-Sb-Te alloy observed by in-situ transmission electron microscopy

Energy Technology Data Exchange (ETDEWEB)

Berlin, Katja, E-mail: katja.berlin@pdi-berlin.de; Trampert, Achim

2017-07-15

Melting and crystallization dynamics of the multi-component Ge-Sb-Te alloy have been investigated by in-situ transmission electron microscopy (TEM). Starting point of the phase transition study is an ordered hexagonal Ge{sub 1}Sb{sub 2}Te{sub 4} thin film on Si(111) where the crystal structure and the chemical composition are verified by scanning TEM and electron energy-loss spectroscopy, respectively. The in-situ observation of the liquid phase at 600°C including the liquid-solid and liquid-vacuum interfaces and their movements was made possible due to an encapsulation of the TEM sample. The solid-liquid interface during melting displays a broad and diffuse transition zone characterized by a vacancy induced disordered state. Although the velocities of interface movements are measured to be in the nanometer per second scale, both, for crystallization and solidification, the underlying dynamic processes are considerably different. Melting reveals linear dependence on time, whereas crystallization exhibits a non-linear time-dependency featuring a superimposed start-stop motion. Our results may provide valuable insight into the atomic mechanisms at interfaces during the liquid-solid phase transition of Ge-Sb-Te alloys. - Highlights: • In-situ TEM observation of liquid Ge-Sb-Te phase transition due to encapsulation. • During melting: Observation of non-ordered interface transition due to premelting. • During solidification: Observation of non-linear time-dependent crystallization.

Liquid-solid phase transition of Ge-Sb-Te alloy observed by in-situ transmission electron microscopy

International Nuclear Information System (INIS)

Berlin, Katja; Trampert, Achim

2017-01-01

Melting and crystallization dynamics of the multi-component Ge-Sb-Te alloy have been investigated by in-situ transmission electron microscopy (TEM). Starting point of the phase transition study is an ordered hexagonal Ge 1 Sb 2 Te 4 thin film on Si(111) where the crystal structure and the chemical composition are verified by scanning TEM and electron energy-loss spectroscopy, respectively. The in-situ observation of the liquid phase at 600°C including the liquid-solid and liquid-vacuum interfaces and their movements was made possible due to an encapsulation of the TEM sample. The solid-liquid interface during melting displays a broad and diffuse transition zone characterized by a vacancy induced disordered state. Although the velocities of interface movements are measured to be in the nanometer per second scale, both, for crystallization and solidification, the underlying dynamic processes are considerably different. Melting reveals linear dependence on time, whereas crystallization exhibits a non-linear time-dependency featuring a superimposed start-stop motion. Our results may provide valuable insight into the atomic mechanisms at interfaces during the liquid-solid phase transition of Ge-Sb-Te alloys. - Highlights: • In-situ TEM observation of liquid Ge-Sb-Te phase transition due to encapsulation. • During melting: Observation of non-ordered interface transition due to premelting. • During solidification: Observation of non-linear time-dependent crystallization.

Concentration of organic compounds in natural waters with solid-phase dispersion based on advesicle modified silica prior to liquid chromatography.

Science.gov (United States)

Parisis, Nikolaos A; Giokas, Dimosthenis L; Vlessidis, Athanasios G; Evmiridis, Nicholaos P

2005-12-02

The ability of vesicle-coated silica to aid the extraction of organic compounds from water prior to liquid chromatographic analysis is presented for the first time. The method is based on the formation of silica supported cationic multi-lamellar vesicles of gemini surfactants inherently ensuring the presence of hydrophilic and hydrophobic sites for the partitioning of analytes bearing different properties. Method development is illustrated by studying the adsolubilization of UV absorbing chemicals from swimming pool water. Due to the requirement for external energy input (intense shearing) a method based on solid-phase dispersion (SPD) was applied producing better results than off-line solid-phase extraction (SPE). Meticulous investigation of the experimental parameters was conducted in order to elucidate the mechanisms behind the proposed extraction pattern. Analyte recoveries were quantitative under the optimum experimental conditions offering recoveries higher than 96% with RSD values below 5%.

Vortex-homogenized matrix solid-phase dispersion for the extraction of short chain chlorinated paraffins from indoor dust samples.

Science.gov (United States)

Chen, Yu-Hsuan; Chang, Chia-Yu; Ding, Wang-Hsien

2016-11-11

A simple and effective method for determining short chain chlorinated paraffins (SCCPs) in indoor dust is presented. The method employed a modified vortex-homogenized matrix solid-phase dispersion (VH-MSPD) prior to its detection by gas chromatography - electron-capture negative-ion mass spectrometry (GC-ECNI-MS) operating in the selected-ion-monitoring (SIM) mode. Under the best extraction conditions, 0.1-g of dust sample was dispersed with 0.1-g of silica gel by using vortex (2min) instead of using a mortar and pestle (3min). After that step, the blend was transferred to a glass column containing 3-g acidic silica gel, 2-g basic silica gel, and 2-g of deactivated silica gel, used as clean-up co-sorbents. Then, target analytes were eluted with 5mL of n-hexane/dichloromethane (2:1, v/v) mixture. The extract was evaporated to dryness under a gentle stream of nitrogen. The residue was then re-dissolved in n-hexane (10μL), and subjected to GC-ECNI-MS analysis. The limits of quantitation (LOQs) ranged from 0.06 to 0.25μg/g for each SCCP congener. Precision was less than 7% for both intra- and inter-day analysis. Trueness was above 89%, which was calculated by mean extraction recovery. The VH-MSPD combined with GC-ECNI-MS was successfully applied to quantitatively detect SCCPs from various indoor dust samples, and the concentrations ranged from 1.2 to 31.2μg/g. Copyright © 2016 Elsevier B.V. All rights reserved.

Investigation of Solid Dispersion of Atorvastatin Calcium in ...

African Journals Online (AJOL)

ATC), a poorly watersoluble 3-hydroxy 3-methyl glutaryl CoA (HMG-CoA) reductase inhibitor, by a solid dispersion technique using polyethylene glycol 6000 (PEG 6000) or polyvinylpyrrolidone k30 (PVP K30). Methods: The solid dispersions were ...

Fabrication of a novel hydrophobic/ion-exchange mixed-mode adsorbent for the dispersive solid-phase extraction of chlorophenols from environmental water samples.

Science.gov (United States)

Gao, Li; Wei, Yinmao

2016-08-01

A novel mixed-mode adsorbent was prepared by functionalizing silica with tris(2-aminoethyl)amine and 3-phenoxybenzaldehyde as the main mixed-mode scaffold due to the presence of the plentiful amino groups and benzene rings in their molecules. The adsorption mechanism was probed with acidic, natural and basic compounds, and the mixed hydrophobic and ion-exchange interactions were found to be responsible for the adsorption of analytes. The suitability of dispersive solid-phase extraction was demonstrated in the determination of chlorophenols in environmental water. Several parameters, including sample pH, desorption solvent, ionic strength, adsorbent dose, and extraction time were optimized. Under the optimal extraction conditions, the proposed dispersive solid-phase extraction coupled with high-performance liquid chromatography showed good linearity range and acceptable limits of detection (0.22∽0.54 ng/mL) for five chlorophenols. Notably, the higher extraction recoveries (88.7∽109.7%) for five chlorophenols were obtained with smaller adsorbent dose (10 mg) and shorter extraction time (15 min) compared with the reported methods. The proposed method might be potentially applied in the determination of trace chlorophenols in real water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid-phase extraction assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet to determine sildenafil and its analogues in dietary supplements.

Science.gov (United States)

Li, Jing; Roh, Si Hun; Shaodong, Jia; Hong, Ji Yeon; Lee, Dong-Kyu; Shin, Byong-Kyu; Park, Jeong Hill; Lee, Jeongmi; Kwon, Sung Won

2017-08-01

A novel analytical method for the simultaneous determination of the concentration of sildenafil and its five analogues in dietary supplements using solid-phase extraction assisted reversed-phase dispersive liquid-liquid microextraction based on solidification of floating organic droplet combined with ion-pairing liquid chromatography with an ultraviolet detector was developed. Parameters that affect extraction efficiency were systematically investigated, including the type of solid-phase extraction cartridge, pH of the extraction environment, and the type and volume of extraction and dispersive solvent. The method linearity was in the range of 5.0-100 ng/mL for sildenafil, homosildenafil, udenafil, benzylsildenafil, and thiosildenafil and 10-100 ng/mL for acetildenafil. The coefficients of determination were ≥0.996 for all regression curves. The sensitivity values expressed as limit of detection were between 2.5 and 7.5 ng/mL. Furthermore, intraday and interday precisions expressed as relative standard deviations were less than 5.7 and 9.9%, respectively. The proposed method was successfully applied to the analysis of sildenafil and its five analogues in complex dietary supplements. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

In vitro Dissolution Studies on Solid Dispersions of Mefenamic Acid.

Science.gov (United States)

Rao, K R S Sambasiva; Nagabhushanam, M V; Chowdary, K P R

2011-03-01

Solid dispersions of mefanamic acid with a water-soluble polymer polyvinyl pyrrolidine and a super disintegrant, primojel were prepared by common solvent and solvent evaporation methods employing methanol as the solvent. The dissolution rate and dissolution efficiency of the prepared solid dispersions were evaluated in comparison to the corresponding pure drug. Solid dispersions of mefenamic acid showed a marked enhancement in dissolution rate and dissolution efficiency. At 1:4 ratio of mefenamic acid-primojel a 2.61 fold increase in the dissolution rate of mefenamic acid was observed with solid dispersion. The solid dispersions in combined carriers gave much higher rates of dissolution than super disintegrants alone. Mefanamic acid-primojel-polyvinyl pyrrolidine (1:3.2:0.8) solid dispersion gave a 4.11 fold increase in the dissolution rate of mefenamic acid. Super disintegrants alone or in combination with polyvinyl pyrrolidine could be used to enhance the dissolution rate of mefenamic acid.

Preparation and Characterization of Solid Dispersions of Artemether by Freeze-Dried Method

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Muhammad Tayyab Ansari

2015-01-01

Full Text Available Solid dispersions of artemether and polyethylene glycol 6000 (PEG6000 were prepared in ratio 12 : 88 (group-1. Self-emulsified solid dispersions of artemether were prepared by using polyethylene glycol 6000, Cremophor-A25, olive oil, Transcutol, and hydroxypropyl methylcellulose (HPMC in ratio 12 : 75 : 5 : 4 : 2 : 2, respectively (group-2. In third group, only Cremophor-A25 was replaced with Poloxamer 188 compared to group-2. The solid dispersions and self-emulsified solid dispersions were prepared by physical and freeze dried methods, respectively. All samples were characterized by X-ray diffraction, attenuated total reflectance Fourier transform infrared spectroscopy, differential scanning calorimeter, scanning electron microscopy, and solubility, dissolution, and stability studies. X-ray diffraction pattern revealed artemether complete crystalline, whereas physical mixture and freeze-dried mixture of all three groups showed reduced peak intensities. In attenuated total reflectance Fourier transform infrared spectroscopy spectra, C–H stretching vibrations of artemether were masked in all prepared samples, while C–H stretching vibrations were representative of polyethylene glycol 6000, Cremophor-A25, and Poloxamer 188. Differential scanning calorimetry showed decreased melting endotherm and increased enthalpy change (ΔH in both physical mixture and freeze-dried mixtures of all groups. Scanning electron microscopy of freeze-dried mixtures of all samples showed glassy appearance, size reduction, and embedment, while their physical mixture showed size reduction and embedment of artemether by excipients. In group-1, solubility was improved up to 15 times, whereas group-2 showed up to 121 times increase but, in group-3, when Poloxamer 188 was used instead of Cremophor-A25, solubility of freeze-dried mixtures was increased up to 135 times. In fasted state simulated gastric fluid at pH 1.6, the dissolution of physical

New method based on combining ultrasonic assisted miniaturized matrix solid-phase dispersion and homogeneous liquid-liquid extraction for the determination of some organochlorinated pesticides in fish

International Nuclear Information System (INIS)

Rezaei, Farahnaz; Hosseini, Mohammad-Reza Milani

2011-01-01

Highlights: → Ultrasonic assisted miniaturized matrix solid-phase dispersion combined with HLLE was developed as a new method for the extraction of OCPs in fish. → The goal of this combination was to enhance the selectivity of HLLE procedure and to extend its application in biological samples. → This method proposed the advantages of good detection limits, lower consumption of reagents, and does not need any special instrumentation. - Abstract: In this study, ultrasonic assisted miniaturized matrix solid-phase dispersion (US-MMSPD) combined with homogeneous liquid-liquid extraction (HLLE) has been developed as a new method for the extraction of organochlorinated pesticides (OCPs) in fish prior to gas chromatography with electron capture detector (GC-ECD). In the proposed method, OCPs (heptachlor, aldrin, DDE, DDD, lindane and endrin) were first extracted from fish sample into acetonitrile by US-MMSPD procedure, and the extract was then used as consolute solvent in HLLE process. Optimal condition for US-MMSPD step was as follows: volume of acetonitrile, 1.5 mL; temperature of ultrasound, 40 deg. C; time of ultrasound, 10 min. For HLLE step, optimal results were obtained at the following conditions: volume of chloroform, 35 μL; volume of aqueous phase, 1.5 mL; volume of double distilled water, 0.5 mL; time of centrifuge, 10 min. Under the optimum conditions, the enrichment factors for the studied compounds were obtained in the range of 185-240, and the overall recoveries were ranged from 39.1% to 81.5%. The limits of detection were 0.4-1.2 ng g -1 and the relative standard deviations for 20 ng g -1 of the OCPs, varied from 3.2% to 8% (n = 4). Finally, the proposed method has been successfully applied to the analysis of the OCPs in real fish sample, and satisfactory results were obtained.

New method based on combining ultrasonic assisted miniaturized matrix solid-phase dispersion and homogeneous liquid-liquid extraction for the determination of some organochlorinated pesticides in fish

Energy Technology Data Exchange (ETDEWEB)

Rezaei, Farahnaz [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Narmak, Tehran 16846 (Iran, Islamic Republic of); Hosseini, Mohammad-Reza Milani, E-mail: drmilani@iust.ac.ir [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Narmak, Tehran 16846 (Iran, Islamic Republic of); Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Narmak, Tehran 16846 (Iran, Islamic Republic of)

2011-09-30

Highlights: {yields} Ultrasonic assisted miniaturized matrix solid-phase dispersion combined with HLLE was developed as a new method for the extraction of OCPs in fish. {yields} The goal of this combination was to enhance the selectivity of HLLE procedure and to extend its application in biological samples. {yields} This method proposed the advantages of good detection limits, lower consumption of reagents, and does not need any special instrumentation. - Abstract: In this study, ultrasonic assisted miniaturized matrix solid-phase dispersion (US-MMSPD) combined with homogeneous liquid-liquid extraction (HLLE) has been developed as a new method for the extraction of organochlorinated pesticides (OCPs) in fish prior to gas chromatography with electron capture detector (GC-ECD). In the proposed method, OCPs (heptachlor, aldrin, DDE, DDD, lindane and endrin) were first extracted from fish sample into acetonitrile by US-MMSPD procedure, and the extract was then used as consolute solvent in HLLE process. Optimal condition for US-MMSPD step was as follows: volume of acetonitrile, 1.5 mL; temperature of ultrasound, 40 deg. C; time of ultrasound, 10 min. For HLLE step, optimal results were obtained at the following conditions: volume of chloroform, 35 {mu}L; volume of aqueous phase, 1.5 mL; volume of double distilled water, 0.5 mL; time of centrifuge, 10 min. Under the optimum conditions, the enrichment factors for the studied compounds were obtained in the range of 185-240, and the overall recoveries were ranged from 39.1% to 81.5%. The limits of detection were 0.4-1.2 ng g{sup -1} and the relative standard deviations for 20 ng g{sup -1} of the OCPs, varied from 3.2% to 8% (n = 4). Finally, the proposed method has been successfully applied to the analysis of the OCPs in real fish sample, and satisfactory results were obtained.

In vitro characterization of a novel polymeric system for preparation of amorphous solid drug dispersions.

Science.gov (United States)

Mahmoudi, Zahra N; Upadhye, Sampada B; Ferrizzi, David; Rajabi-Siahboomi, Ali R

2014-07-01

Preparation of amorphous solid dispersions using polymers is a commonly used formulation strategy for enhancing the solubility of poorly water-soluble drugs. However, often a single polymer may not bring about a significant enhancement in solubility or amorphous stability of a poorly water-soluble drug. This study describes application of a unique and novel binary polymeric blend in preparation of solid dispersions. The objective of this study was to investigate amorphous solid dispersions of glipizide, a BCS class II model drug, in a binary polymeric system of polyvinyl acetate phthalate (PVAP) and hypromellose (hydroxypropyl methylcellulose, HPMC). The solid dispersions were prepared using two different solvent methods: rotary evaporation (rotavap) and fluid bed drug layering on sugar spheres. The performance and physical stability of the dispersions were evaluated with non-sink dissolution testing, powder X-ray diffraction (PXRD), and modulated differential scanning calorimetry (mDSC). PXRD analysis demonstrated an amorphous state for glipizide, and mDSC showed no evidence of phase separation. Non-sink dissolution testing in pH 7.5 phosphate buffer indicated more than twofold increase in apparent solubility of the drug with PVAP-HPMC system. The glipizide solid dispersions demonstrated a high glass transition temperature (Tg) and acceptable chemical and physical stability during the stability period irrespective of the manufacturing process. In conclusion, the polymeric blend of PVAP-HPMC offers a unique formulation approach for developing amorphous solid dispersions with the flexibility towards the use of these polymers in different ratios and combined quantities depending on drug properties.

EVALUATION OF A BUFFERED SOLID PHASE DISPERSION PROCEDURE ADAPTED FOR PESTICIDE ANALYSES IN THE SOIL MATRIX

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Ana María Domínguez

2015-08-01

Full Text Available An evaluation of the pesticides extracted from the soil matrix was conducted using a citrate-buffered solid phase dispersion sample preparation method (QuEChERS. The identification and quantitation of pesticide compounds was performed using gas chromatography-mass spectrometry. Because of the occurrence of the matrix effect in 87% of the analyzed pesticides, the quantification was performed using matrix-matched calibration. The method's quantification limits were between 0.01 and 0.5 mg kg-1. Repeatability and intermediate precision, expressed as a relative standard deviation percentage, were less than 20%. The recoveries in general ranged between 62% and 99%, with a relative standard deviation < 20%. All the responses were linear, with a correlation coefficient (r ≥0.99.

Dispersive solid phase micro-extraction of mercury(II from environmental water and vegetable samples with ionic liquid modified graphene oxide nanoparticles

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Nasrollahpour Atefeh

2017-01-01

Full Text Available A new dispersive solid phase micro-extraction (dispersive-SPME method for separation and preconcentration of mercury(II using ionic liquid modified magnetic reduced graphene oxide (IL-MrGO nanoparticles, prior to the measurement by cold vapour atomic absorption spectrometry (CV-AAS has been developed. The IL-MrGO composite was characterized by Brunauer– Emmett–Teller method (BET for adsorption-desorption measurement, thermogravimetric analysis (TGA, powder X-ray diffraction (XRD and X-ray photoelectron spectroscopy (XPS. The method is based on the sorption of mercury( II on IL-MrGO nanoparticles due to electrostatic interaction and complex formation of ionic liquid part of IL-MrGO with mercury(II. The effect of experimental parameters for preconcentration of mercury(II, such as solution type, concentration and volume of the eluent, pH, time of the sorption and desorption, amount of the sorbent and coexisting ion concentration have been optimized. Under the optimized conditions, a linear response was obtained in the concentration range of 0.08–10 ng mL-1 with a determination coefficient of 0.9995. The limit of detection (LOD of the method at a signal to noise ratio of 3 was 0.01 ng mL-1. Intra-day and inter-day precisions were obtained equal to 3.4 and 4.5 %, respectively. The dispersive solid phase micro-extraction of mercury(II on IL-MrGO nanoparticles coupled with cold vapour atomic absorption spectrometry was successfully used for extraction and determination of mercury(II in water and vegetable samples.

Fundamental aspects of solid dispersion technology for poorly soluble drugs

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Yanbin Huang

2014-02-01

Full Text Available The solid dispersion has become an established solubilization technology for poorly water soluble drugs. Since a solid dispersion is basically a drug–polymer two-component system, the drug–polymer interaction is the determining factor in its design and performance. In this review, we summarize our current understanding of solid dispersions both in the solid state and in dissolution, emphasizing the fundamental aspects of this important technology.

Using Flory-Huggins phase diagrams as a pre-formulation tool for the production of amorphous solid dispersions: a comparison between hot-melt extrusion and spray drying.

Science.gov (United States)

Tian, Yiwei; Caron, Vincent; Jones, David S; Healy, Anne-Marie; Andrews, Gavin P

2014-02-01

Amorphous drug forms provide a useful method of enhancing the dissolution performance of poorly water-soluble drugs; however, they are inherently unstable. In this article, we have used Flory-Huggins theory to predict drug solubility and miscibility in polymer candidates, and used this information to compare spray drying and melt extrusion as processes to manufacture solid dispersions. Solid dispersions were prepared using two different techniques (hot-melt extrusion and spray drying), and characterised using a combination of thermal (thermogravimetric analysis and differential scanning calorimetry), spectroscopic (Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction methods. Spray drying permitted generation of amorphous solid dispersions across a wider drug concentration than melt extrusion. Melt extrusion provided sufficient energy for more intimate mixing to be achieved between drug and polymer, which may improve physical stability. It was also confirmed that stronger drug-polymer interactions might be generated through melt extrusion. Remixing and dissolution of recrystallised felodipine into the polymeric matrices did occur during the modulated differential scanning calorimetry analysis, but the complementary information provided from FTIR confirms that all freshly prepared spray-dried samples were amorphous with the existence of amorphous drug domains within high drug-loaded samples. Using temperature-composition phase diagrams to probe the relevance of temperature and drug composition in specific polymer candidates facilitates polymer screening for the purpose of formulating solid dispersions. © 2013 Royal Pharmaceutical Society.

Phase behavior and phase inversion for dispersant systems

International Nuclear Information System (INIS)

Solheim, A.; Brandvik, P.J.

1991-06-01

This report describes some preliminary phase behavior studies and phase inversion temperature measurements in seawater, bunker oil and dispersant. The objectives have been to find new ways of characterizing dispersants for dispersing oil spill at sea and, perhaps, to throw new lights on the mechanism of dispersion formation (oil-in-water emulsification). The work has been focussed on the relation to phase behavior and the existence of microemulsion in equilibrium with excess oil and water phases. The dispersing process is also compared to the recommended conditions for emulsion formation. When forming an oil-in-water emulsion in an industrial process, it is recommended to choose an emulsifier which gives a phase inversion temperature (PIT) which is 20 - 60 o C higher than the actual temperature for use. The emulsification process must take place close to the PIT which is the temperature at which the emulsion change from oil-in-water emulsion to water-in-oil emulsion when the system is stirred. This condition corresponds to the temperature where the phase behavior change character. The purpose has been to find out if the composition of the dispersants corresponds to the recommendations for oil-in-water emulsification. The amount of experimental work has been limited. Two kinds of experiments have been carried out. Phase behavior studies have been done for seawater, bunker oil and four different dispersants where one had an optimal composition. The phase behavior was hard to interpret and is not recommended for standard dispersants test. The other experimental technique was PIT-measurements by conductivity measurements versus temperature. 4 figs., 1 tab., 4 refs

Solid state synthesis of water-dispersible silicon nanoparticles from silica nanoparticles

International Nuclear Information System (INIS)

Kravitz, Keren; Kamyshny, Alexander; Gedanken, Aharon; Magdassi, Shlomo

2010-01-01

A solid state synthesis for obtaining nanocrystalline silicon was performed by high temperature reduction of commercial amorphous nanosilica with magnesium powder. The obtained silicon powder contains crystalline silicon phase with lattice spacings characteristic of diamond cubic structure (according to high resolution TEM), and an amorphous phase. In 29 Si CP MAS NMR a broad multicomponent peak corresponding to silicon is located at -61.28 to -69.45 ppm, i.e. between the peaks characteristic of amorphous and crystalline Si. The powder has displayed red luminescence while excited under UV illumination, due to quantum confinement within the nanocrystals. The silicon nanopowder was successfully dispersed in water containing poly(vinyl alcohol) as a stabilizing agent. The obtained dispersion was also characterized by red photoluminescence with a band maximum at 710 nm, thus enabling future functional coating applications. - Graphical abstract: High temperature reduction of amorphous nanosilica with magnesium powder results in the formation of powder containing crystalline silicon phase The powder displays red luminescence while excited under UV illumination, due to quantum confinement within the Si nanocrystals, and can be successfully dispersed in water containing poly(vinyl alcohol) as a stabilizing agent. The obtained dispersion was also characterized by red photoluminescence, thus enabling future functional coating applications.

Graphene-coated polystyrene-divinylbenzene dispersive solid-phase extraction coupled with supercritical fluid chromatography for the rapid determination of 10 allergenic disperse dyes in industrial wastewater samples.

Science.gov (United States)

Lou, Chaoyan; Wu, Can; Zhang, Kai; Guo, Dandan; Jiang, Lei; Lu, Yang; Zhu, Yan

2018-05-18

Allergenic disperse dyes are a group of environmental contaminants, which are toxic and mutagenic to human beings. In this work, a method of dispersive solid-phase extraction (d-SPE) using graphene-coated polystyrene-divinylbenzene (G@PS-DVB) microspheres coupled with supercritical fluid chromatography (SFC) was proposed for the rapid determination of 10 allergenic disperse dyes in industrial wastewater samples. G@PS-DVB microspheres were synthesized by coating graphene (G) sheets onto polystyrene-divinylbenzene (PS-DVB) polymers. Such novel sorbents were employed in d-SPE for the purification and concentration of allergenic disperse dyes in wastewater samples prior to the determination by SFC with UV detection. To achieve the maximum extraction efficiency for the target dyes, several parameters influencing d-SPE process such as sorbent dosage, extraction time, desorption conditions were investigated. SFC conditions including stationary phase, modifier composition and percentage, column temperature, backpressure and flow rate were optimized to well separate the allergenic disperse dyes. Under the optimum conditions, satisfactory linear relationship (R ≥ 0.9989) was observed with the concentration of dyes ranging from 0.02 to 10.0 μg/mL. The limits of detection (LOD, S/N = 3) for the ten dyes were in the range of 1.1-15.6 ng/mL. Recoveries for the spiked samples were between 89.1% and 99.7% with relative standard deviations (RSD) lower than 10.5% in all cases. The proposed method is time-saving, green, precise and repeatable for the analysis of the target dyes. Furthermore, the application of G@PS-DVB based d-SPE process can be potentially expanded to isolate and concentrate other aromatic compounds in various matrices and supercritical fluid chromatography methodology featuring rapidity, accuracy and green will be an ideal candidate for the analysis of these compounds. Copyright © 2018 Elsevier B.V. All rights reserved.

Development and evaluation of alginate-chitosan gastric floating beads loading with oxymatrine solid dispersion.

Science.gov (United States)

Liu, Yanhua; Chen, Lihong; Zhou, Chengming; Yang, Jianhong; Hou, Yanhui; Wang, Wenping

2016-01-01

Oxymatrine (OM) can be metabolized to matrine in gastrointestinal ileocecal valve after oral administration, which affects pharmacological activity and reduce bioavailability of OM. A type of multiple-unit alginate-chitosan (Alg-Cs) floating beads was prepared by the ionotropic gelation method for gastroretention delivery of OM. A solid dispersion technique was applied and incorporated into beads to enhance the OM encapsulation efficiency (EE) and sustain the drug release. The surface morphology and internal hollow structure of beads were evaluated using optical microscopy and scanning electron microscopy (SEM). The developed Alg-Cs beads were spherical in shape with hollow internal structure and had particle size of 3.49 ± 0.09 mm and 1.33 ± 0.09 mm for wet and dried beads. Over 84% of the optimized OM solid dispersion-loaded Alg-Cs beads were able to continuously float over the simulated gastric fluid for 12 h in vitro. The OM solid dispersion-loaded Alg-Cs beads showed drug EE of 67.07%, which was much higher than that of beads loading with pure OM. Compared with the immediate release of OM capsules and pure OM-loaded beads, the release of OM from solid dispersion-loaded Alg-Cs beads was in a sustained-release manner for 12 h. Prolonged gastric retention time of over 8.5 h was achieved for OM solid dispersion-loaded Alg-Cs floating beads in healthy rabbit in in vivo floating ability evaluated by X-ray imaging. The developed Alg-Cs beads loading with OM solid dispersion displayed excellent performance features characterized by excellent gastric floating ability, high drug EE and sustained-release pattern. The study illustrated the potential use of Alg-Cs floating beads combined with the solid dispersion technique for prolonging gastric retention and sustaining release of OM, which could provide a promising drug delivery system for gastric-specific delivery of OM for bioavailability enhancement.

Separating DDTs in edible animal fats using matrix solid-phase dispersion extraction with activated carbon filter, Toyobo-KF.

Science.gov (United States)

Furusawa, Naoto

2006-09-01

A technique is presented for the economical, routine, and quantitative analysis of contamination by dichloro-diphenyl-trichloroethanes (DDTs) [pp'-DDT, pp'-dichlorodiphenyl dichloroethylene, and pp'-dichlorodiphenyl dichloreothane in beef tallow and chicken fat samples, based on their separation using matrix solid-phase dispersion (MSPD) extraction with Toyobo-KF, an activated carbon fiber. Toyobo-KF is a newly applied MSPD sorbent, and it is followed by reversed-phase high-performance liquid chromatography (HPLC) with a photodiode array detector. The resulting analytical performance parameters [recoveries of spiked DDTs (0.1, 0.2, and 0.4 microg/g) > or = 81%, with relative standard deviations of < or = 8% (n = 5), and quantitation limits < or = 0.03 microg/g], with minimal handling and cost-efficiency, indicate that the present MSPD-HPLC method may be a useful tool for routine monitoring of DDT contamination in meat.

Phase Evolution and Mechanical Behavior of the Semi-Solid SIMA Processed 7075 Aluminum Alloy

Directory of Open Access Journals (Sweden)

Behzad Binesh

2016-02-01

Full Text Available Microstructural and mechanical behaviors of semi-solid 7075 aluminum alloy were investigated during semi-solid processing. The strain induced melt activation (SIMA process consisted of applying uniaxial compression strain at ambient temperature and subsequent semi-solid treatment at 600–620 °C for 5–35 min. Microstructures were characterized by scanning electron microscope (SEM, energy dispersive spectroscopy (EDS, and X-ray diffraction (XRD. During the isothermal heating, intermetallic precipitates were gradually dissolved through the phase transformations of α-Al + η (MgZn2 → liquid phase (L and then α-Al + Al2CuMg (S + Mg2Si → liquid phase (L. However, Fe-rich precipitates appeared mainly as square particles at the grain boundaries at low heating temperatures. Cu and Si were enriched at the grain boundaries during the isothermal treatment while a significant depletion of Mg was also observed at the grain boundaries. The mechanical behavior of different SIMA processed samples in the semi-solid state were investigated by means of hot compression tests. The results indicated that the SIMA processed sample with near equiaxed microstructure exhibits the highest flow resistance during thixoforming which significantly decreases in the case of samples with globular microstructures. This was justified based on the governing deformation mechanisms for different thixoformed microstructures.

Development of megestrol acetate solid dispersion nanoparticles for enhanced oral delivery by using a supercritical antisolvent process

Directory of Open Access Journals (Sweden)

Ha ES

2015-08-01

Full Text Available Eun-Sol Ha,1 Jeong-Soo Kim,2 In-hwan Baek,3 Jin-Wook Yoo,1 Yunjin Jung,1 Hyung Ryong Moon,1 Min-Soo Kim1 1College of Pharmacy, Pusan National University, 2Dong-A ST Co Ltd, Yongin, 3College of Pharmacy, Kyungsung University, Busan, South Korea Abstract: In the present study, solid dispersion nanoparticles with a hydrophilic polymer and surfactant were developed using the supercritical antisolvent (SAS process to improve the dissolution and oral absorption of megestrol acetate. The physicochemical properties of the megestrol acetate solid dispersion nanoparticles were characterized using scanning electron microscopy, differential scanning calorimetry, powder X-ray diffraction, and a particle-size analyzer. The dissolution and oral bioavailability of the nanoparticles were also evaluated in rats. The mean particle size of all solid dispersion nanoparticles that were prepared was <500 nm. Powder X-ray diffraction and differential scanning calorimetry measurements showed that megestrol acetate was present in an amorphous or molecular dispersion state within the solid dispersion nanoparticles. Hydroxypropylmethyl cellulose (HPMC solid dispersion nanoparticles significantly increased the maximum dissolution when compared with polyvinylpyrrolidone K30 solid dispersion nanoparticles. The extent and rate of dissolution of megestrol acetate increased after the addition of a surfactant into the HPMC solid dispersion nanoparticles. The most effective surfactant was Ryoto sugar ester L1695, followed by d-a-tocopheryl polyethylene glycol 1000 succinate. In this study, the solid dispersion nanoparticles with a drug:HPMC:Ryoto sugar ester L1695 ratio of 1:2:1 showed >95% rapid dissolution within 30 minutes, in addition to good oral bioavailability, with approximately 4.0- and 5.5-fold higher area under the curve (0–24 hours and maximum concentration, respectively, than raw megestrol acetate powder. These results suggest that the preparation of megestrol

Solid phase radioimmunoassays

International Nuclear Information System (INIS)

Wide, L.

1977-01-01

Solid phase coupled antibodies were introduced to facilitate the separation of bound and free labelled ligand in the competitive inhibition radioimmunoassay. Originally, the solid matrix used was in the form of small particles and since then a number of different matrices have been used such as very fine powder particles, gels, paper and plastic discs, magnetic particles and the inside surface of plastic tubes. The coupling of antibodies may be that of a covalent chemical binding, a strong physical adsorbtion, or an immunological binding to a solid phase coupled antigen. New principles of radioimmunoassay such as the solid phase sandwich techniques and the immunoradiometric assay were developped from the use of solid phase coupled antigens and antibodies. The solid phase sandwich techniques are reagent excess methods with a very wide applicability. Several of the different variants of solid phase techniques are suitable for automation. Advantages and disadvantages of solid phase radioimmunoassays when compared with those using soluble reagents are discussed. (orig.) [de

Measurement of phase interaction in dispersed gas-particle two-phase flow by phase-doppler anemometry

Directory of Open Access Journals (Sweden)

Mergheni Ali Mohamed

2008-01-01

Full Text Available For simultaneous measurement of size and velocity distributions of continuous and dispersed phases in a two-phase flow a technique phase-Doppler anemometry was used. Spherical glass particles with a particle diameter range from 102 up to 212 µm were used. In this two-phase flow an experimental results are presented which indicate a significant influence of the solid particles on the flow characteristics. The height of influence of these effects depends on the local position in the jet. Near the nozzle exit high gas velocity gradients exist and therefore high turbulence production in the shear layer of the jet is observed. Here the turbulence intensity in the two-phase jet is decreased compared to the single-phase jet. In the developed zone the velocity gradient in the shear layer is lower and the turbulence intensity reduction is higher. .

Analytical study of solids-gas two phase flow

International Nuclear Information System (INIS)

Hosaka, Minoru

1977-01-01

Fundamental studies were made on the hydrodynamics of solids-gas two-phase suspension flow, in which very small solid particles are mixed in a gas flow to enhance the heat transfer characteristics of gas cooled high temperature reactors. Especially, the pressure drop due to friction and the density distribution of solid particles are theoretically analyzed. The friction pressure drop of two-phase flow was analyzed based on the analytical result of the single-phase friction pressure drop. The calculated values of solid/gas friction factor as a function of solid/gas mass loading are compared with experimental results. Comparisons are made for Various combinations of Reynolds number and particle size. As for the particle density distribution, some factors affecting the non-uniformity of distribution were considered. The minimum of energy dispersion was obtained with the variational principle. The suspension density of particles was obtained as a function of relative distance from wall and was compared with experimental results. It is concluded that the distribution is much affected by the particle size and that the smaller particles are apt to gather near the wall. (Aoki, K.)

Materials research for passive solar systems: Solid-state phase-change materials

Science.gov (United States)

Benson, D. K.; Webb, J. D.; Burrows, R. W.; McFadden, J. D. O.; Christensen, C.

1985-03-01

A set of solid-state phase-change materials is being evaluated for possible use in passive solar thermal energy storage systems. The most promising materials are organic solid solutions of pentaerythritol (C5H12O4), pentaglycerinve (C5H12O3), and neopentyl glycol (C5H12O2). Solid solution mixtures of these compounds can be tailored so that they exhibit solid-to-solid phase transformations at any desired temperature between 25 C and 188 C, and have latent heats of transformation etween 20 and 70 cal/g. Transformation temperatures, specific heats, and latent heats of transformation have been measured for a number of these materials. Limited cyclic experiments suggest that the solid solutions are stable. These phase-change materials exhibit large amounts of undercooling; however, the addition of certain nucleating agents as particulate dispersions in the solid phase-change material greatly reduces this effect. Computer simulations suggest that the use of an optimized solid-state phase-change material in a Trombe wall could provide better performance than a concrete Trombe wall four times thicker and nine times heavier.

Partitioning of fresh crude oil between floating, dispersed and sediment phases: Effect of exposure order to dispersant and granular materials.

Science.gov (United States)

Boglaienko, Daria; Tansel, Berrin

2016-06-15

When three or more high and low energy substrates are mixed, wetting order can significantly affect the behavior of the mixture. We analyzed the phase distribution of fresh floating Louisiana crude oil into dispersed, settled and floating phases depending on the exposure sequence to Corexit 9500A (dispersant) and granular materials. In the experiments artificial sea water at salinity 34‰ was used. Limestone (2.00-0.300 mm) and quartz sand (0.300-0.075 mm) were used as the natural granular materials. Dispersant Corexit 9500A increased the amount of dispersed oil up to 33.76 ± 7.04%. Addition of granular materials after the dispersant increased dispersion of oil to 47.96 ± 1.96%. When solid particles were applied on the floating oil before the dispersant, oil was captured as oil-particle aggregates and removed from the floating layer. However, dispersant addition led to partial release of the captured oil, removing it from the aggregated form to the dispersed and floating phases. There was no visible oil aggregation with the granular materials when quartz or limestone was at the bottom of the flask before the addition of oil and dispersant. The results show that granular materials can be effective when applied from the surface for aggregating or dispersing oil. However, the granular materials in the sediments are not effective neither for aggregating nor dispersing floating oil. Copyright © 2016 Elsevier Ltd. All rights reserved.

High performance preconcentration of inorganic Se species by dispersive micro-solid phase extraction with a nanosilica-ionic liquid hybrid material

Science.gov (United States)

Llaver, Mauricio; Coronado, Eduardo A.; Wuilloud, Rodolfo G.

2017-12-01

A highly sensitive and efficient dispersive micro-solid phase extraction (D-μ-SPE) method was developed for inorganic Se speciation analysis. A novel ionic liquid (IL)-nanomaterial hybrid consisting of 1-dodecyl-3-methylimidazolium bromide-functionalized nanosilica was used for the efficient retention of Se(IV) complexed with ammonium pyrrolidine dithiocarbamate, followed by elution with an ethyl acetate/Triton X-114 mixture and determination by electrothermal atomic absorption spectroscopy. The Se(VI) species was selectively determined by difference between total inorganic Se and Se(IV) after pre-reduction. The IL-nanomaterial hybrid was characterized by Fourier transform infrared spectroscopy and transmission electronic microscopy. Likewise, Se(IV) sorption capacity of the retention material and maximum amount of IL loaded on its surface were determined. Several factors concerning the functionalization, extraction and elution steps were optimized, yielding a 100% extraction efficiency for Se(IV) under optimal conditions. A limit of detection of 1.1 ng L- 1, a relative standard deviation of 5.7% and a 110-fold enhancement factor were obtained. The D-μ-SPE method was successfully applied to several water samples from different origins and compositions, including rain, tap, underground, river and sea.

[Effect of stability and dissolution of realgar nano-particles using solid dispersion technology].

Science.gov (United States)

Guo, Teng; Shi, Feng; Yang, Gang; Feng, Nian-Ping

2013-09-01

To improve the stability and dissolution of realgar nano-particles by solid dispersion. Using polyethylene glycol 6000 and poloxamer-188 as carriers, the solid dispersions were prepare by melting method. XRD, microscopic inspection were used to determine the status of realgar nano-particles in solid dispersions. The content and stability test of As(2)0(3) were determined by DDC-Ag method. Hydride generation atomic absorption spectrometry was used to determine the content of Arsenic and investigated the in vitro dissolution behavior of solid dispersions. The results of XRD and microscopic inspection showed that realgar nano-particles in solid dispersions were amorphous. The dissolution amount and rate of Arsenic from realgar nano-particles of all solid dispersions were increased significantly, the reunion of realgar nano-particles and content of As(2)0(3) were reduced for the formation of solid dispersions. The solid dispersion of realgar nano-particles with poloxamer-188 as carriers could obviously improve stability, dissolution and solubility.

Phase segregation in cerium-lanthanum solid solutions

NARCIS (Netherlands)

Belliere, V.; Joorst, G; Stephan, O; de Groot, FMF; Weckhuysen, BM

2006-01-01

Electron energy-loss spectroscopy (EELS) in combination with scanning transmission electron microscopy ( STEM) reveals that the La enrichment at the surface of cerium-lanthanum solid solutions is an averaged effect and that segregation occurs in a mixed oxide phase. This separation occurs within a

Solid phase microextraction.

Science.gov (United States)

Pawliszyn, J

2001-01-01

Solid Phase Microextraction (SPME) uses a small volume of sorbent dispersed typically on the surface of small fibres, to isolate and concentrate analytes from sample matrix. After contact with sample, analytes are absorbed or adsorbed by the fibre phase (depending on the nature of the coating) until an equilibrium is reached in the system. The amount of an analyte extracted by the coating at equilibrium is determined by the magnitude of the partition coefficient of the analyte between the sample matrix and the coating material. After the extraction step, the fibres are transferred, with the help of a syringe-like handling device, to analytical instrument, for separation and quantitation of target analytes. This technique integrates sampling, extraction and sample introduction and is a simple way of facilitating on-site monitoring. Applications of this technique include environmental monitoring, industrial hygiene, process monitoring, clinical, forensic, food, flavour, fragrance and drug analyses, in laboratory and on-site analysis.

Development and Physicochemical Characterization of Sirolimus Solid Dispersions Prepared by Solvent Evaporation Method

Directory of Open Access Journals (Sweden)

Shahram Emami

2014-12-01

Full Text Available Purpose: The aim of the present investigation was preparation and characterization of sirolimus solid dispersions by solvent evaporation technique to improve its dissolution properties. Methods: Polyvinylpyrrolidone (PVP, Poloxamer 188 and Cremophore RH40 were used to prepare the solid dispersions of sirolimus. In vitro dissolution study using USP type I apparatus, were performed in distilled water (containing SLS 0.4% for pure sirolimus, physical mixtures, Rapamune and prepared solid dispersions. The characterization of solid dispersions was performed using Fourier Transform Infrared (FTIR Spectroscopy and Differential Scanning Calorimetry (DSC. Results: More than 75% of sirolimus was released within 30 minutes from all prepared solid dispersions. The dissolution rate of all prepared solid dispersion powders were more than physical mixtures. The absence of sirolimus peak in the DSC spectrum of solid dispersions indicated the conversion of crystalline form of sirolimus into amorphous form. The results from FT-IR spectroscopy showed that there was no significant change in the FT-IR spectrum of solid dispersions indicating absence of well-defined interaction between drug and carriers. Conclusion: It was concluded that solid dispersion method, using PVP, Poloxamer 188 and Cremophore RH40 can improve dissolution rate of sirolimus.

Direct phase selection of initial phases from single-wavelength anomalous dispersion (SAD) for the improvement of electron density and ab initio structure determination.

Science.gov (United States)

Chen, Chung-De; Huang, Yen-Chieh; Chiang, Hsin-Lin; Hsieh, Yin-Cheng; Guan, Hong-Hsiang; Chuankhayan, Phimonphan; Chen, Chun-Jung

2014-09-01

Optimization of the initial phasing has been a decisive factor in the success of the subsequent electron-density modification, model building and structure determination of biological macromolecules using the single-wavelength anomalous dispersion (SAD) method. Two possible phase solutions (φ1 and φ2) generated from two symmetric phase triangles in the Harker construction for the SAD method cause the well known phase ambiguity. A novel direct phase-selection method utilizing the θ(DS) list as a criterion to select optimized phases φ(am) from φ1 or φ2 of a subset of reflections with a high percentage of correct phases to replace the corresponding initial SAD phases φ(SAD) has been developed. Based on this work, reflections with an angle θ(DS) in the range 35-145° are selected for an optimized improvement, where θ(DS) is the angle between the initial phase φ(SAD) and a preliminary density-modification (DM) phase φ(DM)(NHL). The results show that utilizing the additional direct phase-selection step prior to simple solvent flattening without phase combination using existing DM programs, such as RESOLVE or DM from CCP4, significantly improves the final phases in terms of increased correlation coefficients of electron-density maps and diminished mean phase errors. With the improved phases and density maps from the direct phase-selection method, the completeness of residues of protein molecules built with main chains and side chains is enhanced for efficient structure determination.

Magnetic silica nanomaterials for solid-phase extraction combined with dispersive liquid-liquid microextraction of ultra-trace quantities of plasticizers

International Nuclear Information System (INIS)

Yamini, Yadollah; Faraji, Mohammad; Adeli, Mahnaz

2015-01-01

We are presenting surface modified magnetic silica nanoparticles (m-Si-NPs) for use in solid-phase extraction combined with dispersive liquid-liquid microextraction (DLLME). The m-Si-NPs were surface-functionalized with octadecyl groups to give a material for the extraction of the plasticizers dibutyl phthalate, di(2-ethylhexyl) adipate and di(2-ethylhexyl) phthalate from water samples. The functionalized m-Si-NPs were characterized by scanning electron microscopy, FTIR spectroscopy, thermal gravimetric analysis, and vibrating sample magnetometry. The results showed that the m-Si-NPs were well functionalized with octadecyl groups. The effects of various experimental variables on the extraction efficiencies were investigated. The analytes were quantified by GC/FID. Under optimal conditions, the calibration plots are linear in the range from 0.01 to 100 μg∙L -1 , and very high enrichment factors (mean value ∼20,000) were obtained. As a result of the high enrichment factors, the detection limits are as low as 2–3 ng∙L -1 . The method was successfully employed to the extraction of the plasticizers from (spiked) water samples, and recoveries are in the order of 93.9 to 106.7 %. The method is low cost, fast, and very sensitive (author)

Matrix solid-phase dispersion extraction of organophosphorus pesticide using SiO2-poly(N-vinylimidazole)

International Nuclear Information System (INIS)

Gutiérrez-Solís, M C; Muñoz-Rodríguez, D; Carrera-Figueiras, C; Ávila-Ortega, A; Medina-Peralta, S

2013-01-01

A sorbent material based on silica particles modified with poly(N-vinylimidazole) (SiO 2 -PVI) has been evaluated for the treatment of samples by matrix solid-phase dispersion (MSPD). The extraction of four organophosphorus pesticides was done from a spiked tomato and the extracts were analyzed by gas chromatography coupled to mass spectrometry. Six elution solvents were evaluated and acetone was selected due to better recovery of the four pesticides and low background signal in the chromatograms. A factorial design 2 4 was used for selection of extraction conditions. The factors were contact time, acetone volume, treatment (with or without freeze-drying) and adsorbent (SiO 2 or SiO 2 -PVI). The best recoveries were obtained using 15 minutes of contact, 2 mL of solvent and sorbent without freeze-drying. The recoveries were between 60 and 83% for SiO 2 -PVI in spiked tomato with 0.2 and 0.8μg/g.

Innovative separation and preconcentration technique of coagulating homogenous dispersive micro solid phase extraction exploiting graphene oxide nanosheets.

Science.gov (United States)

Ghazaghi, Mehri; Mousavi, Hassan Zavvar; Rashidi, Ali Morad; Shirkhanloo, Hamid; Rahighi, Reza

2016-01-01

A uniquely novel, fast, and facile technique is introduced for the first time in which a scant amount of graphene oxide (GO), without modification, has been utilized in dispersive mode of solid phase extraction (SPE) for an efficient yet simple separation. The proposed method of coagulating homogenous dispersive micro solid phase extraction (CHD-µSPE) is based on coagulation of homogeneous GO solution with the aid of polyetheneimine (PEI). CHD-µSPE use full adsorption capacity of GO because in this method was used GO solution obtained from synthesis process without drying step and stacking nanosheets. In optimized condition, 30 µL GO solution (7 mg mL(-1)), obtained in synthesis process, was injected into 1.5 mL the sample solution followed by immediate injection of 53 µL PEI solution (1 mg mL(-1)). After inserting PEI, GO sheets aggregate and can be readily separated by centrifugation. PEI not only cause aggregation of GO, but also form three-dimensional network of GO with easy handling in following separation steps. Lead, cadmium, and chromium were selected as model analytes and the effecting parameters including the amount of GO, concentration of PEI, sample pH, extraction time, and type of desorption solvent were investigated and optimized. The results indicate that the proposed CHD-µSPE method can be successfully applied GO in dispersive mode of SPE without effecting on good capability adsorption of GO. The novel method was applied in determination of lead, cadmium, and chromium in water, human saliva, and urine samples by electrothermal atomic absorption spectrometry. The detection limits are as low as 0.035, 0.005, and 0.012 µg L(-1) for Pb, Cd, and Cr respectively. The intra-day precisions (RSDs) were lower than 3.8%. CHD-µSPE method showed a good linear ranges of 0.24-15.6, 0.015-0.95 and 0.039-2.33 µg L(-1) for Pb, Cd and Cr respectively. Method performance was investigated by determination of mentioned metal ions in river water, human urine and

Determination of phenolic acids and flavonoids in raw propolis by silica-supported ionic liquid-based matrix solid phase dispersion extraction high performance liquid chromatography-diode array detection.

Science.gov (United States)

Wang, Zhibing; Sun, Rui; Wang, Yuanpeng; Li, Na; Lei, Lei; Yang, Xiao; Yu, Aimin; Qiu, Fangping; Zhang, Hanqi

2014-10-15

The silica-supported ionic liquid (S-SIL) was prepared by impregnation and used as the dispersion adsorbent of matrix solid phase dispersion (MSPD) for the simultaneous extraction of eight phenolic acids and flavonoids, including caffeic acid, ferulic acid, morin, luteolin, quercetin, apigenin, chrysin, and kaempferide in raw propolis. High performance liquid chromatography with a Zorbax SB-C18 column (150mm×4.6mm, 3.5μm) was used for separation of the analytes. The mobile phase consisted of 0.2% phosphoric acid aqueous solution and acetonitrile and the flow rate of the mobile phase was 0.5mL/min. The experimental conditions for silica-supported ionic liquid-based matrix solid phase dispersion (S-SIL-based MSPD) were optimized. S-SIL containing 10% [C6MIM]Cl was used as dispersant, 20mL of n-hexane as washing solvent and 15mL of methanol as elution solvent. The ratio of S-SIL to sample was selected to be 4:1. The standard curves showed good linear relationship (r>0.9995). The limits of detection and quantification were in the range of 5.8-22.2ngmL(-1) and 19.2-74.0ngmL(-1), respectively. The relative standard deviations (RSDs) of intra-day and inter-day determination were lower than 8.80% and 11.19%, respectively. The recoveries were between 65.51% and 92.32% with RSDs lower than 8.95%. Compared with ultrasound-assisted extraction (UAE) and soxhlet extraction, the present method consumed less sample, organic solvent, and extraction time, although the extraction yields obtained by S-SIL-based MSPD are slightly lower than those obtained by UAE. Copyright © 2014 Elsevier B.V. All rights reserved.

Recovery evaluation of organophosphorus pesticides from bee pollen by matrix solid-phase dispersion extraction using sorbents based on silica and titania

International Nuclear Information System (INIS)

Torres-Perea, C; Muñoz-Rodríguez, D; Carrera-Figueiras, C; Medina-Peralta, S; Moguel-Ordóñez, Y B

2013-01-01

This work focused on the evaluation of the recovery of organophosphorus pesticides from bee pollen after matrix solid phase-dispersion extraction (MSPD). Materials based on silica, titania and titania modified with polivylnylimidazole or polyestirene were used as adsorbents for the extraction of pesticides. Small amounts of fortified pollen (0.1 g, at 1 micro-g/g of pesticides), adsorbent (0.4 g) and solvent elution (1 mL de acetonitrile – ACN) were used in the extractions. For recovery evaluation, pollen extracts were analyzed by gas chromatography coupled with mass spectrometry.

Rapid and sensitive determination of major polyphenolic components in Euphoria longana Lam. seeds using matrix solid-phase dispersion extraction and UHPLC with hybrid linear ion trap triple quadrupole mass spectrometry.

Science.gov (United States)

Rathore, Atul S; Sathiyanarayanan, L; Deshpande, Shreekant; Mahadik, Kakasaheb R

2016-11-01

A rapid and sensitive method for the extraction and determination of four major polyphenolic components in Euphoria longana Lam. seeds is presented for the first time based on matrix solid-phase dispersion extraction followed by ultra high performance liquid chromatography with hybrid triple quadrupole linear ion trap mass spectrometry. Matrix solid-phase dispersion method was designed for the extraction of Euphoria longana seed constituents and compared with microwave-assisted extraction and ultrasonic-assisted extraction methods. An Ultra high performance liquid chromatography with hybrid triple quadrupole linear ion-trap mass spectrometry method was developed for quantitative analysis in multiple-reaction monitoring mode in negative electrospray ionization. The chromatographic separation was accomplished using an ACQUITY UPLC BEH C 18 (2.1 mm × 50 mm, 1.7 μm) column with gradient elution of 0.1% aqueous formic acid and 0.1% formic acid in acetonitrile. The developed method was validated with acceptable linearity (r 2 > 0.999), precision (RSD ≤ 2.22%) and recovery (RSD ≤ 2.35%). The results indicated that matrix solid-phase dispersion produced comparable extraction efficiency compared with other methods nevertheless was more convenient and time-saving with reduced requirements on sample and solvent volumes. The proposed method is rapid and sensitive in providing a promising alternative for extraction and comprehensive determination of active components for quality control of Euphoria longana products. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid dispersion application in pharmaceutical technology: Methods of preparation and characterization

OpenAIRE

Medarević, Đorđe; Ibrić, Svetlana; Đuriš, Jelena; Đurić, Zorica

2013-01-01

A growing number of newly synthesized drugs exhibit low aqueous solubility, leading to poor bioavailability. Therefore, improving drug solubility and dissolution rate became one of the greatest challenges during formulation development. Solid dispersions formulation is one of the commonly investigated techniques for improving solubility of poorly soluble drugs. Solid dispersions are dispersions of one or more drugs in an inert carrier (matrix) in the solid state prepared by melting, solvent, ...

Turbulence modification due to bubbles and particles in dispersed two-phase upflows in a vertical pipe

International Nuclear Information System (INIS)

Hosokawa, Shigeo; Tomiyama, Akio

1999-01-01

One of the key issues in two-phase turbulence modeling is the turbulence modification due to the momentum exchange between the dispersed and continuous phases. As for the gas-liquid two-phase flows in vertical pipes, Serizawa and Kataoka carried out detailed measurement of turbulence intensity and detected the turbulence modification. Gore and Crowe pointed out that the modification is well correlated with the ratio of a particle diameter to a turbulence length scale (d/l t ). However the modification may depend on not only the length scales but also the eddy viscosities of shear-induced and particle-induced turbulence. Hosokawa et al. proposed the ratio φ of the eddy viscosity induced by a dispersed phase to the shear-induced eddy viscosity and confirmed that measured turbulence modification was well correlated with φ for a gas-solid two-phase flow. In this study, we examine whether or not φ is also applicable to gas-liquid and solid-liquid two-phase dispersed upflows in vertical pipes. Using the eddy viscosity ratio instead of d/l t , we could obtain much better correlation. The critical point at which no modification occurred was close to φ = 1, irrespective of a type of a two-phase dispersed flow. Consequently, we could confirm that the eddy viscosity ratio is a more appropriate parameter for correlating the turbulent modification than the conventional critical parameter d/l t . (author)

Application of dispersive liquid-liquid microextraction and dispersive micro-solid-phase extraction for the determination of quinolones in swine muscle by high-performance liquid chromatography with diode-array detection

International Nuclear Information System (INIS)

Tsai, Wen-Hsien; Chuang, Hung-Yi; Chen, Ho-Hsien; Huang, Joh-Jong; Chen, Hwi-Chang; Cheng, Shou-Hsun; Huang, Tzou-Chi

2009-01-01

Dispersive liquid-liquid microextraction (DLLME) and dispersive micro-solid-phase extraction (DMSPE) are two simple and low-cost sample preparation methods for liquid samples. In this work, these two methods were applied to solid tissue sample for the determination of seven quinolones by high-performance liquid chromatography with diode-array detection (HPLC-DAD). After the homogenization of the swine muscle with acetonitrile and salt-promoted partitioning, small amounts of the extract were used for the DLLME and DMSPE methods. In the DLLME approach, the target analytes in the extraction solvent were rapidly extracted into a small volume of dichloromethane for drying and the residue was reconstituted for HPLC-DAD analysis. In the DMSPE approach, the target analytes in the extraction solvent were trapped by dispersive silica-based PSA (primary and secondary amine) sorbents and desorbed into a small amount of desorption solution for HPLC-DAD analysis. Under the optimal conditions, relative recoveries were determined for swine muscle spiked 50-200 μg kg -1 and quantification was achieved by matrix-matched calibration. The calibration curves of seven quinolones showed linearity with a correlation coefficient value above 0.998 for both approaches. Relative recoveries ranged from 93.0 to 104.7% and from 95.5 to 111.0% for DLLME and DMSPE, respectively. Limits of detection (LODs) ranged from 5.6 to 23.8 μg kg -1 and from 7.5 to 26.3 μg kg -1 for DLLME and DMSPE, respectively.

Mechanism for enhanced absorption of a solid dispersion formulation of LY2300559 using the artificial stomach duodenum model.

Science.gov (United States)

Polster, Christopher S; Wu, Sy-Juen; Gueorguieva, Ivelina; Sperry, David C

2015-04-06

An artificial stomach duodenum (ASD) model has been used to demonstrate the performance difference between two formulations of LY2300559, a low-solubility acidic developmental drug. The two formulations investigated were a conventional high-shear wet granulation (HSWG) formulation and a solid dispersion formulation. A pharmacokinetic study in humans demonstrated the enhanced performance of the solid dispersion formulation relative to the HSWG formulation. The Cmax and AUC of the solid dispersion was 2.6 and 1.9 times greater, respectively, compared to the HSWG formulation. In the ASD, the solid dispersion formulation performance was characterized by three main phases: (1) rapid release in the stomach, creating a supersaturated concentration of drug, (2) precipitation in the stomach, and (3) rapid redissolution of the precipitate in the duodenum to concentration levels that are supersaturated relative to crystalline drug. A series of complementary experiments were employed to describe this performance behavior mechanistically. Imaging experiments with a pH indicating dye showed that local pH gradients from meglumine in the solid dispersion formulation were responsible for creating a high initial supersaturation concentration in the stomach. Upon dissipation of meglumine, the drug precipitated in the stomach as an amorphous solid. Because the precipitated drug is in an amorphous form, it can then rapidly redissolve as it transits to the more neutral environment of the duodenum. This unexpected sequence of physical state changes gives a mechanistic explanation for the enhanced in vivo performance of the solid dispersion formulation relative to the HSWG formulation.

FORMULATION AND EVALUATION OF MEFENAMIC ACID SOLID DISPERSIONS USING PEG-4000

OpenAIRE

Shaik Jamal Shariff; Shaik Saleem; Alaparthi Naga Pavan Kumar; Bachupally Ajay Kumar; Punuru Madhusudhan

2013-01-01

Mefenamic acid (MA) solid Dispersions were prepared employing methanol as a common solvent using PEG-4000 as a drug carrier with two different techniques namely, melting method and solvent evaporation in varied ratios. The prepared solid dispersions were evaluated and compared with that of pure drug (mefenamic acid) in respect to the dissolution rate and dissolution efficiency. It is noted that solid dispersions of mefenamic acid showed a remarkable increase in dissolution rate and dissolutio...

Determination of selected UV filters in indoor dust by matrix solid-phase dispersion and gas chromatography-tandem mass spectrometry.

Science.gov (United States)

Negreira, N; Rodríguez, I; Rubí, E; Cela, R

2009-07-31

A simple, inexpensive sample preparation procedure, based on the matrix solid-phase dispersion (MSPD) technique, for the determination of six UV filters: 2-ethylhexyl salicylate (EHS), 3,3,5-trimethylcyclohexyl salicylate (Homosalate, HMS), 3-(4-methylbenzylidene) camphor (4-MBC), isoamyl-p-methoxycinnamate (IAMC), 2-ethylhexyl-p-methoxycinnamate (EHMC) and octocrylene (OCR), in dust from indoor environments is presented and the influence of several operational parameters on the extraction performance discussed. Under the final working conditions, sieved samples (0.5 g) were mixed with the same amount of anhydrous sodium sulphate and dispersed with 2 g of octadecyl bonded silica (C18) in a mortar with a pestle. This blend was transferred to a polypropylene solid-phase extraction cartridge containing 2 g of activated silica, as the clean-up co-sorbent. The cartridge was first rinsed with 5 mL of n-hexane and the analytes were then recovered with 4 mL of acetonitrile. This extract was adjusted to 1 mL, filtered and the compounds were determined by gas chromatography combined with tandem mass spectrometry (GC-MS/MS). Recoveries for samples spiked at two different concentrations ranged between 77% and 99%, and the limits of quantification (LOQs) of the method between 10 and 40 ng g(-1). Analysis of settled dust from different indoor areas, including private flats, public buildings and vehicle cabins, showed that EHMC and OCR were ubiquitous in this matrix, with maximum concentrations of 15 and 41 microg g(-1), respectively. Both UV filters were also quantified in dust reference material SRM 2585 for first time. EHS, 4-MBC and IAMC were detected in some of the analyzed samples, although at lower concentrations than EHMC and OCR.

Vortex-Assisted Dispersive Micro-Solid Phase Extraction Using CTAB-Modified Zeolite NaY Sorbent Coupled with HPLC for the Determination of Carbamate Insecticides.

Science.gov (United States)

Salisaeng, Pawina; Arnnok, Prapha; Patdhanagul, Nopbhasinthu; Burakham, Rodjana

2016-03-16

A vortex-assisted dispersive micro-solid phase extraction (VA-D-μ-SPE) based on cetyltrimethylammonium bromide (CTAB)-modified zeolite NaY was developed for preconcentration of carbamate pesticides in fruits, vegetables, and natural surface water prior to analysis by high performance liquid chromatography with photodiode array detection. The small amounts of solid sorbent were dispersed in a sample solution, and extraction occurred by adsorption in a short time, which was accelerated by vortex agitation. Finally, the sorbents were filtered from the solution, and the analytes were subsequently desorbed using an appropriate solvent. Parameters affecting the VA-D-μ-SPE performance including sorbent amount, sample volume, desorption solvent ,and vortex time were optimized. Under the optimum condition, linear dynamic ranges were achieved between 0.004-24.000 mg kg(-1) (R(2) > 0.9946). The limits of detection (LODs) ranged from 0.004-4.000 mg kg(-1). The applicability of the developed procedure was successfully evaluated by the determination of the carbamate residues in fruits (dragon fruit, rambutan, and watermelon), vegetables (cabbage, cauliflower, and cucumber), and natural surface water.

Preconcentration of Trace Neonicotinoid Insecticide Residues Using Vortex-Assisted Dispersive Micro Solid-Phase Extraction with Montmorillonite as an Efficient Sorbent

Directory of Open Access Journals (Sweden)

Khwankaew Moyakao

2018-04-01

Full Text Available In this work, we investigated montmorillonite for adsorption of neonicotinoid insecticides in vortex-assisted dispersive micro-solid phase extraction (VA-d-μ-SPE. High-performance liquid chromatography with photodiode array detection was used for quantification and determination of neonicotinoid insecticide residues, including thiamethoxam, clothianidin, imidacloprid, acetamiprid, and thiacloprid. In this method, the solid sorbent was dispersed into the aqueous sample solution and vortex agitation was performed to accelerate the extraction process. Finally, the solution was filtered from the solid sorbent with a membrane filter. The parameters affecting the extraction efficiency of the proposed method were optimized, such as amount of sorbent, sample volume, salt addition, type and volume of extraction solvent, and vortex time. The adsorbing results show that montmorillonite could be reused at least 4 times and be used as an effective adsorbent for rapid extraction/preconcentration of neonicotinoid insecticide residues. Under optimum conditions, linear dynamic ranges were achieved between 0.5 and 1000 ng mL−1 with a correlation of determination (R2 greater than 0.99. Limit of detection (LOD ranged from 0.005 to 0.065 ng mL−1, while limit of quantification (LOQ ranged from 0.008 to 0.263 ng mL−1. The enrichment factor (EF ranged from 8 to 176-fold. The results demonstrated that the proposed method not only provided a more simple and sensitive method, but also can be used as a powerful alternative method for the simultaneous determination of insecticide residues in natural surface water and fruit juice samples.

Interfacial phase formation of Al-Cu bimetal by solid-liquid casting method

Directory of Open Access Journals (Sweden)

Ying Fu

2017-05-01

Full Text Available The solid-liquid method was used to prepare the continuous casting of copper cladding aluminium by liquid aluminum alloy and solid copper, and the interfacial phase formation of Al-Cu bimetal at different pouring temperatures (700, 750, 800 oC was investigated by means of metallograph, scanning electron microscopy (SEM and energy dispersive spectrometry (EDS methods. The results showed that the pouring temperature of aluminum melt had an important influence on the element diffusion of Cu from the solid Cu to Al alloy melt and the reactions between Al and Cu, as well as the morphology of the Al-Cu interface. When the pouring temperature was 800 oC, there were abundant Al-Cu intermetallic compounds (IMCs near the interface. However, a lower pouring temperature (700 oC resulted in the formation of cavities which was detrimental to the bonding and mechanical properties. Under the conditions in this study, the good metallurgical bonding of Al-Cu was achieved at a pouring temperature of 750 oC.

Microparticles Containing Curcumin Solid Dispersion: Stability, Bioavailability and Anti-Inflammatory Activity.

Science.gov (United States)

Teixeira, C C C; Mendonça, L M; Bergamaschi, M M; Queiroz, R H C; Souza, G E P; Antunes, L M G; Freitas, L A P

2016-04-01

This work aimed at improving the solubility of curcumin by the preparation of spray-dried ternary solid dispersions containing Gelucire®50/13-Aerosil® and quantifying the resulting in vivo oral bioavailability and anti-inflammatory activity. The solid dispersion containing 40% of curcumin was characterised by calorimetry, infrared spectroscopy and X-ray powder diffraction. The solubility and dissolution rate of curcumin in aqueous HCl or phosphate buffer improved up to 3600- and 7.3-fold, respectively. Accelerated stability test demonstrated that the solid dispersion was stable for 9 months. The pharmacokinetic study showed a 5.5-fold increase in curcumin in rat blood plasma when compared to unprocessed curcumin. The solid dispersion also provided enhanced anti-inflammatory activity in rat paw oedema. Finally, the solid dispersion proposed here is a promising way to enhance curcumin bioavailability at an industrial pharmaceutical perspective, since its preparation applies the spray drying, which is an easy to scale up technique. The findings herein stimulate further in vivo evaluations and clinical tests as a cancer and Alzheimer chemoprevention agent.

Investigation of metal-matrix composite containing liquid-phase dispersion

Czech Academy of Sciences Publication Activity Database

Strunz, Pavel; Mukherji, D.; Gilles, R.; Geue, T.; Rösler, J.

2012-01-01

Roč. 340, 012098 (2012), s. 1-15 ISSN 1742-6588. [5th European Conference on Neutron Scattering. Praha, 17.07.2011-21.07.2011] R&D Projects: GA MPO FR-TI1/378 Grant - others:European Commission(XE) RII3-CT-2003-505925 Program:FP6 Institutional support: RVO:61389005 Keywords : metal-matrix composite * liquid-phase dispersion * strengthening * neutron diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism http://iopscience.iop.org/1742-6596/340/1/012098

Determination of ibuprofen enantiomers in breast milk using vortex-assisted matrix solid-phase dispersion and direct chiral liquid chromatography.

Science.gov (United States)

León-González, M E; Rosales-Conrado, N

2017-09-08

A mixture of β-cyclodextrin (β-CD) and primary and secondary amine (PSA) sorbents was employed for the extraction and quantification of ibuprofen enantiomers from human breast milk, combining a vortex-assisted matrix solid-phase dispersion method (MSPD) and direct chiral liquid chromatography (CLC) with ultraviolet detection (UV). The MSPD sample preparation procedure was optimized focusing on both the type and amount of dispersion/sorption sorbents and the nature of the elution solvent, in order to obtain acceptable recoveries and avoiding enantiomer conversion. These MSPD parameters were optimized with the aid of an experimental design approach. Hence, a factorial design was used for identification of the main variables affecting the extraction process of ibuprofen enantiomers. Under optimum selected conditions, MSPD combined with direct CLC-UV was successfully applied for ibuprofen enantiomeric determination in breast milk at enantiomer levels between 0.15 and 6.0μgg -1 . The proposed analytical method also provided good repeatability, with relative standard deviations of 6.4% and 8.3% for the intra-day and inter-day precision, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation of milk samples for immunoassay and liquid chromatographic screening using matrix solid-phase dispersion.

Science.gov (United States)

Barker, S A; Long, A R

1994-01-01

The use of drugs to maintain the health and maximize the output of dairy cattle has made the monitoring of milk for such agents essential. Screening tests based on immunological, microbial inhibition, and bacterial receptor assays have been developed for the detection of violative levels of therapeutic substances. However, such assays are not infallible, and false positive or negative results can occur when contaminants bind receptors or compete for the binding of the target residues. Such effects may arise from dietary sources, diseases, or other variables. Thus, a violation by such a test is not definitive until further confirmation is obtained. Our laboratory has developed extraction procedures for several drugs used in dairy production. Our method uses matrix solid-phase dispersion (MSPD) to isolate drugs away from contaminants and to eliminate many possible interferences. MSPD can also be used to enhance the specificity of such assays by fractionating various classes of drugs that may cross-react. Similarly, such methods may be used for liquid chromatographic screening and confirmation of a suspect sample.

Direct phase selection of initial phases from single-wavelength anomalous dispersion (SAD) for the improvement of electron density and ab initio structure determination

International Nuclear Information System (INIS)

Chen, Chung-De; Huang, Yen-Chieh; Chiang, Hsin-Lin; Hsieh, Yin-Cheng; Guan, Hong-Hsiang; Chuankhayan, Phimonphan; Chen, Chun-Jung

2014-01-01

A novel direct phase-selection method to select optimized phases from the ambiguous phases of a subset of reflections to replace the corresponding initial SAD phases has been developed. With the improved phases, the completeness of built residues of protein molecules is enhanced for efficient structure determination. Optimization of the initial phasing has been a decisive factor in the success of the subsequent electron-density modification, model building and structure determination of biological macromolecules using the single-wavelength anomalous dispersion (SAD) method. Two possible phase solutions (ϕ 1 and ϕ 2 ) generated from two symmetric phase triangles in the Harker construction for the SAD method cause the well known phase ambiguity. A novel direct phase-selection method utilizing the θ DS list as a criterion to select optimized phases ϕ am from ϕ 1 or ϕ 2 of a subset of reflections with a high percentage of correct phases to replace the corresponding initial SAD phases ϕ SAD has been developed. Based on this work, reflections with an angle θ DS in the range 35–145° are selected for an optimized improvement, where θ DS is the angle between the initial phase ϕ SAD and a preliminary density-modification (DM) phase ϕ DM NHL . The results show that utilizing the additional direct phase-selection step prior to simple solvent flattening without phase combination using existing DM programs, such as RESOLVE or DM from CCP4, significantly improves the final phases in terms of increased correlation coefficients of electron-density maps and diminished mean phase errors. With the improved phases and density maps from the direct phase-selection method, the completeness of residues of protein molecules built with main chains and side chains is enhanced for efficient structure determination

Anomalous dispersion enhanced Cerenkov phase-matching

Energy Technology Data Exchange (ETDEWEB)

Kowalczyk, T.C.; Singer, K.D. [Case Western Reserve Univ., Cleveland, OH (United States). Dept. of Physics; Cahill, P.A. [Sandia National Labs., Albuquerque, NM (United States)

1993-11-01

The authors report on a scheme for phase-matching second harmonic generation in polymer waveguides based on the use of anomalous dispersion to optimize Cerenkov phase matching. They have used the theoretical results of Hashizume et al. and Onda and Ito to design an optimum structure for phase-matched conversion. They have found that the use of anomalous dispersion in the design results in a 100-fold enhancement in the calculated conversion efficiency. This technique also overcomes the limitation of anomalous dispersion phase-matching which results from absorption at the second harmonic. Experiments are in progress to demonstrate these results.

On the study of the solid-solid phase transformation of TlBiTe2

International Nuclear Information System (INIS)

Chrissafis, K.; Vinga, E.S.; Paraskevopoulos, K.M.; Polychroniadis, E.K.

2003-01-01

The narrow gap semiconductor TlBiTe 2 undergoes a solid-solid phase transformation from the rhombohedral (D 3d ) to the cubic (O h ) phase. The present paper deals with the study of this phase transformation combining the results of Differential Scanning Calorimetry (DSC) and Transmission Electron Microscopy (TEM). It has been found that during heating the transformation is an athermal activated process, which can be described only by a combination of more than one processes while during cooling it exhibits an expectable thermal hysteresis due to the volume difference. The results of the kinetic analysis combined with the electron microscopy findings, supported also by the Fourier Transform Infrared (FTIR) spectroscopy ones, lead to the conclusion that TlBiTe 2 undergoes a multiple-step, displacive, martensitic type transformation. (Abstract Copyright [2003], Wiley Periodicals, Inc.)

Magnetic dispersive solid-phase extraction based on graphene oxide/Fe3 O4 @polythionine nanocomposite followed by atomic absorption spectrometry for zinc monitoring in water, flour, celery and egg.

Science.gov (United States)

Babaei, Azar; Zeeb, Mohsen; Es-Haghi, Ali

2018-07-01

Magnetic graphene oxide nanocomposite has been proposed as a promising and sustainable sorbent for the extraction and separation of target analytes from food matrices. Sample preparation based on nanocomposite presents several advantages, such as desired efficiency, reasonable selectivity and high surface-area-to-volume ratio. A new graphene oxide/Fe 3 O 4 @polythionine (GO/Fe 3 O 4 @PTh) nanocomposite sorbent was introduced for magnetic dispersive solid-phase extraction and flame atomic absorption spectrometric detection of zinc(II) in water, flour, celery and egg. To fabricate the sorbent, an oxidative polymerization of thionine on the surface of magnetic GO was applied, while polythionine was simply employed as a surface modifier to improve extraction yield. The properties of the sorbent were characterized by transmission electron microscopy, scanning electron microscopy, X-ray diffraction, energy-dispersive X-ray analysis, vibrating sample magnetometry and Fourier transform-infrared spectroscopy. The calibration curve showed linearity in the range of 0.5-30 ng mL -1 . Limits of detection (S/N = 3) and quantification (S/N = 10) were 0.08 and 0.5 ng mL -1 , respectively. The method was applied for trace-level determination of Zn(II) in water and food samples, and its validation was investigated by recovery experiments and analyzing certified reference material. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

A basic insight into the stability and manufacturing aspects of solid dispersions

Directory of Open Access Journals (Sweden)

Jishnu Vijay

2012-01-01

Full Text Available The development of a bioavailable dosage form is the most challenging task for the researchers. In the arena of advanced drug delivery systems, the solid dispersion techniques seem to be a promising system for the development of an optimized, bioavailable formulation of Class 2 drugs. The methods of formulation of solid dispersion have been summarized. This article is an effort to define a solid dispersion and its classification. The prospective of the stability of solid dispersion has also been discussed. Moreover, the major techniques that have been used so far such as the fusion/melting method, solvent evaporation method, hot melt extrusion method, supercritical fluid methods, have also been detailed.

Water-induced phase separation of miconazole-poly (vinylpyrrolidone-co-vinyl acetate) amorphous solid dispersions: Insights with confocal fluorescence microscopy.

Science.gov (United States)

Saboo, Sugandha; Taylor, Lynne S

2017-08-30

The aim of this study was to evaluate the utility of confocal fluorescence microscopy (CFM) to study the water-induced phase separation of miconazole-poly (vinylpyrrolidone-co-vinyl acetate) (mico-PVPVA) amorphous solid dispersions (ASDs), induced during preparation, upon storage at high relative humidity (RH) and during dissolution. Different fluorescent dyes were added to drug-polymer films and the location of the dyes was evaluated using CFM. Orthogonal techniques, in particular atomic force microscopy (AFM) coupled with nanoscale infrared spectroscopy (AFM-nanoIR), were used to provide additional analysis of the drug-polymer blends. The initial miscibility of mico-PVPVA ASDs prepared under low humidity conditions was confirmed by AFM-nanoIR. CFM enabled rapid identification of drug-rich and polymer-rich phases in phase separated films prepared under high humidity conditions. The identity of drug- and polymer-rich domains was confirmed using AFM-nanoIR imaging and localized IR spectroscopy, together with Lorentz contact resonance (LCR) measurements. The CFM technique was then utilized successfully to further investigate phase separation in mico-PVPVA films exposed to high RH storage and to visualize phase separation dynamics following film immersion in buffer. CFM is thus a promising new approach to study the phase behavior of ASDs, utilizing drug and polymer specific dyes to visualize the evolution of heterogeneity in films exposed to water. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of the major constituents in fruit of Arctium lappa L. by matrix solid-phase dispersion extraction coupled with HPLC separation and fluorescence detection.

Science.gov (United States)

Liu, He; Zhang, Yupu; Sun, Yantao; Wang, Xue; Zhai, Yujuan; Sun, Ye; Sun, Shuo; Yu, Aimin; Zhang, Hanqi; Wang, Yinghua

2010-10-15

The arctiin and arctigenin in the fruit of Arctium lappa L. were extracted by matrix solid-phase dispersion (MSPD) and determined by high-performance liquid chromatography (HPLC) with fluorescence detection. The experimental conditions for the MSPD were optimized. Silica gel was selected as dispersion adsorbent and methanol as elution solvent. The calibration curve showed good relationship (r>0.9998) in the concentration range of 0.010-5.0μgmL(-1) for arctiin and 0.025-7.5μgmL(-1) for arctigenin. The recoveries were between 74.4% and 100%. The proposed method consumed less sample, time and solvent compared with conventional methods, including ultrasonic and Soxhlet extraction. Copyright © 2010 Elsevier B.V. All rights reserved.

Modeling solid-fuel dispersal during slow loss-of-flow-type transients

International Nuclear Information System (INIS)

DiMelfi, R.J.; Fenske, G.R.

1981-01-01

The dispersal, under certain accident conditions, of solid particles of fast-reactor fuel is examined in this paper. In particular, we explore the possibility that solid-fuel fragmentation and dispersal can be driven by expanding fission gas, during a slow LOF-type accident. The consequences of fragmentation are studied in terms of the size and speed of dispersed particles, and the overall quantity of fuel moved. (orig.)

Characterization of the molecular distribution of drugs in glassy solid dispersions at the nano-meter scale, using differential scanning calorimetry and gravimetric water vapour sorption techniques.

Science.gov (United States)

van Drooge, D J; Hinrichs, W L J; Visser, M R; Frijlink, H W

2006-03-09

The molecular distribution in fully amorphous solid dispersions consisting of poly(vinylpyrrolidone) (PVP)-diazepam and inulin-diazepam was studied. One glass transition temperature (T(g)), as determined by temperature modulated differential scanning calorimetry (TMDSC), was observed in PVP-diazepam solid dispersions prepared by fusion for all drug loads tested (10-80 wt.%). The T(g) of these solid dispersions gradually changed with composition and decreased from 177 degrees C for pure PVP to 46 degrees C for diazepam. These observations indicate that diazepam was dispersed in PVP on a molecular level. However, in PVP-diazepam solid dispersions prepared by freeze drying, two T(g)'s were observed for drug loads above 35 wt.% indicating phase separation. One T(g) indicated the presence of amorphous diazepam clusters, the other T(g) was attributed to a PVP-rich phase in which diazepam was dispersed on a molecular level. With both the value of the latter T(g) and the DeltaC(p) of the diazepam glass transition the concentrations of molecular dispersed diazepam could be calculated (27-35 wt.%). Both methods gave similar results. Water vapour sorption (DVS) experiments revealed that the PVP-matrix was hydrophobised by the incorporated diazepam. TMDSC and DVS results were used to estimate the size of diazepam clusters in freeze dried PVP-diazepam solid dispersions, which appeared to be in the nano-meter range. The inulin-diazepam solid dispersions prepared by spray freeze drying showed one T(g) for drug loads up to 35 wt.% indicating homogeneous distribution on a molecular level. However, this T(g) was independent of the drug load, which is unexpected because diazepam has a lower T(g) than inulin (46 and 155 degrees C, respectively). For higher drug loads, a T(g) of diazepam as well as a T(g) of the inulin-rich phase was observed, indicating the formation of amorphous diazepam clusters. From the DeltaC(p) of the diazepam glass transition the amount of molecularly dispersed

Speciation analysis of aqueous nanoparticulate diclofenac complexes by solid-phase microextraction

NARCIS (Netherlands)

Zielinska, K.; Leeuwen, van H.P.; Thibault, S.; Town, R.M.

2012-01-01

The dynamic sorption of an organic compound by nanoparticles (NPs) is analyzed by solid-phase microextraction (SPME) for the example case of the pharmaceutical diclofenac in dispersions of impermeable (silica, SiO(2)) and permeable (bovine serum albumin, BSA) NPs. It is shown that only the

Electron-beam-irradiation-induced crystallization of amorphous solid phase change materials

Science.gov (United States)

Zhou, Dong; Wu, Liangcai; Wen, Lin; Ma, Liya; Zhang, Xingyao; Li, Yudong; Guo, Qi; Song, Zhitang

2018-04-01

The electron-beam-irradiation-induced crystallization of phase change materials in a nano sized area was studied by in situ transmission electron microscopy and selected area electron diffraction. Amorphous phase change materials changed to a polycrystalline state after being irradiated with a 200 kV electron beam for a long time. The results indicate that the crystallization temperature strongly depends on the difference in the heteronuclear bond enthalpy of the phase change materials. The selected area electron diffraction patterns reveal that Ge2Sb2Te5 is a nucleation-dominated material, when Si2Sb2Te3 and Ti0.5Sb2Te3 are growth-dominated materials.

Three-dimensional ionic liquid functionalized magnetic graphene oxide nanocomposite for the magnetic dispersive solid phase extraction of 16 polycyclic aromatic hydrocarbons in vegetable oils.

Science.gov (United States)

Zhang, Yun; Zhou, Hua; Zhang, Zhe-Hua; Wu, Xiang-Lun; Chen, Wei-Guo; Zhu, Yan; Fang, Chun-Fu; Zhao, Yong-Gang

2017-03-17

In this paper, a novel three-dimensional ionic liquid functionalized magnetic graphene oxide nanocomposite (3D-IL@mGO) was prepared, and used as an effective adsorbent for the magnetic dispersive solid phase extraction (MSPE) of 16 polycyclic aromatic hydrocarbons (PAHs) in vegetable oil prior to gas chromatography-mass spectrometry (GC-MS). The properties of 3D-IL@mGO were characterized by scanning electron micrographs (SEM), X-ray photoelectron spectroscopy (XPS), vibrating sample magnetometer (VSM). The 3D-IL@mGO, functionalized by ionic liquid, exhibited high adsorption toward PAHs. Compared to molecularly imprinted solid phase extraction (MISPE), the MSPE method based on 3D-IL@mGO had less solvent consumption and low cost, and was more efficent to light PAHs in quantitative analysis. Furthermore, the rapid and accurate GC-MS method coupled with 3D-IL@mGO MSPE procedure was successfully applied for the analysis of 16 PAHs in eleven vegetable oil samples from supermarket in Zhejiang Province. The results showed that the concentrations of BaP in 3 out of 11 samples were higher than the legal limit (2.0μg/kg, Commission Regulation 835/2011a), the sum of 8 heavy PAHs (BaA, CHR, BbF, BkF, BaP, IcP, DaA, BgP) in 11 samples was between 3.03μg/kg and 229.5μg/kg. Validation results on linearity, specificity, accuracy, precision and stability, as well as on application to the analysis of PAHs in oil samples demonstrated the applicability to food safety risk monitoring in China. Copyright © 2017 Elsevier B.V. All rights reserved.

A REVIEW ON SOLID DISPERSION: A DISSOLUTION ENHANCEMENT TECHNIQUE

OpenAIRE

Ingle U.S.; Gaikwad P.D.; Bankar V.H.; Pawar S.P.

2011-01-01

The enhancement of the oral bioavailability is currently one of the greatest challenges in the development of poorly water soluble drugs. To increase the dissolution and hence the bioavaibility it is important to increase the solubility of the poorly water soluble drugs. One of the possible ways to overcome this limitation is the use of solid dispersion technology. This article contains the different methods and mechanism used in the solid dispersion technology also overlooks the various carr...

Carbon-free Solid Dispersion LiCoO2 Redox Couple Characterization and Electrochemical Evaluation for All Solid Dispersion Redox Flow Batteries

International Nuclear Information System (INIS)

Qi, Zhaoxiang; Liu, Aaron L.; Koenig, Gary M.

2017-01-01

Highlights: • LiCoO 2 particles can be cycled in carbon-free and binder-free coin cells. • A carbon-free LiCoO 2 suspension is electrochemically oxidized and reduced. • Comparable size LiCoO 2 and Li 4 Ti 5 O 12 suspensions have similar rheological properties. • First demonstration of redox couples with solid suspensions for both electrodes. - Abstract: Semi-solid flow batteries have been reported to have among the highest energy densities for redox flow batteries, however, they rely on percolated carbon networks which increase the electrolyte viscosity significantly. We report the first demonstration of carbon-free redox flow couples comprised of dispersed lithium-ion battery active material suspensions, with sub-micrometer LiCoO 2 (LCO) particles at the cathode and Li 4 Ti 5 O 12 (LTO) particles at the anode. Both electrochemical and rheological properties of the LCO suspensions are reported and compared to previous reports for LTO dispersed electrochemical redox couples. An LTO anode and LCO cathode full cell was constructed and reversible electrochemical redox reaction of the dispersed particles was successfully demonstrated. This carbon-free dispersed lithium-ion active material full cell provides a proof-of-concept for a system that lies between the relatively high viscosity semi-solid flow cells with percolated carbon networks and the relatively low energy density conventional flow cells comprised of dissolved transition metals, providing a system for future study of the trade-off between energy density and viscosity for electrochemical flow cells that rely on solid active materials.

Dispersion of a layered electron gas with nearest neighbour-tunneling

International Nuclear Information System (INIS)

Miesenboeck, H.M.

1988-09-01

The dispersion of the first plasmon band is calculated within the Random Phase Approximation for a superlattice of two-dimensional electron-gases, mutually interacting, and with nearest neighbour hopping between the planes. It is further shown that the deviations of this dispersion from the one in systems with zero interplane motion are very small in commonly realized experimental situations and that they are expected to be observable only in samples with plane distances of 100A and less. (author). 15 refs, 3 figs, 1 tab

Numerical predictions of particle dispersed two-phase flows, using the LSD and SSF models

International Nuclear Information System (INIS)

Avila, R.; Cervantes de Gortari, J.; Universidad Nacional Autonoma de Mexico, Mexico City. Facultad de Ingenieria)

1988-01-01

A modified version of a numerical scheme which is suitable to predict parabolic dispersed two-phase flow, is presented. The original version of this scheme was used to predict the test cases discussed during the 3rd workshop on TPF predictions in Belgrade, 1986. In this paper, two particle dispersion models are included which use the Lagrangian approach predicting test case 1 and 3 of the 4th workshop. For the prediction of test case 1 the Lagrangian Stochastic Deterministic model (LSD) is used providing acceptable good results of mean and turbulent quantities for both solid and gas phases; however, the computed void fraction distribution is not in agreement with the measurements at locations away from the inlet, especially near the walls. Test case 3 is predicted using both the LSD and the Stochastic Separated Flow (SSF) models. It was found that the effects of turbulence modulation are large when the LSD model is used, whereas the particles have a negligible influence on the continuous phase if the SSF model is utilized for the computations. Predictions of gas phase properties based on both models agree well with measurements; however, the agreement between calculated and measured solid phase properties is less satisfactory. (orig.)

Dispersed-phase catalysis in coal liquefaction

International Nuclear Information System (INIS)

Utz, B.R.; Cugini, A.V.; Frommell, E.A.

1990-01-01

This paper reports that the specific reaction (activation) conditions for the conversion of catalyst precursors to unsupported catalyst have a direct effect on the catalytic activity and dispersion. The importance of reaction intermediates in decomposition of ammonium heptamolybdate and ammonium tetrathiomolybdate, and the sensitivity of these intermediates to reaction conditions, were studied in coal liquefaction systems. Recent results indicate that optimization of activation conditions facilitates the formation of a highly dispersed and active form of molybdenum disulfide for coal liquefaction. The use of the catalyst precursors ammonium heptamolybdate, ammonium tetrathiomolybdate, and molybdenum trisulfide for the conversion of coal to soluble products will be discussed. The use of an unsupported dispersed-phase catalyst for direct coal liquefaction is not a novel concept and has been employed in may studies with varying success. Dispersed-phase catalysts soluble and oil-soluble salts, and as finely divided powders. While some methods of catalyst introduction give higher dispersion of the catalyst and greater activity for the liquefaction of coal, all of the techniques allow the formation of a finely dispersed inorganic phase

Matrix solid-phase dispersion followed by gas chromatography tandem mass spectrometry for the determination of benzotriazole UV absorbers in sediments.

Science.gov (United States)

Carpinteiro, I; Abuín, B; Ramil, M; Rodríguez, I; Cela, R

2012-01-01

A cost-effective and low solvent consumption method, based on the matrix solid-phase dispersion (MSPD) technique, for the determination of six benzotriazole UV absorbers in sediments is presented. Sieved samples (0.5 g) were first mixed in a mortar with a solid sorbent and then transferred to a polypropylene syringe containing a layer of clean-up co-sorbent. Analytes were eluted with a suitable solvent and further determined by gas chromatography with tandem mass spectrometry (GC-MS/MS). Under final conditions, diatomaceous earth and silica, deactivated to 10%, were used as inert dispersant and clean-up co-sorbent, respectively. Analytes were recovered using just 5 mL of dichloromethane, and this extract was concentrated and exchanged to 1 mL of isooctane. Further removal of co-extracted sulphur was achieved adding activated copper powder to final extracts, which were stored overnight, before injection in the GC-MS/MS system. The accuracy of the method was assessed with river and marine sediment samples showing different carbon contents and spiked at different concentrations in the range from 40 to 500 ng g(-1). Recoveries varied between 78% and 110% with associated standard deviations below 14%. The limits of quantification of the method stayed between 3 and 15 ng g(-1). Levels of target compounds in sediment samples ranged from not detected up to a maximum of 56 ng g(-1) for Tinuvin 328.

Dependence of charge transfer phenomena during solid-air two-phase flow on particle disperser

Science.gov (United States)

Tanoue, Ken-ichiro; Suedomi, Yuuki; Honda, Hirotaka; Furutani, Satoshi; Nishimura, Tatsuo; Masuda, Hiroaki

2012-12-01

An experimental investigation of the tribo-electrification of particles has been conducted during solid-air two-phase turbulent flow. The current induced in a metal plate by the impact of polymethylmethacrylate (PMMA) particles in a high-speed air flow was measured for two different plate materials. The results indicated that the contact potential difference between the particles and a stainless steel plate was positive, while for a nickel plate it was negative. These results agreed with theoretical contact charge transfer even if not only the particle size but also the kind of metal plate was changed. The specific charge of the PMMA particles during solid-air two-phase flow using an ejector, a stainless steel branch pipe, and a stainless steel straight pipe was measured using a Faraday cage. Although the charge was negative in the ejector, the particles had a positive specific charge at the outlet of the branch pipe, and this positive charge increased in the straight pipe. The charge decay along the flow direction could be reproduced by the charging and relaxation theory. However, the proportional coefficients in the theory changed with the particle size and air velocity. Therefore, an unexpected charge transfer occurred between the ejector and the branch pipe, which could not be explained solely by the contact potential difference. In the ejector, an electrical current in air might have been produced by self-discharge of particles with excess charge between the nickel diffuser in the ejector and the stainless steel nozzle or the stainless steel pipe due to a reversal in the contact potential difference between the PMMA and the stainless steel. The sign of the current depended on the particle size, possibly because the position where the particles impacted depended on their size. When dual coaxial glass pipes were used as a particle disperser, the specific charge of the PMMA particles became more positive along the particle flow direction due to the contact

Physicochemical characterization and dissolution enhancement of loratadine by solid dispersion technique

International Nuclear Information System (INIS)

Bandari, Suresh; Jadav, Subash; Eedara, Basanth Babu; Jukanti, Raju; Veerareddy, Prabhakar Reddy

2013-01-01

The purpose of this investigation was to enhance the dissolution rate of loratadine using polyethylene glycol 6000 (PEG) solid dispersions (SDs). The solubility behavior of loratadine in the presence of polyethylene glycol 4000 and polyethylene glycol 6000 in water showed linear increase with increasing concentrations of PEG, indicating A L type solubility diagrams. SDs of loratadine with PEG 6000 were prepared at 1 : 1, 1 : 3, 1 : 5, 1 : 7 and 1 : 9 ratios by the solvent evaporation method. Solid dispersions were characterized for drug content, dissolution behavior and for physicochemical characteristics. The dissolution rate of loratadine was enhanced rapidly with increasing concentrations of PEG 6000 in SDs. Fourier transform infrared (FTIR) studies showed the stability of loratadine and the absence of a well-defined loratadine - PEG 6000 interaction. Differential scanning calorimetry (DSC) and X-ray powder diffractometry (XRD) studies revealed the amorphous state of loratadine in SDs of loratadine with PEG 6000 which was further confirmed from scanning electron microscopy (SEM) studies. The flow properties of the blend, physical characteristics and disintegration time of the tablets formulated indicated that PEG 6000 SD can be used to formulate fast release loratadine tablets

Physicochemical characterization and dissolution enhancement of loratadine by solid dispersion technique

Energy Technology Data Exchange (ETDEWEB)

Bandari, Suresh; Jadav, Subash; Eedara, Basanth Babu; Jukanti, Raju; Veerareddy, Prabhakar Reddy [St. Peter’s Institute of Pharmaceutical Sciences, Warangal (India)

2013-01-15

The purpose of this investigation was to enhance the dissolution rate of loratadine using polyethylene glycol 6000 (PEG) solid dispersions (SDs). The solubility behavior of loratadine in the presence of polyethylene glycol 4000 and polyethylene glycol 6000 in water showed linear increase with increasing concentrations of PEG, indicating A{sub L} type solubility diagrams. SDs of loratadine with PEG 6000 were prepared at 1 : 1, 1 : 3, 1 : 5, 1 : 7 and 1 : 9 ratios by the solvent evaporation method. Solid dispersions were characterized for drug content, dissolution behavior and for physicochemical characteristics. The dissolution rate of loratadine was enhanced rapidly with increasing concentrations of PEG 6000 in SDs. Fourier transform infrared (FTIR) studies showed the stability of loratadine and the absence of a well-defined loratadine - PEG 6000 interaction. Differential scanning calorimetry (DSC) and X-ray powder diffractometry (XRD) studies revealed the amorphous state of loratadine in SDs of loratadine with PEG 6000 which was further confirmed from scanning electron microscopy (SEM) studies. The flow properties of the blend, physical characteristics and disintegration time of the tablets formulated indicated that PEG 6000 SD can be used to formulate fast release loratadine tablets.

Enhancement of dissolution of Telmisartan through use of solid dispersion technique surface solid dispersion

Directory of Open Access Journals (Sweden)

Bhumika Patel

2012-01-01

Full Text Available The present study was aimed to increase the solubility of the poorly water soluble drug Telmisartan by using Surface solid dispersion (SSD made of polymers like Poloxamer 407, PEG 6000 by Solvent evaporation method. The drug was solubilized by surfactants and/or polymers then adsorbed onto the surface of extremely fine carriers to increase its surface area and to form the SSD which give the more Surface area for absorption of the drug. A 2 2 full factorial design was used to investigate for each carrier the joint influence of formulation variables: Amount of carrier and adsorbent. Saturation solubility studies shows the improvement in solubility of drug batch SSD 8 give more solubility improvement than the other batch, in-vitro dissolution of pure drug, physical mixtures and SSDs were carried out in that SSDs were found to be effective in increasing the dissolution rate of Telmisartan in form of SSD when compared to pure drug. Also FT-IR spectroscopy, differential scanning calorimetry and X-ray diffractometry studies were carried out in order to characterize the drug and Surface solid dispersion. Furthermore, both DSC and X-ray diffraction showed a decrease in the melting enthalpy and reduced drug crystallinity consequently in SSDs. However, infrared spectroscopy revealed no drug interactions with the carriers.

Electron Holography: phases matter.

Science.gov (United States)

Lichte, Hannes

2013-06-01

Essentially, all optics is wave optics, be it with light, X-rays, neutrons or electrons. The information transfer from the object to the image can only be understood in terms of waves given by amplitude and phase. However, phases are difficult to measure: for slowly oscillating waves such as sound or low-frequency electromagnetic waves, phases can be measured directly; for high frequencies this has to be done by heterodyne detection, i.e. superposition with a reference and averaging over time. In optics, this is called interferometry. Because interference is mostly very difficult to achieve, phases have often been considered 'hidden variables' seemingly pulling the strings from backstage, only visible by their action on the image intensity. This was almost the case in conventional Electron Microscopy with the phase differences introduced by an object. However, in the face of the urgent questions from solid state physics and materials science, these phases have to be determined precisely, because they encode the most dominant object properties, such as charge distributions and electromagnetic fields. After more than six decades of very patient advancement, electron interferometry and holography offer unprecedented analytical facilities down to an atomic scale. Akira Tonomura has prominently contributed to the present state.

Membranes as separators of dispersed emulsion phases

OpenAIRE

Lefferts, A.G.

1997-01-01

The reuse or discharge of industrial waste waters, containing small fractions of dispersed oil, requires a purification treatment for which membranes can be used. If only little oil is present, removal of the dispersed phase might be preferable to the more commonly applied removal of the continuous phase. For this purpose dispersed phase separators can be applied, which combine the features of conventional coalescers and membrane filtration. The membrane surface promotes coalescence ...

The electronic structures of solids

CERN Document Server

Coles, B R

2013-01-01

The Electronic Structures of Solids aims to provide students of solid state physics with the essential concepts they will need in considering properties of solids that depend on their electronic structures and idea of the electronic character of particular materials and groups of materials. The book first discusses the electronic structure of atoms, including hydrogen atom and many-electron atom. The text also underscores bonding between atoms and electrons in metals. Discussions focus on bonding energies and structures in the solid elements, eigenstates of free-electron gas, and electrical co

A novel and alternative approach to controlled release drug delivery system based on solid dispersion technique

Directory of Open Access Journals (Sweden)

Tapan Kumar Giri

2012-12-01

Full Text Available The solid dispersion method was originally used to improve the dissolution properties and the bioavailability of poorly water soluble drugs by dispersing them into water soluble carriers. In addition to the above, dissolution retardation through solid dispersion technique using water insoluble and water swellable polymer for the development of controlled release dosage forms has become a field of interest in recent years. Development of controlled release solid dispersion has a great advantage for bypassing the risk of a burst release of drug; since the structure of the solid dispersion is monolithic where drug molecules homogeneously disperse. Despite the remarkable potential and extensive research being conducted on controlled release solid dispersion system, commercialization and large scale production are limited. The author expects that recent technological advances may overcome the existing limitations and facilitate the commercial utilization of the techniques for manufacture of controlled release solid dispersions. This article begins with an overview of the different carriers being used for the preparation of controlled release solid dispersion and also different techniques being used for the purpose. Kinetics of drug release from these controlled release solid dispersions and the relevant mathematical modeling have also been reviewed in this manuscript.

Solid-state, triboelectrostatic and dissolution characteristics of spray-dried piroxicam-glucosamine solid dispersions.

Science.gov (United States)

Adebisi, Adeola O; Kaialy, Waseem; Hussain, Tariq; Al-Hamidi, Hiba; Nokhodchi, Ali; Conway, Barbara R; Asare-Addo, Kofi

2016-10-01

This work explores the use of both spray drying and d-glucosamine HCl (GLU) as a hydrophilic carrier to improve the dissolution rate of piroxicam (PXM) whilst investigating the electrostatic charges associated with the spray drying process. Spray dried PXM:GLU solid dispersions were prepared and characterised (XRPD, DSC, SEM). Dissolution and triboelectric charging were also conducted. The results showed that the spray dried PXM alone, without GLU produced some PXM form II (DSC results) with no enhancement in solubility relative to that of the parent PXM. XRPD results also showed the spray drying process to decrease the crystallinity of GLU and solid dispersions produced. The presence of GLU improved the dissolution rate of PXM. Spray dried PXM: GLU at a ratio of 2:1 had the most improved dissolution. The spray drying process generally yielded PXM-GLU spherical particles of around 2.5μm which may have contributed to the improved dissolution. PXM showed a higher tendency for charging in comparison to the carrier GLU (-3.8 versus 0.5nC/g for untreated material and -7.5 versus 3.1nC/g for spray dried materials). Spray dried PXM and spray dried GLU demonstrated higher charge densities than untreated PXM and untreated GLU, respectively. Regardless of PXM:GLU ratio, all spray dried PXM:GLU solid dispersions showed a negligible charge density (net-CMR: 0.1-0.3nC/g). Spray drying of PXM:GLU solid dispersions can be used to produce formulation powders with practically no charge and thereby improving handling as well as dissolution behaviour of PXM. Copyright © 2016 Elsevier B.V. All rights reserved.

The influence of second-phase dispersion on environmental embrittlement of Ni3(Si,Ti) alloys

International Nuclear Information System (INIS)

Takasugi, T.; Hanada, S.

1999-01-01

Some quaternary Ni 3 (Si,Ti) alloyed with transition elements V, Nb, Zr and Hf was prepared beyond their maximum solubility limits to investigate the effect of second-phase dispersion on moisture-induced embrittlement. V-added Ni 3 (Si,Ti) alloy contained ductile fcc-type Ni solid solution as the second-phase, while Nb-, Zr- and Hf-added Ni 3 (Si,Ti) alloys contained hard dispersion compounds as the second-phase. V- and Nb-added Ni 3 (Si,Ti) alloys did not display reduced tensile elongation in air, indicating that their second phases have the effect of suppressing the moisture-induced embrittlement. Possible mechanisms for the beneficial effect by the second phase on the moisture-induced embrittlement of V- and Nb-added Ni 3 (Si,Ti) alloys are discussed in association with hydrogen behavior and deformation property in the constituent phases or at matrix/second-phase interface

Three phase carbon EOS model with electronic excitation

International Nuclear Information System (INIS)

van Thiel, M.; Ree, F.H.; Grover, R.

1987-07-01

A simple and rapid way for computing EOS data of multiphase solids with a liquid phase is described with emphasis on carbon. The method uses a scaling model for the liquid phase and includes a provision for electronic effects. The free energy minimum determines the stable phase

Dispersive solid phase microextraction with magnetic graphene oxide as the sorbent for separation and preconcentration of ultra-trace amounts of gold ions.

Science.gov (United States)

Kazemi, Elahe; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad

2015-08-15

A selective, simple and rapid dispersive solid phase microextraction was developed using magnetic graphene oxide (MGO) as an efficient sorbent for the separation and preconcentration of gold ions. The MGO was synthesized by means of the simple one step chemical coprecipitation method, characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). Gold ions retained by the sorbent were eluted using 0.5mol L(-)(1) thiourea in 0.1mol L(-1) HCl solution and determined by the flow injection flame atomic absorption spectrometry (FI-FAAS). The factors affecting the separation and preconcentration of gold were investigated and optimized. Under the optimized conditions, the method exhibited a linear dynamic range of 0.02-100.0µg L(-)(1) with a detection limit of 4ng L(-1) and an enrichment factor of 500. The relative standard deviations of 3.2% and 4.7% (n=6) were obtained at 20µg L(-1) level of gold ions for the intra and the inter day analysis, respectively. The method was successfully applied to the determination of gold ions in water and waste water samples as well as a certified reference material (CCU-1b, copper flotation concentrate). Copyright © 2015 Elsevier B.V. All rights reserved.

Development and characterization of an atorvastatin solid dispersion formulation using skimmed milk for improved oral bioavailability

Directory of Open Access Journals (Sweden)

Ankush Choudhary

2012-08-01

Full Text Available Atorvastatin has low aqueous solubility resulting in low oral bioavailability (12% and thus presents a challenge in formulating a suitable dosage form. To improve the aqueous solubility, a solid dispersion formulation of atorvastatin was prepared by lyophilization utilising skimmed milk as a carrier. Six different formulations were prepared with varying ratios of drug and carrier and the corresponding physical mixtures were also prepared. The formation of a solid dispersion formulation was confirmed by differential scanning calorimetry and X-ray diffraction studies. The optimum drug-to-carrier ratio of 1:9 enhanced solubility nearly 33-fold as compared to pure drug. In vitro drug release studies exhibited a cumulative release of 83.69% as compared to 22.7% for the pure drug. Additionally, scanning electron microscopy studies suggested the conversion of crystalline atorvastatin to an amorphous form. In a Triton-induced hyperlipidemia model, a 3-fold increase in the lipid lowering potential was obtained with the reformulated drug as compared to pure drug. These results suggest that solid dispersion of atorvastatin using skimmed milk as carrier is a promising approach for oral delivery of atorvastatin.

Simultaneous determination and qualitative analysis of six types of components in Naoxintong capsule by miniaturized matrix solid-phase dispersion extraction coupled with ultra high-performance liquid chromatography with photodiode array detection and quadrupole time-of-flight mass spectrometry.

Science.gov (United States)

Wang, Huilin; Jiang, Yan; Ding, Mingya; Li, Jin; Hao, Jia; He, Jun; Wang, Hui; Gao, Xiu-Mei; Chang, Yan-Xu

2018-02-03

A simple and effective sample preparation process based on miniaturized matrix solid-phase dispersion was developed for simultaneous determination of phenolic acids (gallic acid, chlorogenic acid, ferulic acid, 3,5-dicaffeoylqunic acid, 1,5-dicaffeoylqunic acid, rosmarinic acid, lithospermic acid, and salvianolic acid B), flavonoids (kaempferol-3-O-rutinoside, calycosin, and formononetin), lactones (ligustilide and butyllidephthalide), monoterpenoids (paeoniflorin), phenanthraquinones (cryptotanshinone), and furans (5-hydroxymethylfurfural) in Naoxintong capsule by ultra high-performance liquid chromatography. The optimized condition was that 25 mg Naoxintong powder was blended homogeneously with 100 mg Florisil PR for 4 min. One milliliter of methanol/water (75:25, v/v) acidified by 0.05% formic acid was selected to elute all components. It was found that the recoveries of the six types of components ranged from 61.36 to 96.94%. The proposed miniaturized matrix solid-phase dispersion coupled with ultra high-performance liquid chromatography was successfully applied to simultaneous determination of the six types of components in Naoxintong capsules. The results demonstrated that the proposed miniaturized matrix solid-phase dispersion coupled with ultra high-performance liquid chromatography could be used as an environmentally friendly tool for the extraction and determination of multiple bioactive components in natural products. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation of amorphous solid dispersions by rotary evaporation and KinetiSol Dispersing: approaches to enhance solubility of a poorly water-soluble gum extract.

Science.gov (United States)

Bennett, Ryan C; Brough, Chris; Miller, Dave A; O'Donnell, Kevin P; Keen, Justin M; Hughey, Justin R; Williams, Robert O; McGinity, James W

2015-03-01

Acetyl-11-keto-β-boswellic acid (AKBA), a gum resin extract, possesses poor water-solubility that limits bioavailability and a high melting point making it difficult to successfully process into solid dispersions by fusion methods. The purpose of this study was to investigate solvent and thermal processing techniques for the preparation of amorphous solid dispersions (ASDs) exhibiting enhanced solubility, dissolution rates and bioavailability. Solid dispersions were successfully produced by rotary evaporation (RE) and KinetiSol® Dispersing (KSD). Solid state and chemical characterization revealed that ASD with good potency and purity were produced by both RE and KSD. Results of the RE studies demonstrated that AQOAT®-LF, AQOAT®-MF, Eudragit® L100-55 and Soluplus with the incorporation of dioctyl sulfosuccinate sodium provided substantial solubility enhancement. Non-sink dissolution analysis showed enhanced dissolution properties for KSD-processed solid dispersions in comparison to RE-processed solid dispersions. Variances in release performance were identified when different particle size fractions of KSD samples were analyzed. Selected RE samples varying in particle surface morphologies were placed under storage and exhibited crystalline growth following solid-state stability analysis at 12 months in comparison to stored KSD samples confirming amorphous instability for RE products. In vivo analysis of KSD-processed solid dispersions revealed significantly enhanced AKBA absorption in comparison to the neat, active substance.

Pharmaceutical development of an oral tablet formulation containing a spray dried amorphous solid dispersion of docetaxel or paclitaxel

NARCIS (Netherlands)

Sawicki, Emilia; Beijnen, Jos H|info:eu-repo/dai/nl/071919570; Schellens, Jan H M|info:eu-repo/dai/nl/073926272; Nuijen, Bastiaan

2016-01-01

Previously, it was shown in Phase I clinical trials that solubility-limited oral absorption of docetaxel and paclitaxel can be drastically improved with a freeze dried solid dispersion (fdSD). These formulations, however, are unfavorable for further clinical research because of limitations in

Graphene Inks with Cellulosic Dispersants: Development and Applications for Printed Electronics

Science.gov (United States)

Secor, Ethan Benjamin

Graphene offers promising opportunities for applications in printed and flexible electronic devices due to its high electrical and thermal conductivity, mechanical flexibility and strength, and chemical and environmental stability. However, scalable production and processing of graphene presents a critical technological challenge preventing the application of graphene for flexible electronic interconnects, electrochemical energy storage, and chemically robust electrical contacts. In this thesis, a promising and versatile platform for the production, patterning, and application of graphene inks is presented based on cellulosic dispersants. Graphene is produced from flake graphite using scalable liquid-phase exfoliation methods, using the polymers ethyl cellulose and nitrocellulose as multifunctional dispersing agents. These cellulose derivatives offer high colloidal stability and broadly tunable rheology for graphene dispersions, providing an effective and tunable platform for graphene ink development. Thermal or photonic annealing decomposes the polymer dispersant to yield high conductivity, flexible graphene patterns for various electronics applications. In particular, the chemical stability of graphene enables robust electrical contacts for ceramic, metallic, organic and electrolytic materials, validating the diverse applicability of graphene in printed electronics. Overall, the strategy for graphene ink design presented here offers a simple, efficient, and versatile method for integrating graphene in a wide range of printed devices and systems, providing both fundamental insight for nanomaterial ink development and realistic opportunities for practical applications.

Solubility Enhancement and Formulation of Mouth Dissolving Tablet of Clonazepam with Solid Dispersion Technology

Directory of Open Access Journals (Sweden)

Swati C. Jagdale

2012-01-01

Full Text Available Clonazepam (CLZ is an anticonvulsant benzodiazepine widely used in the treatment of epilepsy. CLZ is a BCS Class II drug and its bioavailability is thus dissolution limited. The objective of the present study was to prepare solid dispersions (SDs of CLZ by various techniques, using the amphiphilic carrier Gelucire 50/13 in various proportions, to increase its water solubility. Drug-polymer interactions were investigated by Fourier-transform infrared (FTIR and UltraViolet (UV spectroscopy. The SDs were characterized physically by differential scanning calorimetry (DSC and X-ray diffraction (XRD. A phase solubility study was performed and the stability constant (Ks was found to be 275.27, while the negative Gibbs free energy (ΔGo tr indicated spontaneous solubilization of the drug. The dissolution study showed that the SDs considerably enhanced the dissolution rate of the drug. The FTIR and UV spectra revealed no chemical incompatibility between the drug and Gelucire 50/13. XRD patterns and the DSC profiles indicated the CLZ was in the amorphous form, which explains the improved dissolution rate of the drug from its SDs. Finally, mouth dissolving tablets (MDTs were prepared from the optimized batches (kneading method of solid dispersion, using crospovidone and Doshion P544 resin as superdisintegrants. The tablets were characterized by in-vitro disintegration and dissolution tests. The study of the MDTs showed disintegration times in the range 32.0±0.85 to 20.0±1.30 sec and dissolution was faster than for the commercial preparation. In conclusion, this investigation demonstrated the potential of solid dispersions of a drug with Gelucire 50/13 for promoting the dissolution of the drug and contributed to the understanding of the effect of a superdisintegrant on mouth dissolving tablets containing a solid dispersion of a hydrophobic drug.

Solid Phases Precipitating in Artificial Urine in the Absence and Presence of Bacteria Proteus mirabilis—A Contribution to the Understanding of Infectious Urinary Stone Formation

Directory of Open Access Journals (Sweden)

Jolanta Prywer

2018-04-01

Full Text Available Magnesium ammonium phosphate hexahydrate, called struvite, is the dominant component of infectious urinary stones. In addition to struvite, infectious urinary stones include solid phases with poor crystallinity as well as amorphous matter. This article is devoted to the analysis of these solid phases, because they have not been characterized well until now. The solid phases tested were obtained from artificial urine in the absence and presence of Proteus mirabilis. The solid phases were characterized by different techniques (X-ray Diffraction, Energy Dispersive X-ray, Scanning Electron Microscopy, as well as Raman and Infrared Spectroscopies. According to the results these phases are carbonate apatite (CA, hydroxylapatite (HAP, amorphous calcium carbonate (ACC, amorphous calcium phosphate (ACP and/or amorphous carbonated calcium phosphate (ACCP. Carbonate apatite and hydroxylapatite may occur in non-stoichiometric forms, i.e., various anions can be substituted for CO32−, OH−, and PO43− groups in them. The non-stoichiometry of carbonate apatite and hydroxylapatite also implies a deficiency of calcium ions, i.e., calcium ions may be partially replaced by other cations. Experimental techniques and chemical speciation analysis demonstrate that the presence of magnesium influences the formation of CA and HAP.

Multiple Linear Regression Modeling To Predict the Stability of Polymer-Drug Solid Dispersions: Comparison of the Effects of Polymers and Manufacturing Methods on Solid Dispersion Stability.

Science.gov (United States)

Fridgeirsdottir, Gudrun A; Harris, Robert J; Dryden, Ian L; Fischer, Peter M; Roberts, Clive J

2018-03-29

Solid dispersions can be a successful way to enhance the bioavailability of poorly soluble drugs. Here 60 solid dispersion formulations were produced using ten chemically diverse, neutral, poorly soluble drugs, three commonly used polymers, and two manufacturing techniques, spray-drying and melt extrusion. Each formulation underwent a six-month stability study at accelerated conditions, 40 °C and 75% relative humidity (RH). Significant differences in times to crystallization (onset of crystallization) were observed between both the different polymers and the two processing methods. Stability from zero days to over one year was observed. The extensive experimental data set obtained from this stability study was used to build multiple linear regression models to correlate physicochemical properties of the active pharmaceutical ingredients (API) with the stability data. The purpose of these models is to indicate which combination of processing method and polymer carrier is most likely to give a stable solid dispersion. Six quantitative mathematical multiple linear regression-based models were produced based on selection of the most influential independent physical and chemical parameters from a set of 33 possible factors, one model for each combination of polymer and processing method, with good predictability of stability. Three general rules are proposed from these models for the formulation development of suitably stable solid dispersions. Namely, increased stability is correlated with increased glass transition temperature ( T g ) of solid dispersions, as well as decreased number of H-bond donors and increased molecular flexibility (such as rotatable bonds and ring count) of the drug molecule.

Studies on Dissolution Enhancement of Prednisolone, a Poorly Water-Soluble Drug by Solid Dispersion Technique

Directory of Open Access Journals (Sweden)

Parvin Zakeri-Milani

2011-06-01

Full Text Available Introduction: Prednisolone is a class II substance according to the Biopharmaceutics Classification System. It is a poorly water soluble agent. The aim of the present study was to improve dissolution rate of a poorly water-soluble drug, prednisolone, by a solid dispersion technique. Methods: Solid dispersion of prednisolone was prepared with PEG 6000 or different carbohydrates such as lactose and dextrin with various ratios of the drug to carrier i.e., 1:10, 1:20 and 1:40. Solid dispersions were prepared by coevaporation method. The evaluation of the properties of the dispersions was performed using dissolution studies, Fourier-transform infrared spectroscopy and x-ray powder diffractometery. Results: The results indicated that lactose is suitable carriers to enhance the in vitro dissolution rate of prednisolone. The data from the x-ray diffraction showed that the drug was still detectable in its solid state in all solid dispersions except solid dispersions prepared by dextrin as carrier. The results from infrared spectroscopy showed no well-defined drug–carrier interactions for coevaporates. Conclusion: Solid dispersion of a poorly water-soluble drug, prednisolone may alleviate the problems of delayed and inconsistent rate of dissolution of the drug.

Quantitation of tetrabromobisphenol-A from dust sampled on consumer electronics by dispersed liquid-liquid microextraction

International Nuclear Information System (INIS)

Di Napoli-Davis, Gina; Owens, Janel E.

2013-01-01

Tetrabromobisphenol-A (TBBPA) is a brominated flame retardant used worldwide. Despite its widespread use, there are few data concerning environmental concentrations of TBBPA. Thus, the objective of this work was to optimize an ultrasound-assisted dispersed liquid-liquid microextraction (DLLME) method to analyze swabbed surfaces of consumer electronics to determine TBBPA concentrations. Upon sample preparation with DLLME, TBBPA was derivatized with acetic anhydride and then analyzed by gas chromatography–mass spectrometry (GC/MS). Using a 13 C 12 -TBBPA internal standard to improve precision and quantitation, a recovery study was performed. At concentrations of 250–1000 ng/mL, recoveries were 104–106%. Sample preparation with solid phase extraction had comparable recoveries, although overall, improved analyte recovery and precision were achieved with DLLME. In a small survey study, TBBPA concentrations in dust collected from 100 cm 2 areas on electronic surfaces (monitor, microwave, refrigerator, and TV) were determined to range from less than the LOQ to 523 ng/mL. -- Highlights: •Tetrabromobisphenol-A (TBBPA) concentrations in dust samples were determined. •Dust samples were collected from surfaces of consumer electronics. •Dispersed liquid-liquid microextraction was used to prepare samples for GC/MS. •A 13 C 12 -labeled internal standard was used to improve precision and quantitation. •TBBPA was found in dust samples at levels below LOQ to 523 ng/mL. -- This work describes the analysis of the brominated flame retardant, tetrabromobisphenol-A (TBBPA), from dust sampled on surfaces of consumer electronics

Impact of in situ polymer coating on particle dispersion into solid laser-generated nanocomposites.

Science.gov (United States)

Wagener, Philipp; Brandes, Gudrun; Schwenke, Andreas; Barcikowski, Stephan

2011-03-21

The crucial step in the production of solid nanocomposites is the uniform embedding of nanoparticles into the polymer matrix, since the colloidal properties or specific physical properties are very sensitive to particle dispersion within the nanocomposite. Therefore, we studied a laser-based generation method of a nanocomposite which enables us to control the agglomeration of nanoparticles and to increase the single particle dispersion within polyurethane. For this purpose, we ablated targets of silver and copper inside a polymer-doped solution of tetrahydrofuran by a picosecond laser (using a pulse energy of 125 μJ at 33.3 kHz repetition rate) and hardened the resulting colloids into solid polymers. Electron microscopy of these nanocomposites revealed that primary particle size, agglomerate size and particle dispersion strongly depend on concentration of the polyurethane added before laser ablation. 0.3 wt% polyurethane is the optimal polymer concentration to produce nanocomposites with improved particle dispersion and adequate productivity. Lower polyurethane concentration results in agglomeration whereas higher concentration reduces the production rate significantly. The following evaporation step did not change the distribution of the nanocomposite inside the polyurethane matrix. Hence, the in situ coating of nanoparticles with polyurethane during laser ablation enables simple integration into the structural analogue polymer matrix without additives. Furthermore, it was possible to injection mold these in situ-stabilized nanocomposites without affecting particle dispersion. This clarifies that sufficient in situ stabilization during laser ablation in polymer solution is able to prevent agglomeration even in a hot polymer melt.

Determination of Parabens by Injection-Port Derivatization Coupled With Gas-Chromatography-Mass Spectrometry and Matrix Solid Phase Dispersion

Science.gov (United States)

Djatmika, Rosalina; Ding, Wang-Hsien; Sulistyarti, Hermin

2018-01-01

A rapid determination of four parabens preservatives (methyl paraben, ethyl paraben, propyl paraben, and butyl paraben) in marketed seafood is presented. Analytes were extracted and purified using matrix solid-phase dispersion (MSPD) method, followed by Injection port acylation gas chromatography-mass spectrometry (GC-MS) with acetic anhydride reagent. In this method, acylation of parabens was performed by acetic anhydride at GC injection-port generating reduction of the time-consuming sample-processing steps, and the amount of toxic reagents and solvents. The parameters affecting this method such as injection port temperature, purge-off time and acylation (acetic anhydride) volume were studied. In addition, the MSPD influence factors (including the amount of dispersant and clean-up co-sorbent, as well as the volume of elution solvent) were also investigated. After MSPD method and Injection port acylation applied, good linearity of analytes was achieved. The limits of quantitation (LOQs) were 0.2 to 1.0 ng/g (dry weight). Compared with offline derivatization commonly performed, injection port acylation employs a rapid, simple, low-cost and environmental-friendly derivatization process. The optimized method has been successfully applied for the analysis of parabens in four kind of marketed seafood. Preliminary results showed that the total concentrations of four selected parabens ranged from 16.7 to 44.7 ng/g (dry weight).

Iron oxide functionalized graphene nano-composite for dispersive solid phase extraction of chemical warfare agents from aqueous samples.

Science.gov (United States)

Chinthakindi, Sridhar; Purohit, Ajay; Singh, Varoon; Tak, Vijay; Goud, D Raghavender; Dubey, D K; Pardasani, Deepak

2015-05-15

Present study deals with the preparation and evaluation of graphene based magnetic nano-composite for dispersive solid phase extraction of Chemical Weapons Convention (CWC) relevant chemicals from aqueous samples. Nano-composite, Fe3O4@SiO2-G was synthesized by covalently bonding silica coated Fe3O4 onto the graphene sheets. Nerve agents (NA), Sulfur mustard (SM) and their non-toxic environmental markers were the target analytes. Extraction parameters like amount of sorbent, extraction time and desorption conditions were optimized. Dispersion of 20 milligram of sorbent in 200mL of water sample for 20min. followed by methanol/chloroform extraction produced average to good recoveries (27-94%) of targeted analytes. Recoveries of real agents exhibited great dependency upon sample pH and ionic strength. Sarin produced maximum recovery under mild acidic conditions (56% at pH 5) while VX demanded alkaline media (83% at pH 9). Salts presence in the aqueous samples was found to be advantageous, raising the recoveries to as high as 94% for SM. Excellent limits of detection (LOD) for sulphur mustard and VX (0.11ngmL(-1) and 0.19ngmL(-1) respectively) proved the utility of the developed method for the off-site analysis of CWC relevant chemicals. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation and characterization of etoricoxib solid dispersions using lipid carriers by spray drying technique

OpenAIRE

Chauhan, Bhaskar; Shimpi, Shyam; Paradkar, Anant

2005-01-01

The basic objectives of this study were to prepare and characterize solid dispersions of poorly water-soluble drug etoricoxib using lipid carriers by spray drying technique. The properties of solid dispersions were studied by diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), differential scanning calorimetry (DSC), hotstage microscopy (HSM), radiograph powder diffraction (XRPD), and dissolution studies. The absence of etoricoxib peaks in XRPD profiles of solid dispersions ...

Solid phase epitaxy of amorphous silicon carbide: Ion fluence dependence

International Nuclear Information System (INIS)

Bae, I.-T.; Ishimaru, Manabu; Hirotsu, Yoshihiko; Sickafus, Kurt E.

2004-01-01

We have investigated the effect of radiation damage and impurity concentration on solid phase epitaxial growth of amorphous silicon carbide (SiC) as well as microstructures of recrystallized layer using transmission electron microscopy. Single crystals of 6H-SiC with (0001) orientation were irradiated with 150 keV Xe ions to fluences of 10 15 and 10 16 /cm 2 , followed by annealing at 890 deg. C. Full epitaxial recrystallization took place in a specimen implanted with 10 15 Xe ions, while retardation of recrystallization was observed in a specimen implanted with 10 16 /cm 2 Xe ions. Atomic pair-distribution function analyses and energy dispersive x-ray spectroscopy results suggested that the retardation of recrystallization of the 10 16 Xe/cm 2 implanted sample is attributed to the difference in amorphous structures between the 10 15 and 10 16 Xe/cm 2 implanted samples, i.e., more chemically disordered atomistic structure and higher Xe impurity concentration in the 10 16 Xe/cm 2 implanted sample

Inducing Strong Density Modulation with Small Energy Dispersion in Particle Beams and the Harmonic Amplifier Free Electron Laser

CERN Document Server

McNeil, Brian W J; Robb, Gordon

2005-01-01

We present a possible method of inducing a periodic density modulation in a particle beam with little increase in the energy dispersion of the particles. The flow of particles in phase space does not obey Liouville's Theorem. The method relies upon the Kuramoto-like model of collective synchronism found in free electron generators of radiation, such as Cyclotron Resonance Masers and the Free Electron Laser. For the case of an FEL interaction, electrons initially begin to bunch and emit radiation energy with a correlated energy dispersion which is periodic with the FEL ponderomotive potential. The relative phase between potential and particles is then changed by approximately 180 degrees. The particles continue to bunch, however, there is now a correlated re-absorption of energy from the field. We show that, by repeating this relative phase change many times, a significant density modulation of the particles may be achieved with only relatively small energy dispersion. A similar method of repeated relative ele...

Dispersion Corrected Structural Properties and Quasiparticle Band Gaps of Several Organic Energetic Solids.

Science.gov (United States)

Appalakondaiah, S; Vaitheeswaran, G; Lebègue, S

2015-06-18

We have performed ab initio calculations for a series of energetic solids to explore their structural and electronic properties. To evaluate the ground state volume of these molecular solids, different dispersion correction methods were accounted in DFT, namely the Tkatchenko-Scheffler method (with and without self-consistent screening), Grimme's methods (D2, D3(BJ)), and the vdW-DF method. Our results reveal that dispersion correction methods are essential in understanding these complex structures with van der Waals interactions and hydrogen bonding. The calculated ground state volumes and bulk moduli show that the performance of each method is not unique, and therefore a careful examination is mandatory for interpreting theoretical predictions. This work also emphasizes the importance of quasiparticle calculations in predicting the band gap, which is obtained here with the GW approximation. We find that the obtained band gaps are ranging from 4 to 7 eV for the different compounds, indicating their insulating nature. In addition, we show the essential role of quasiparticle band structure calculations to correlate the gap with the energetic properties.

Dispersive solid-phase microextraction and capillary electrophoresis separation of food colorants in beverages using diamino moiety functionalized silica nanoparticles as both extractant and pseudostationary phase.

Science.gov (United States)

Liu, Feng-Jie; Liu, Chuan-Ting; Li, Wei; Tang, An-Na

2015-01-01

In this work, a new method for the determination of food colorants in beverage samples is developed, using diamino moiety functionalized silica nanoparticles (dASNPs) as both adsorbents in dispersive solid-phase microextraction (dSPME) and pseudostationary phases (PSPs) in capillary electrophoresis (CE) separation. dASNPs were firstly used as adsorbents for the preconcentration of four colorants by the dSPME process. After that, colorants were efficiently separated by CE using 30 mM phosphate buffer (pH 6.0) containing 2 mM β-CD and 0.9 mg/mL dASNPs as additives. All factors influencing dSPME and CE separations were optimized in detail. The investigated analytes showed good linearities with correlation coefficients (R(2)) higher than 0.9932. The limits of detection for the four food colorants were between 0.030 and 0.36 mg/L, which are lower than those reported previously. The established method was also used to analyze four colorants in beverage samples with recoveries ranging from 82.7% to 114.6%. To the best of our knowledge, this is the first time to use NPs both as extractants in dSPME and pseudostationary phases in CE for the analytical purpose. Copyright © 2014 Elsevier B.V. All rights reserved.

Phenyltrichlorosilane-functionalized magnesium oxide microspheres: Preparation, characterization and application for the selective extraction of dioxin-like polycyclic aromatic hydrocarbons in soils with matrix solid-phase dispersion

Energy Technology Data Exchange (ETDEWEB)

Tan, Dongqin [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Jin, Jing [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); Li, Fang [Shenzhen Institutes of Advanced Technology, Chinese Academy of Science, Shenzhen 518055 (China); Sun, Xiaoli [Department of Chemistry, Lishui University, Lishui 32300 (China); Dhanjai; Ni, Yuwen [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); Chen, Jiping, E-mail: chenjp@dicp.ac.cn [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China)

2017-03-01

Magnesium oxide microspheres functionalized with phenyltrichlorosilane (PTS-MgO) were synthesized by surface modification through silanization reaction, which was confirmed by Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), X-ray diffraction (XRD), thermogravimetry analysis (TGA) and N{sub 2} adsorption-desorption. The result indicated that PTS-MgO not only possessed the ability of enhancing the retention with PAHs, but also weakening the interference from chlorinated compounds. As a sorbent for the matrix solid-phase dispersion (MSPD) extraction, PTS-MgO was used to selectively extract seven dioxin-like polycyclic aromatic hydrocarbons (DL-PAHs) from soil samples. Various parameters affecting the recoveries of seven DL-PAHs were investigated and optimized, such as sorbent/sample mass ratio, grinding time, rinsing and eluting conditions. Under the optimized conditions, the developed method combining MSPD with HPLC-FLD exhibited good sensitivity (0.02–0.12 ng g{sup −1} detection of limits) and linearity (linear correlation coefficient greater than 0.9997). Satisfactory recoveries with DL-PAHs spiked at two levels (10 and 80 ng g{sup −1}) were obtained in the range of 72.2–113.1% with RSD < 9.6%, indicating that PTS-MgO had a potential in MSPD extraction of DL-PAHs in soils. Additionally, the proposed MSPD-HPLC-FLD method was also verified by detecting seven DL-PAHs in the standard reference soil. Based on the developed method, DL-PAHs in soil samples were detected with the concentration ranging from 70.08 to 555.05 ng g{sup −1} dry weight (dw). The total toxic equivalency quotients (TEQ) of seven DL-PAHs varied from 9.93 to 143.94 ng TEQ/g dw. - Highlights: • Phenyltrichlorosilane modified magnesium oxide microsphere (PTS-MgO) was presented. • PTS-MgO was used for a new sorbent material in matrix solid-phase dispersion. • The sorbent showed high selectivity for DL-PAHs with satisfactory recoveries obtained. • The

Influence of Calcium on Microbial Reduction of Solid Phase Uranium (VI)

International Nuclear Information System (INIS)

Liu, Chongxuan; Jeon, Byong-Hun; Zachara, John M.; Wang, Zheming

2007-01-01

The effect of calcium on microbial reduction of a solid phase U(VI), sodium boltwoodite (NaUO2SiO3OH · 1.5H2O), was evaluated in a culture of a dissimilatory metal-reducing bacterium (DMRB), Shewanella oneidensis strain MR-1. Batch experiments were performed in a non-growth bicarbonate medium with lactate as electron donor at pH 7 buffered with PIPES. Calcium increased both the rate and extent of Na-boltwoodite dissolution by increasing its solubility through the formation of a ternary aqueous calcium-uranyl-carbonate species. The ternary species, however, decreased the rates of microbial reduction of aqueous U(VI). Laser-induced fluorescence spectroscopy (LIFS) and transmission electron microscopy (TEM) revealed that microbial reduction of solid phase U(VI) is a sequentially coupled process of Na-boltwoodite dissolution, U(VI) aqueous speciation, and microbial reduction of dissolved U(VI) to U(IV) that accumulated on bacterial surfaces/periplasm. The overall rates of microbial reduction of solid phase U(VI) can be described by the coupled rates of dissolution and microbial reduction that were both influenced by calcium. The results demonstrated that dissolved U(VI) concentration during microbial reduction was a complex function of solid phase U(VI) dissolution kinetics, aqueous U(VI) speciation, and microbial activity

Ionic-liquid-based dispersive liquid-liquid microextraction combined with magnetic solid-phase extraction for the determination of aflatoxins B1 , B2 , G1 , and G2 in animal feeds by high-performance liquid chromatography with fluorescence detection.

Science.gov (United States)

Zhao, Jiao; Zhu, Yan; Jiao, Yang; Ning, Jinyan; Yang, Yaling

2016-10-01

A novel two-step extraction technique combining ionic-liquid-based dispersive liquid-liquid microextraction with magnetic solid-phase extraction was developed for the preconcentration and separation of aflatoxins in animal feedstuffs before high-performance liquid chromatography coupled with fluorescence detection. In this work, ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate was used as the extractant in dispersive liquid-liquid microextraction, and hydrophobic pelargonic acid modified Fe 3 O 4 magnetic nanoparticles as an efficient adsorbent were applied to retrieve the aflatoxins-containing ionic liquid. Notably, the target of magnetic nanoparticles was the ionic liquid rather than the aflatoxins. Because of the rapid mass transfer associated with the dispersive liquid-liquid microextraction and magnetic solid phase steps, fast extraction could be achieved. The main parameters affecting the extraction recoveries of aflatoxins were investigated and optimized. Under the optimum conditions, vortexing at 2500 rpm for 1 min in the dispersive liquid-liquid microextraction and magnetic solid-phase extraction and then desorption by sonication for 2 min with acetonitrile as eluent. The recoveries were 90.3-103.7% with relative standard deviations of 3.2-6.4%. Good linearity was observed with correlation coefficients ranged from 0.9986 to 0.9995. The detection limits were 0.632, 0.087, 0.422 and 0.146 ng/mL for aflatoxins B 1 , B2, G1, and G2, respectively. The results were also compared with the pretreatment method carried out by conventional immunoaffinity columns. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characterization during storage and dissolution of Solid dispersions containing furosemide and hydroxypropyl methylcellulose

DEFF Research Database (Denmark)

Nielsen, Line Hagner; Rades, T.; Müllertz, A.

2013-01-01

Solid dispersions containing furosemide and various amounts of hydroxypropyl methylcellulose (HPMC) were prepared by spray drying to investigate if the physical stability of amorphous furosemide during storage and dissolution could be improved by formulating the drug as a solid dispersion. All...

Comparison of three different types of cilostazol-loaded solid dispersion: Physicochemical characterization and pharmacokinetics in rats.

Science.gov (United States)

Mustapha, Omer; Kim, Kyung Soo; Shafique, Shumaila; Kim, Dong Shik; Jin, Sung Giu; Seo, Youn Gee; Youn, Yu Seok; Oh, Kyung Taek; Yong, Chul Soon; Kim, Jong Oh; Choi, Han-Gon

2017-06-01

The aim of this research was to compare three different types of cilostazol-loaded solid dispersion system including solvent-evaporated, solvent-wetted and surface-attached solid dispersion. The effect of polymers and surfactants on the aqueous solubility of cilostazol was investigated, leading to the selection of polyvinylpyrrolidone (PVP) and sodium lauryl sulphate (SLS). Employing a spray-drying technique, numerous surface-attached, solvent-evaporated and solvent-wetted solid dispersions were prepared with various amounts PVP and SLS using water, 90% ethanol and acetone, respectively. Their physicochemical properties, solubility, dissolution and oral bioavailability in rats were assessed compared to the drug powder. Among each solid dispersion system tested, the surface-attached, solvent-evaporated and solvent-wetted solid dispersions composed of cilostazol, PVP and SLS at weight ratios of 3.0 : 0.75 : 1.5, 3.0 : 3.0 : 1.5 and 3.0 : 3.0 : 1.5, respectively, provided the highest drug solubility and dissolution. The solvent-evaporated solid dispersion gave homogeneous and very small spherical particles, in which the drug was changed to an amorphous state. In the solvent-wetted solid dispersion, the amorphous drug was attached to the polymer surface. Conversely, in the surface-attached solid dispersion, the carriers were adhered onto the surface of the unchanged crystalline drug. The solubility, dissolution and oral bioavailability were significantly increased in the order of solvent-evaporated>solvent-wetted>surface-attached>drug powder. Thus, the type of solid dispersion considerably affected the physicochemical properties, aqueous solubility and oral bioavailability. Furthermore, the cilostazol-loaded solvent-evaporated solid dispersion with the highest oral bioavailability would be actively recommended as a practical oral pharmaceutical product. Copyright © 2017 Elsevier B.V. All rights reserved.

The mechanisms of drug release from solid dispersions in water-soluble polymers.

Science.gov (United States)

Craig, Duncan Q M

2002-01-14

Solid dispersions in water-soluble carriers have attracted considerable interest as a means of improving the dissolution rate, and hence possibly bioavailability, of a range of hydrophobic drugs. However, despite the publication of numerous original papers and reviews on the subject, the mechanisms underpinning the observed improvements in dissolution rate are not yet understood. In this review the current consensus with regard to the solid-state structure and dissolution properties of solid dispersions is critically assessed. In particular the theories of carrier- and drug-controlled dissolution are highlighted. A model is proposed whereby the release behaviour from the dispersions may be understood in terms of the dissolution or otherwise of the drug into the concentrated aqueous polymer layer adjacent to the solid surface, including a derivation of an expression to describe the release of intact particles from the dispersions. The implications of a deeper understanding of the dissolution mechanisms are discussed, with particular emphasis on optimising the choice of carrier and manufacturing method and the prediction of stability problems.

Phase noise of dispersion-managed solitons

International Nuclear Information System (INIS)

Spiller, Elaine T.; Biondini, Gino

2009-01-01

We quantify noise-induced phase deviations of dispersion-managed solitons (DMS) in optical fiber communications and femtosecond lasers. We first develop a perturbation theory for the dispersion-managed nonlinear Schroedinger equation (DMNLSE) in order to compute the noise-induced mean and variance of the soliton parameters. We then use the analytical results to guide importance-sampled Monte Carlo simulations of the noise-driven DMNLSE. Comparison of these results with those from the original unaveraged governing equations confirms the validity of the DMNLSE as a model for many dispersion-managed systems and quantify the increased robustness of DMS with respect to noise-induced phase jitter.

Evaluation of alternative environmentally friendly matrix solid phase dispersion solid supports for the simultaneous extraction of 15 pesticides of different chemical classes from drinking water treatment sludge.

Science.gov (United States)

Soares, Karina Lotz; Cerqueira, Maristela Barnes Rodrigues; Caldas, Sergiane Souza; Primel, Ednei Gilberto

2017-09-01

This study describes the development, optimization and validation of a method for the extraction of 15 pesticides of different chemical classes in drinking water treatment sludge (DWTS) by vortex-assisted Matrix Solid Phase Dispersion (MSPD) with determination by gas chromatography coupled to mass spectrometry. It focused on the application of alternative and different solid supports to the extraction step of the MSPD. The main parameters that influenced the extraction were studied in order to obtain better recovery responses. Recoveries ranged from 70 to 120% with RSD below 20% for all analytes. Limits of quantification (LOQ) of the method ranged from 5 to 500 μg kg -1 whereas the analytical curves showed correlation coefficients above 0.997. The method under investigation used low volume of solvent (5 mL), low sample mass (1.5 g) and low mass of chitin (0.5 g), an environmentally friendly support. It has advantages, such as speed, simplicity and low cost material, over other methods. When the method was applied, 4 out of 15 pesticides were detected in the DWTS samples in concentrations below the LOQ. Copyright © 2017 Elsevier Ltd. All rights reserved.

Rapid and selective screening of melamine in bovine milk using molecularly imprinted matrix solid-phase dispersion coupled with liquid chromatography-ultraviolet detection.

Science.gov (United States)

Yan, Hongyuan; Cheng, Xiaoling; Sun, Ning; Cai, Tianyu; Wu, Ruijun; Han, Kun

2012-11-01

A simple, convenient and high selective molecularly imprinted matrix solid-phase dispersion (MI-MSPD) using water-compatible cyromazine-imprinted polymer as adsorbent was proposed for the rapid screening of melamine from bovine milk coupled with liquid chromatography-ultraviolet detection. The molecularly imprinted polymers (MIPs) synthesized by cyromazine as dummy template and reformative methanol-water system as reaction medium showed higher affinity and selectivity to melamine, and so they were applied as the specific dispersant of MSPD to extraction of melamine and simultaneously eliminate the effect of template leakage on quantitative analysis. Under the optimized conditions, good linearity was obtained in a range of 0.24-60.0μgg(-1) with the correlation coefficient of 0.9994. The recoveries of melamine at three spiked levels were ranged from 86.0 to 96.2% with the relative standard deviation (RSD)≤4.0%. This proposed MI-MSPD method combined the advantages of MSPD and MIPs, and could be used as an alternative tool for analyzing the residues of melamine in complex milk samples. Copyright © 2012 Elsevier B.V. All rights reserved.

A comparative study of the effect of spray drying and hot-melt extrusion on the properties of amorphous solid dispersions containing felodipine.

Science.gov (United States)

Mahmah, Osama; Tabbakh, Rami; Kelly, Adrian; Paradkar, Anant

2014-02-01

To compare the properties of solid dispersions of felodipine for oral bioavailability enhancement using two different polymers, polyvinylpyrrolidone (PVP) and hydroxypropyl methylcellulose acetate succinate (HPMCAS), by hot-melt extrusion (HME) and spray drying. Felodipine solid dispersions were prepared by HME and spray drying techniques. PVP and HPMCAS were used as polymer matrices at different drug : polymer ratios (1 : 1, 1 : 2 and 1 : 3). Detailed characterization was performed using differential scanning calorimetry, powder X-ray diffractometry, scanning electron microscopy and in-vitro dissolution testing. Dissolution profiles were evaluated in the presence of sodium dodecyl sulphate. Stability of different solid dispersions was studied under accelerated conditions (40°C/75% RH) over 8 weeks. Spray-dried formulations were found to release felodipine faster than melt extruded formulations for both polymer matrices. Solid dispersions containing HMPCAS exhibited higher drug release rates and better wettability than those produced with a PVP matrix. No significant differences in stability were observed except with HPMCAS at a 1 : 1 ratio, where crystallization was detected in spray-dried formulations. Solid dispersions of felodipine produced by spray drying exhibited more rapid drug release than corresponding melt extruded formulations, although in some cases improved stability was observed for melt extruded formulations. © 2013 Royal Pharmaceutical Society.

Geminate electron--cation recombination in disordered solids

International Nuclear Information System (INIS)

Berlin, Y.A.; Chekunaev, N.I.; Goldanskii, V.I.

1990-01-01

A theory of a geminate electron--cation recombination has been developed using the percolation approach to the description of the electron transport in disordered solids. Following this approach all trapping sites are separated into two groups. The first group forms a diffusion cluster responsible for the macroscopic charge transfer in disordered media whilethe second group consists of isolated traps playing the role of origins and sinks for mobile electrons. In the framework of such a model an equation has been derived describing the electron motion in the Coulomb field of a parent cation. The solution of this equation in the long time limit shows that the recombination rate decreases vs time as t -(1+α/2) with α being a positive constant or a very weak function of t. In the particular case of Gaussian diffusion α=1 and the kinetic law obtained reduces to that predicted by the well-known Onsager--Smoluchowski theory. However for the dispersive (non-Gaussian) transport in highly disordered systems α<1 and its value depends on the type of disorder, on the energy level structure of trapped electrons and on the specific mechanism of electron migration through the medium

Dissolution rate enhancement of repaglinide by solid dispersion

African Journals Online (AJOL)

Keywords: Diabetes, Solid dispersion, Repaglinide, Solubility, Dissolution, Burst release. Tropical Journal of ... high lipophilicity (logP = 3.97) and relatively low oral bioavailability (56 .... II drug, i.e., low soluble and high permeable in nature. As.

Application of solvent-assisted dispersive solid phase extraction as a new, fast, simple and reliable preconcentration and trace detection of lead and cadmium ions in fruit and water samples.

Science.gov (United States)

Behbahani, Mohammad; Ghareh Hassanlou, Parmoon; Amini, Mostafa M; Omidi, Fariborz; Esrafili, Ali; Farzadkia, Mehdi; Bagheri, Akbar

2015-11-15

In this research, a new sample treatment technique termed solvent-assisted dispersive solid phase extraction (SA-DSPE) was developed. The new method was based on the dispersion of the sorbent into the sample to maximize the contact surface. In this approach, the dispersion of the sorbent at a very low milligram level was achieved by injecting a mixture solution of the sorbent and disperser solvent into the aqueous sample. Thereby, a cloudy solution formed. The cloudy solution resulted from the dispersion of the fine particles of the sorbent in the bulk aqueous sample. After extraction, the cloudy solution was centrifuged and the enriched analytes in the sediment phase dissolved in ethanol and determined by flame atomic absorption spectrophotometer. Under the optimized conditions, the detection limit for lead and cadmium ions was 1.2 μg L(-1) and 0.2 μg L(-1), respectively. Furthermore, the preconcentration factor was 299.3 and 137.1 for cadmium and lead ions, respectively. SA-DSPE was successfully applied for trace determination of lead and cadmium in fruit (Citrus limetta, Kiwi and pomegranate) and water samples. Finally, the introduced sample preparation method can be used as a simple, rapid, reliable, selective and sensitive method for flame atomic absorption spectrophotometric determination of trace levels of lead and cadmium ions in fruit and water samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

Characterisation of Gliclazide-PEG 8000 Solid Dispersions

African Journals Online (AJOL)

Erah

Purpose: The aim of the present study was to characterise gliclazide solid dispersions (SDs) ... Results: The solubility of gliclazide increased with increasing amount of PEG 8000 in aqueous medium. ... FTIR analysis demonstrated the absence of well-defined gliclazide - PEG 8000 .... voltage of 35 kV and 20 mA current. The.

Spectral phase shift and residual angular dispersion of an accousto-optic programme dispersive filter

International Nuclear Information System (INIS)

Boerzsoenyi, A.; Meroe, M.

2010-01-01

Complete text of publication follows. There is an increasing demand for active and precise dispersion control of ultrashort laser pulses. In chirped pulse amplification (CPA) laser systems, the dispersion of the optical elements of the laser has to be compensated at least to the fourth order to obtain high temporal contrast compressed pulses. Nowadays the most convenient device for active and programmable control of spectral phase and amplitude of broadband laser pulses is the acousto-optic programmable dispersive filter (AOPDF), claimed to be able to adjust the spectral phase up to the fourth order. Although it has been widely used, surprisingly enough there has been only a single, low resolution measurement reported on the accuracy of the induced spectral phase shift of the device. In our paper we report on the first systematic experiment aiming at the precise characterization of an AOPDF device. In the experiment the spectral phase shift of the AOPDF device was measured by spectrally and spatially resolved interferometry, which is especially powerful tool to determine small dispersion values with high accuracy. Besides the spectral phase dispersion, we measured both the propagation direction angular dispersion (PDAD) and the phase front angular dispersion (PhFAD). Although the two quantities are equal for plane waves, there may be noticeable difference for Gaussian pulses. PDAD was determined simply by focusing the beam on the slit of an imaging spectrograph, while PhFAD was measured by the use of an inverted Mach-Zehnder interferometer and an imaging spectrograph. In the measurements, the spectral phase shift and both types of angular dispersion have been recorded upon the systematic change of all the accessible functions of the acousto-optic programmable dispersive filter. The measured values of group delay dispersion (GDD) and third order dispersion (TOD) have been found to agree with the preset values within the error of the measurement (1 fs 2 and 10 fs 3

Speciation analysis of mercury by dispersive solid-phase extraction coupled with capillary electrophoresis.

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Li, Jinhua; Liu, Junying; Lu, Wenhui; Gao, Fangfang; Wang, Liyan; Ma, Jiping; Liu, Huitao; Liao, Chunyang; Chen, Lingxin

2018-04-23

A pretreatment method of dispersive solid-phase extraction (DSPE) along with back-extraction followed by CE-UV detector was developed for the determination of mercury species in water samples. Sulfhydryl-functionalized SiO 2 microspheres (SiO 2 -SH) were synthesized and used as DSPE adsorbents for selective extraction and enrichment of three organic mercury species namely ethylmercury (EtHg), methylmercury (MeHg), and phenylmercury (PhHg), along with L-cysteine (L-cys) containing hydrochloric acid as back-extraction solvent. Several main extraction parameters were systematically investigated including sample pH, amount of adsorbent, extraction and back-extraction time, volume of eluent, and concentration of hydrochloric acid. Under optimal conditions, good linearity was achieved with correlation coefficients over 0.9990, in the range of 4-200 μg/L for EtHg, and 2-200 μg/L for MeHg and PhHg. The LODs were obtained of 1.07, 0.34, and 0.24 μg/L for EtHg, MeHg, and PhHg, respectively, as well as the LOQs were 3.57, 1.13, and 0.79 μg/L, respectively, with enrichment factors ranging from 109 to 184. Recoveries were attained with tap and lake water samples in a range of 62.3-107.2%, with relative standard deviations of 3.5-10.1%. The results proved that the method of SiO 2 -SH based DSPE coupled with CE-UV was a simple, rapid, cost-effective, and eco-friendly alternative for the determination of mercury species in water samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

PREFACE: International Workshop on Dirac Electrons in Solids 2015

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Ogata, M.; Suzumura, Y.; Fuseya, Y.; Matsuura, H.

2015-04-01

It is our pleasure to publish the Proceedings of the International Workshop on Dirac Electrons in Solids held in University of Tokyo, Japan, for January 14-15, 2015. The workshop was organized by the entitled project which lasted from April 2012 to March 2015 with 10 theorists. It has been supported by a Grand-in-Aid for Scientific Research (A) from the Ministry of Education, Culture, Sports, Science, and Technology, Japan. The subjects discussed in the workshop include bismuth, organic conductors, graphene, topological insulators, new materials including Ca3PbO, and new directions in theory (superconductivity, orbital susceptibility, etc). The number of participants was about 70 and the papers presented in the workshop include four invited talks, 16 oral presentations, and 23 poster presentations. Dirac electron systems appear in various systems, such as graphene, quasi-two-dimensional organic conductors, bismuth, surface states in topological insulators, new materials like Ca3PbO. In these systems, characteristic transport properties caused by the linear dispersion of Dirac electrons and topological properties, have been extensively discussed. In addition to these, there are many interesting research fields such as Spin-Hall effect, orbital diamagnetism due to interband effects, Landau levels characteristic to Dirac dispersion, anomalous interlayer transport phenomena and magnetoresistance, the effects of spin-orbit interaction, and electron correlation. The workshop focused on recent developments of theory and experiment of Dirac electron systems in the above materials. We note that all papers published in this volume of Journal of Physics: Conference Series were peer reviewed. Reviews were performed by expert referees with professional knowledge and high scientific standards in this field. Editors made efforts so that the papers may satisfy the criterion of a proceedings journal published by IOP Publishing. We hope that all the participants of the workshop

Dispersion self-energy of the electron

International Nuclear Information System (INIS)

Hawton, M.

1991-01-01

Electron mass renormalization and the Lamb shift have been investigated using the dispersion self-energy formalism. If shifts of both the electromagnetic field and quantum-mechanical transitions frequencies are considered, absorption from the electromagnetic field is canceled by emission due to atomic fluctuations. The frequencies of all modes are obtained from the self-consistency condition that the field seen by the electron is the same as the field produced by the expectation value of current. The radiation present can thus be viewed as arising from emission and subsequent reabsorption by matter. As developed here, the numerical predictions of dispersion theory are identical to those of quantum electrodynamics. The physical picture implied by dispersion theory is discussed in the context of semiclassical theories and quantum electrodynamics

Investigation into process of solid-phase synthesis of calcium vanadates

International Nuclear Information System (INIS)

Fotiev, A.A.; Krasnenko, T.I.; Slobodin, B.V.

1983-01-01

Processes of solid-phase synthesis of calcium vanadates by Toubandt method, measuring electric conductivity and Ca 45 and V 48 radioactive indicators are investigated. It is shown that reaction diffusion during calcium vanadates production from oxides is ensured by calcium and oxygen ions or calcium ions and electrons through the product layer, as to oxygen - through the gas phase

Development and Optimization of Osmotically Controlled Asymmetric Membrane Capsules for Delivery of Solid Dispersion of Lycopene

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Nitin Jain

2014-01-01

Full Text Available The aim of the present investigation is to develop and statistically optimize the osmotically controlled asymmetric membrane capsules of solid dispersion of lycopene. Solid dispersions of lycopene with β-cyclodextrin in different ratios were prepared using solvent evaporation method. Solubility studies showed that the solid dispersion with 1 : 5 (lycopene : β-cyclodextrin exhibited optimum solubility (56.25 mg/mL for osmotic controlled delivery. Asymmetric membrane capsules (AMCs were prepared on glass mold pins via dip coating method. Membrane characterization by scanning electron microscopy showed inner porous region and outer dense region. Central composite design response surface methodology was applied for the optimization of AMCs. The independent variables were ethyl cellulose (X1, glycerol (X2, and NaCl (X3 which were varied at different levels to analyze the effect on dependent variables (percentage of cumulative drug release (Y1 and correlation coefficient of drug release (Y2. The effect of independent variables on the response was significantly influential. The F18 was selected as optimized formulation based on percentage of CDR (cumulative drug release of 85.63% and correlation coefficient of 0.9994. The optimized formulation was subjected to analyze the effect of osmotic pressure and agitational intensity on percentage of CDR. The drug release was independent of agitational intensity but was dependent on osmotic pressure of dissolution medium.

Determination of soy proteins in food samples by dispersive solid-phase immunoextraction and dynamic long-wavelength fluorometry

International Nuclear Information System (INIS)

Molina-Delgado, María Ángeles; Aguilar-Caballos, María Paz; Gomez-Hens, Agustina

2013-01-01

We report on a method for the determination of soy proteins in food samples via dispersive solid-phase immunoextraction using gold-coated magnetic nanoparticles (NPs) as a support. Soy proteins were first extracted using anti-soy protein antibodies immobilized on the NPs, and then quantified by measuring the increase in fluorescence of the long-wavelength fluorophore cresyl violet in the presence of the anionic surfactant sodium dodecyl sulfate at neutral pH in a flow system. The method involves the use of two standard or sample aliquots. The fluorescence intensity of one aliquot is directly measured whereas that of the other aliquot is measured after immunoextraction. The difference between the peak heights of both aliquots serves as the analytical information that is directly proportional to the protein concentration. The limit of detection is 0.35 mg L −1 , the linear range is from 1 to 15 mg L −1 , and the relative standard deviation is < 5 %. Proteins such as bovine serum albumin and globulins do not interfere at the same concentration level. The method was applied to the analysis of soy-based beverages and gave recoveries in the range between 80.0 and 107.3 %. (author)

Ultrathin-shell boron nitride hollow spheres as sorbent for dispersive solid-phase extraction of polychlorinated biphenyls from environmental water samples.

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Fu, Meizhen; Xing, Hanzhu; Chen, Xiangfeng; Chen, Fan; Wu, Chi-Man Lawrence; Zhao, Rusong; Cheng, Chuange

2014-11-21

Boron nitride hollow spheres with ultrathin-shells were synthesized and used as sorbents for dispersive solid-phase extraction of aromatic pollutants at trace levels from environmental water samples. Polychlorinated biphenyls (PCBs) were selected as target compounds. Sample quantification and detection were performed by gas chromatography-tandem mass spectrometry. Extraction parameters influencing the extraction efficiency were optimized through response surface methodology using the Box-Behnken design. The proposed method achieved good linearity within the concentration range of 0.15-250 ng L(-1) PCBs, low limits of detection (0.04-0.09 ng L(-1), S/N=3:1), good repeatability of the extractions (relative standard deviation, spring waters were analyzed using the developed method. Results demonstrated that the hexagonal boron nitride-based material has significant potential as a sorbent for organic pollutant extraction from environmental water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Simultaneous determination of fumonisins B1 and B2 in different types of maize by matrix solid phase dispersion and HPLC-MS/MS.

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de Oliveira, Gabriel Barros; de Castro Gomes Vieira, Carolyne Menezes; Orlando, Ricardo Mathias; Faria, Adriana Ferreira

2017-10-15

This work involved the optimization and validation of a method, according to Directive 2002/657/EC and the Analytical Quality Assurance Manual of Ministério da Agricultura, Pecuária e Abastecimento, Brazil, for simultaneous extraction and determination of fumonisins B1 and B2 in maize. The extraction procedure was based on a matrix solid phase dispersion approach, the optimization of which employed a sequence of different factorial designs. A liquid chromatography-tandem mass spectrometry method was developed for determining these analytes using the selected reaction monitoring mode. The optimized method employed only 1g of silica gel for dispersion and elution with 70% ammonium formate aqueous buffer (50mmolL -1 , pH 9), representing a simple, cheap and chemically friendly sample preparation method. Trueness (recoveries: 86-106%), precision (RSD ≤19%), decision limits, detection capabilities and measurement uncertainties were calculated for the validated method. The method scope was expanded to popcorn kernels, white maize kernels and yellow maize grits. Copyright © 2017 Elsevier Ltd. All rights reserved.

INVESTIGATION OF THE PHARMACO-TECHNOLOGICAL PROPERTIES OF SOLID DISPERSIONS OF THIOCTIC ACID, OBTAINED BY MICRONIZATION

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Kovalevska, I. V.

2018-04-01

Full Text Available Introduction. Thioctic acid is used in the treatment of diseases that are characterized by lack of mitochondrial activity, which is responsible for the formation of free radicals. Widespread use of thioctic acid is due to the chemical structure. The thioctic acid exhibits biological activity in both hydrophilic and hydrophobic environments. Thioctic acid is an enzyme cofactor and a powerful antioxidant, it regulates the transcription of numerous genes, participates in regulation of glucose and lipid metabolism, increases insulin sensitivity, and forms complexes with heavy metals. Thioctic acid has a high pharmacological potential, which is confirmed by the evidence base of clinical trials. An analysis of the literature on the oral use of thioctic acid indicates that solid dosage forms can be used for long-term therapy. This route of administration is limited by factors such as reduced solubility in acidic environments and enzymatic degradation. For this reason, the search for various compositions of auxiliary substances and methods of obtaining drugs is an urgent task of pharmaceutical technology. Material & methods. Objects of study were solid dispersions of thioctic acid (SDTA on the basis of cellulose derivatives: microcrystalline (MCC, HPMC (hydroxypropyl methylcellulose and polyvinylpyrrolidone (PVP as compared to thioctic acid (TA. The samples were made by solid phase method using micronization in a laboratory shredder at a ratio of 1: 1. Pharmacological and technological parameters were determined according to generally accepted methods. Results & discussion. In appearance the resulting mixtures had lemon color, without inclusions and the formation of conglomerates, with homogeneous sized particles According to the pharmaco-technological studies, the samples do not have a satisfactory flowability. The values of the Carr index and the ratio of Hausner make it possible to conclude that there is a large force of cohesion between the

Determination of Triazine Herbicides in Drinking Water by Dispersive Micro Solid Phase Extraction with Ultrahigh-Performance Liquid Chromatography-High-Resolution Mass Spectrometric Detection.

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Chen, Dawei; Zhang, Yiping; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

2015-11-11

A novel dispersive micro solid phase extraction (DMSPE) method based on a polymer cation exchange material (PCX) was applied to the simultaneous determination of the 30 triazine herbicides in drinking water with ultrahigh-performance liquid chromatography-high-resolution mass spectrometric detection. Drinking water samples were acidified with formic acid, and then triazines were adsorbed by the PCX sorbent. Subsequently, the analytes were eluted with ammonium hydroxide/acetonitrile. The chromatographic separation was performed on an HSS T3 column using water (4 mM ammonium formate and 0.1% formic acid) and acetonitrile (0.1% formic acid) as the mobile phase. The method achieved LODs of 0.2-30.0 ng/L for the 30 triazines, with recoveries in the range of 70.5-112.1%, and the precision of the method was better than 12.7%. These results indicated that the proposed method had the advantages of convenience and high efficiency when applied to the analysis of the 30 triazines in drinking water.

Solid-phase extraction in combination with dispersive liquid-liquid microextraction and ultra-high performance liquid chromatography-tandem mass spectrometry analysis: the ultra-trace determination of 10 antibiotics in water samples.

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Liang, Ning; Huang, Peiting; Hou, Xiaohong; Li, Zhen; Tao, Lei; Zhao, Longshan

2016-02-01

A novel method, solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME), was developed for ultra-preconcentration of 10 antibiotics in different environmental water samples prior to ultra-high performance liquid chromatography-tandem mass spectrometry detection. The optimized results were obtained as follows: after being adjusted to pH 4.0, the water sample was firstly passed through PEP-2 column at 10 mL min(-1), and then methanol was used to elute the target analytes for the following steps. Dichloromethane was selected as extraction solvent, and methanol/acetonitrile (1:1, v/v) as dispersive solvent. Under optimal conditions, the calibration curves were linear in the range of 1-1000 ng mL(-1) (sulfamethoxazole, cefuroxime axetil), 5-1000 ng mL(-1) (tinidazole), 10-1000 ng mL(-1) (chloramphenicol), 2-1000 ng mL(-1) (levofloxacin oxytetracycline, doxycycline, tetracycline, and ciprofloxacin) and 1-400 ng mL(-1) (sulfadiazine) with a good precision. The LOD and LOQ of the method were at very low levels, below 1.67 and 5.57 ng mL(-1), respectively. The relative recoveries of the target analytes were in the range from 64.16% to 99.80% with relative standard deviations between 0.7 and 8.4%. The matrix effect of this method showed a great decrease compared with solid-phase extraction and a significant value of enrichment factor (EF) compared with dispersive liquid-liquid microextraction. The developed method was successfully applied to the extraction and analysis of antibiotics in different water samples with satisfactory results.

Acid functionalized, highly dispersed carbonaceous spheres: an effective solid acid for hydrolysis of polysaccharides

International Nuclear Information System (INIS)

Jiang Yijun; Li Xiutao; Cao Quan; Mu Xindong

2011-01-01

Highly dispersed carbonaceous spheres with sulfonic acid groups were successfully prepared from glucose by hydrothermal method. Transmission electron microscopy (TEM) showed the as-synthesized carbonaceous materials were uniform, spherical in shape with an average diameter of about 450 nm. Fourier transform infrared (FT-IR) proved that –SO 3 H, –COOH, OH groups were grafted on the surface of the carbonaceous spheres during the sulfonation. Interestingly, the functionalized carbonaceous spheres exhibited high dispersibility in the polar solvent due to the hydrophilic groups on the surface. The mechanism of the formation for the carbonaceous spheres was also discussed based on the analysis of structure and composition. At last, the functionalized carbonaceous spheres were employed as solid acid to hydrolyze starch and cellulose. By comparison, the as-synthesized catalyst showed considerable high yield of glucose.

Acid functionalized, highly dispersed carbonaceous spheres: an effective solid acid for hydrolysis of polysaccharides

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Jiang, Yijun; Li, Xiutao; Cao, Quan; Mu, Xindong

2011-02-01

Highly dispersed carbonaceous spheres with sulfonic acid groups were successfully prepared from glucose by hydrothermal method. Transmission electron microscopy (TEM) showed the as-synthesized carbonaceous materials were uniform, spherical in shape with an average diameter of about 450 nm. Fourier transform infrared (FT-IR) proved that -SO3H, -COOH, OH groups were grafted on the surface of the carbonaceous spheres during the sulfonation. Interestingly, the functionalized carbonaceous spheres exhibited high dispersibility in the polar solvent due to the hydrophilic groups on the surface. The mechanism of the formation for the carbonaceous spheres was also discussed based on the analysis of structure and composition. At last, the functionalized carbonaceous spheres were employed as solid acid to hydrolyze starch and cellulose. By comparison, the as-synthesized catalyst showed considerable high yield of glucose.

To evaluate the change in release from solid dispersion using sodium lauryl sulfate and model drug sulfathiazole.

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Dave, Rutesh H; Patel, Hardikkumar H; Donahue, Edward; Patel, Ashwinkumar D

2013-10-01

The solubility of drugs remains one of the most challenging aspects of formulation development. There are numerous ways to improve the solubility of drugs amongst which the most promising strategy is solid dispersion. Different ratios of sulfathiazole: PVP-K29/32: sodium lauryl sulfate (SLS) were prepared (1:1:0.1, 1:1:0.5, 1:1:1) and various methods were employed to characterize the prepared solid dispersions, namely modulated differential scanning calorimeter, X-ray powder diffraction, Fourier Transformed Infrared Spectroscopy and dissolution studies. Lack of crystallinity was observed in internal and external systems suggesting a loss of crystallinity, whereas the physical mixtures showed a characteristic peak of sulfathiazole. In vitro dissolution results clearly showed that the incorporation of a relatively small amount of surfactants (5, 20 or 33% w/w) into a solid dispersion can improve its dissolution rates compared to binary solid dispersion (SD) alone and pure sulfathiazole. In all ratios solid dispersion internal shows a higher dissolution rate compared to a physical mixture and solid dispersion external which suggests that the way that the surfactant is incorporated into the solid dispersion plays an important role in changing the solubility of a drug. The solubilization mechanism is mainly responsible for this higher dissolution rate when we incorporate the SLS in SD.

Solid-phase extraction followed by dispersive liquid-liquid microextraction for the sensitive determination of ecstasy compounds and amphetamines in biological samples

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H. A. Mashayekhi

2014-09-01

Full Text Available A novel approach for the determination of ecstasy and amphetamines (3,4-methylenedioxymethylamphetamine (MDMA, Ecstasy, 3,4-methylenedioxyamphetamine (MDA, 3,4-methylenedioxyethylamphetamine (MDEA and 3,4-methylenedioxypropylamphetamine (MDPA in biological samples is presented. The analytes were extracted from the matrix and transferred to a small volume of a high density, water insoluble solvent using solid-phase extraction (SPE followed by dispersive liquid-liquid microextraction (DLLME. This combination not only resulted in a high enrichment factor, but also it could be used in complex matrices (biological samples. Some important extraction parameters, such as sample solution flow rate, sample pH, type and volume of extraction and disperser solvents as well as the salt addition, were studied and optimized. Under the optimized conditions, the calibration graphs were linear in the range of 0.5-500 µg L-1 and 1.0-500 µg L-1 with detection limits in the range of 0.1-0.3 µg L-1 and 0.2-0.7 µg L-1 in urine and plasma samples, respectively. The results showed that SPE-DLLME is a suitable method for the determination of ecstasy components and amphetamines in biological and water samples. DOI: http://dx.doi.org/10.4314/bcse.v28i3.3

Preconcentration of uranium in water samples using dispersive liquid-liquid micro- extraction coupled with solid-phase extraction and determination with inductively coupled plasma-optical emission spectrometry

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M. Rezaee,

2015-10-01

Full Text Available A new liquid phase microextraction method based on the dispersion of an extraction solvent into aqueous phase coupled with solid-phase extraction was investigated for the extraction, preconcentration and determination of uranium in water samples. 1-(2-Pyridylazo-2-naphthol reagent (PAN at pH 6.0 was used as a chelating agent prior to extraction. After concentration and purification of the samples in SPE C18 sorbent, 1.5 mL elution sample containing 40.0 µL chlorobenzene was injected into the 5.0 mL pure water. After extraction and centrifuging, the sedimented phase was evaporated and the residue was dissolved in nitric acid (0.5 M and was injected by injection valve into the ICP-OES. Some important extraction parameters, such as sample solution flow rate, sample pH, type and volume of extraction and disperser solvents as well as the salt addition were studied and optimized. Under the optimum conditions, the calibration graph was linear in the range of 0.5-500 µg L-1. The detection limit was 0.1 µg L-1. The relative standard deviation (RSD at 5.0 µg L-1 concentration level was 6.6%. Finally, the developed method was successfully applied to the extraction and determination of uranium in the well, river, mineral, waste and tap water samples and satisfactory results were obtained.DOI: http://dx.doi.org/10.4314/bcse.v29i3.4

Development of a Matrix Solid-Phase Dispersion Extraction Combined with UPLC/Q-TOF-MS for Determination of Phenolics and Terpenoids from the Euphorbia fischeriana.

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Li, Wenjing; Lin, Yu; Wang, Yuchun; Hong, Bo

2017-09-11

A method based on a simplified extraction by matrix solid phase dispersion (MSPD) followed by ultra-performance liquid chromatography coupled with the quadrupole time-of-flight tandem mass spectrometry (UPLC/Q-TOF-MS) determination is validated for analysis of two phenolics and three terpenoids in Euphorbia fischeriana . The optimized experimental parameters of MSPD including dispersing sorbent (silica gel), ratio of sample to dispersing sorbent (1:2), elution solvent (water-ethanol: 30-70) and volume of the elution solvent (10 mL) were examined and set down. The highest extraction yields of chromatogram information and the five compounds were obtained under the optimized conditions. A total of 25 constituents have been identified and five components have been quantified from Euphorbia fischeriana . A linear relationship (r² ≥ 0.9964) between the concentrations and the peak areas of the mixed standard substances were revealed. The average recovery was between 92.4% and 103.2% with RSD values less than 3.45% ( n = 5). The extraction yields of two phenolics and three terpenoids obtained by the MSPD were higher than those of traditional reflux and sonication extraction with reduced requirement on sample, solvent and time. In addition, the optimized method will be applied for analyzing terpenoids in other Chinese herbal medicine samples.

Investigation of liquid phase axial dispersion in Taylor bubble flow by radiotracer residence time distribution analysis

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Jin J.H.

2013-05-01

Full Text Available A gas-liquid Taylor bubble flow occurs in small diameter channels in which gas bubbles are separated by slugs of pure liquid. This type of flow regime is well suited for solid catalyzed gas-liquid reactors in which the reaction efficiency is a strong function of axial dispersion in the regions of pure liquid. This paper presents an experimental study of liquid phase axial dispersion in a Taylor bubble flow developed in a horizontal tube using high speed photography and radiotracer residence time distribution (RTD analysis. A parametric dependence of axial dispersion on average volume fraction of gas phase was also investigated by varying the relative volumetric flow rates of the two phases. 137mBa produced from a 137Cs/137mBa radionuclide generator was used as radiotracer and measurements were made using the NaI(Tl scintillation detectors. Validation of 137mBa in the form of barium chloride as aqueous phase radiotracer was also carried out. Axial Dispersion Model (ADM was used to simulate the hydrodynamics of the system and the results of the experiment are presented. It was observed that the system is characterized by very high values of Peclet Number (Pe∼102 which reveals an approaching plug type flow. The experimental and model estimated values of mean residence times were observed in agreement with each other.

Prediction of Phase Behavior of Spray-Dried Amorphous Solid Dispersions: Assessment of Thermodynamic Models, Standard Screening Methods and a Novel Atomization Screening Device with Regard to Prediction Accuracy

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Aymeric Ousset

2018-03-01

Full Text Available The evaluation of drug–polymer miscibility in the early phase of drug development is essential to ensure successful amorphous solid dispersion (ASD manufacturing. This work investigates the comparison of thermodynamic models, conventional experimental screening methods (solvent casting, quench cooling, and a novel atomization screening device based on their ability to predict drug–polymer miscibility, solid state properties (Tg value and width, and adequate polymer selection during the development of spray-dried amorphous solid dispersions (SDASDs. Binary ASDs of four drugs and seven polymers were produced at 20:80, 40:60, 60:40, and 80:20 (w/w. Samples were systematically analyzed using modulated differential scanning calorimetry (mDSC and X-ray powder diffraction (XRPD. Principal component analysis (PCA was used to qualitatively assess the predictability of screening methods with regards to SDASD development. Poor correlation was found between theoretical models and experimentally-obtained results. Additionally, the limited ability of usual screening methods to predict the miscibility of SDASDs did not guarantee the appropriate selection of lead excipient for the manufacturing of robust SDASDs. Contrary to standard approaches, our novel screening device allowed the selection of optimal polymer and drug loading and established insight into the final properties and performance of SDASDs at an early stage, therefore enabling the optimization of the scaled-up late-stage development.

Simultaneous determination of seven synthetic colorants in wine by dispersive micro-solid-phase extraction coupled with reversed-phase high-performance liquid chromatography.

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Zhang, Yun; Zhou, Hua; Wang, Yougang; Wu, Xianglun; Zhao, Yonggang

2015-02-01

A novel and effective dispersive micro-solid-phase extraction (d-µ-SPE) using ethanediamine-functionalized magnetic Fe3O4 polymer (EDA-MP) as an efficient adsorbent in wine sample was developed. Based on this, a simple and time-saving analytical method for the simultaneous determination of seven synthetic colorants (i.e., tartrazine, amaranth, carmine, sunset yellow, allura red, brilliant blue and erythrosine) in wine by reversed-phase high-performance liquid chromatography with an ultraviolet detector was established. The experimental parameters, including the chromatographic retention behavior of studied synthetic colorants, the effect of the usage amount of cross-linking monomer, the effect of the usage amount of EDA-MP on the recovery and the recyclability of the adsorbents, were studied in detail. The results showed that the EDA-MP could be reused efficiently at least six times. Under optimized conditions, the recoveries for all analytes were in the range of 88.6-105.2%, with the intraday relative standard deviations (RSDs) ranging from 2.1 to 8.2% and the interday RSDs ranging from 3.4 to 8.7%, and all the analytes had good linearities in the tested ranges with correlation coefficients (r(2)) >0.9995. The limits of quantification for seven synthetic colorants were between 0.12 and 0.45 mg L(-1). The developed method was successfully applied to wine samples, and it was confirmed that the EDA-MP particles were highly effective d-µ-SPE materials. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

REVIEW ON SPRAY DRIED SOLID DISPERSION

OpenAIRE

Zambre Radhika Ashok, Dr. Shendge R.S, Narode Pravin Ravindra, Sonawane Swapnil Prakash

2018-01-01

The drug solubility is the most challenging aspect for the formulation development. The poorly soluble drug has poor dissolution and absorption of drug. The low aqueous solubility of drug is required to formulate the drug into more soluble and hence bioavailable drug product. The different technique is being used to enhance the solubility of poorly water soluble drugs. Spray dried solid dispersion of drug is one of the most widely used technology to enhance the solubility of the poorly water ...

Development of novel sibutramine base-loaded solid dispersion with gelatin and HPMC: physicochemical characterization and pharmacokinetics in beagle dogs.

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Lim, Hyun-Tae; Balakrishnan, Prabagar; Oh, Dong Hoon; Joe, Kwan Hyung; Kim, Young Ran; Hwang, Doo Hyung; Lee, Yong-Bok; Yong, Chul Soon; Choi, Han-Gon

2010-09-15

To develop a novel sibutramine base-loaded solid dispersion with enhanced solubility and bioavailability, various solid dispersions were prepared using a spray drying technique with hydrophilic polymers such as gelatin, HPMC and citric acid. Their solubility, thermal characteristics and crystallinity were investigated. The dissolution and pharmacokinetics of the sibutramine base-loaded solid dispersion were then compared with a sibutramine hydrochloride monohydrate-loaded commercial product (Reductil). The solid dispersions prepared with gelatin gave higher drug solubility than those prepared without gelatin, irrespective of the amount of polymer. The sibutramine base-loaded solid dispersions containing hydrophilic polymer and citric acid showed higher drug solubility compared to sibutramine base and sibutramine hydrochloride monohydrate. Among the formulations tested, the solid dispersion composed of sibutramine base/gelatin/HPMC/citric acid at the weight ratio of 1/0.8/0.2/0.5 gave the highest solubility of 5.03+/-0.24 mg/ml. Our DSC and powder X-ray diffraction results showed that the drug was present in an altered amorphous form in this solid dispersion. The difference factor (f(1)) values between solid dispersion and commercial product were 2.82, 6.65 and 6.31 at pH 1.2, 4.0 and 6.8, respectively. Furthermore, they had the similarity factor (f(2)) value of 65.68, 53.43 and 58.97 at pH 1.2, 4.0 and 6.8, respectively. Our results suggested that the solid dispersion and commercial product produced a similar correlation of dissolution profiles at all pH ranges. The AUC, C(max) and T(max) of the parent drug and metabolite I and II from the solid dispersion were not significantly different from those of the commercial product, suggesting that the solid dispersion might be bioequivalent to the commercial product in beagle dogs. Thus, the sibutramine base-loaded solid dispersion prepared with gelatin, HPMC and citric acid is a promising candidate for improving the

Zinc oxide crystal whiskers as a novel sorbent for solid-phase extraction of flavonoids.

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Wang, Licheng; Shangguan, Yangnan; Hou, Xiudan; Jia, Yong; Liu, Shujuan; Sun, Yingxin; Guo, Yong

2017-08-15

As a novel solid-phase extraction material, zinc oxide crystal whiskers were used to extract flavonoid compounds and showed good extraction abilities. X-ray diffraction, scanning electron microscopy with energy dispersive X-ray spectroscopy and surface area/pore volume characterized the sorbent. The zinc oxide was packed into a solid-phase extraction micro-column and its extraction ability was evaluated by four model flavonoid compounds. The sample loading and elution parameters were optimized and the zinc oxide based analytical method for flavonoids was established. It showed that the method has wide linearities from 1 to 150μg/L and low limits of detection at 0.25μg/L. The relative standard deviations of a single column repeatability and column to column reproducibility were less than 6.8% and 10.6%. Several real samples were analyzed by the established method and satisfactory results were obtained. The interactions between flavonoids and zinc oxide were calculated and proved to be from the Van der Waals' forces between the 4p and 5d orbitals from zinc atom and the neighboring π orbitals from flavonoid phenyl groups. Moreover, the zinc oxide crystal whiskers showed good stability and could be reused more than 50 times under the operation conditions. This work proves that the zinc oxide crystal whiskers are a good candidate for flavonoids enrichment. Copyright © 2017. Published by Elsevier B.V.

Effects of calcination temperature on phase formation and particle size of Zn{sub 2}Nb{sub 34}O{sub 87} powder synthesized by solid-state reaction

Energy Technology Data Exchange (ETDEWEB)

Amonpattaratkit, Penphitcha, E-mail: p.amonpattaratkit@gmail.com [Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Ananta, Supon, E-mail: suponananta@yahoo.com [Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand)

2013-05-15

The solid-state mixed oxide method via a rapid vibro-milling technique was explored for the preparation of single-phase Zn{sub 2}Nb{sub 34}O{sub 87} nanopowders. Phase formation of zinc niobate was investigated as a function of calcination temperature by using a combination of thermogravimetric/differential thermal analyzer (TG/DTA) and X-ray diffraction (XRD) techniques. Morphology, particle size and chemical composition of the powders were determined by scanning electron microscopy (SEM) and energy-dispersive X-ray (EDX) technique. The obtained results clearly revealed the influences of calcination temperature on phase formation and particle size of Zn{sub 2}Nb{sub 34}O{sub 87} nanopowder. - Highlights: ► Single phase Zn{sub 2}Nb{sub 34}O{sub 87} was firstly prepared by solid-state mixed oxide method via a rapid vibro-milling technique. ► The influences of calcination temperature on phase formation and particle size were investigated. ► Zn{sub 2}Nb{sub 34}O{sub 87} powders were characterized by TG–DTA, XRD, SEM and EDX.

Taurine zinc solid dispersions attenuate doxorubicin-induced hepatotoxicity and cardiotoxicity in rats

International Nuclear Information System (INIS)

Wang, Yu; Mei, Xueting; Yuan, Jingquan; Lu, Wenping; Li, Binglong; Xu, Donghui

2015-01-01

The clinical efficacy of anthracycline anti-neoplastic agents is limited by cardiac and hepatic toxicities. The aim of this study was to assess the hepatoprotective and cardioprotective effects of taurine zinc solid dispersions, which is a newly-synthesized taurine zinc compound, against doxorubicin-induced toxicity in Sprague–Dawley rats intraperitoneally injected with doxorubicin hydrochloride (3 mg/kg) three times a week (seven injections) over 28 days. Hemodynamic parameters, levels of liver toxicity markers and oxidative stress were assessed. Taurine zinc significantly attenuated the reductions in blood pressure, left ventricular pressure and ± dp/dtmax, increases in serum alanine aminotransferase and aspartate aminotransferase activities, and reductions in serum Zn 2+ and albumin levels (P < 0.05 or 0.01) induced by doxorubicin. In rats treated with doxorubicin, taurine zinc dose-dependently increased liver superoxide dismutase activity and glutathione concentration, and decreased malondialdehyde level (P < 0.01). qBase + was used to evaluate the stability of eight candidate reference genes for real-time quantitative reverse-transcription PCR. Taurine zinc dose-dependently increased liver heme oxygenase-1 and UDP-glucuronyl transferase mRNA and protein expression (P < 0.01). Western blotting demonstrated that taurine zinc inhibited c-Jun N-terminal kinase phosphorylation by upregulating dual-specificity phosphoprotein phosphatase-1. Additionally, taurine zinc inhibited cardiomyocyte apoptosis as there was decreased TUNEL/DAPI positivity and protein expression of caspase-3. These results indicate that taurine zinc solid dispersions prevent the side-effects of anthracycline-based anticancer therapy. The mechanisms might be associated with the enhancement of antioxidant defense system partly through activating transcription to synthesize endogenous phase II medicine enzymes and anti-apoptosis through inhibiting JNK phosphorylation. - Highlights: �

Taurine zinc solid dispersions attenuate doxorubicin-induced hepatotoxicity and cardiotoxicity in rats

Energy Technology Data Exchange (ETDEWEB)

Wang, Yu; Mei, Xueting; Yuan, Jingquan; Lu, Wenping; Li, Binglong; Xu, Donghui, E-mail: Donghuixu007@163.com

2015-11-15

The clinical efficacy of anthracycline anti-neoplastic agents is limited by cardiac and hepatic toxicities. The aim of this study was to assess the hepatoprotective and cardioprotective effects of taurine zinc solid dispersions, which is a newly-synthesized taurine zinc compound, against doxorubicin-induced toxicity in Sprague–Dawley rats intraperitoneally injected with doxorubicin hydrochloride (3 mg/kg) three times a week (seven injections) over 28 days. Hemodynamic parameters, levels of liver toxicity markers and oxidative stress were assessed. Taurine zinc significantly attenuated the reductions in blood pressure, left ventricular pressure and ± dp/dtmax, increases in serum alanine aminotransferase and aspartate aminotransferase activities, and reductions in serum Zn{sup 2+} and albumin levels (P < 0.05 or 0.01) induced by doxorubicin. In rats treated with doxorubicin, taurine zinc dose-dependently increased liver superoxide dismutase activity and glutathione concentration, and decreased malondialdehyde level (P < 0.01). qBase{sup +} was used to evaluate the stability of eight candidate reference genes for real-time quantitative reverse-transcription PCR. Taurine zinc dose-dependently increased liver heme oxygenase-1 and UDP-glucuronyl transferase mRNA and protein expression (P < 0.01). Western blotting demonstrated that taurine zinc inhibited c-Jun N-terminal kinase phosphorylation by upregulating dual-specificity phosphoprotein phosphatase-1. Additionally, taurine zinc inhibited cardiomyocyte apoptosis as there was decreased TUNEL/DAPI positivity and protein expression of caspase-3. These results indicate that taurine zinc solid dispersions prevent the side-effects of anthracycline-based anticancer therapy. The mechanisms might be associated with the enhancement of antioxidant defense system partly through activating transcription to synthesize endogenous phase II medicine enzymes and anti-apoptosis through inhibiting JNK phosphorylation. - Highlights: �

Dynamic speciation analysis of atrazine in aqueous latex nanoparticle dispersions using solid phase microextraction (SPME)

NARCIS (Netherlands)

Benhabib, K.; Town, R.M.; Leeuwen, van H.P.

2009-01-01

Solid phase microextraction (SPME) is applied in the dynamic speciation analysis of the pesticide atrazine in an aqueous medium containing sorbing latex nanoparticles. It is found that the overall rate of extraction of the analyte is faster than in the absence of nanoparticles and governed by the

In-Vial Micro-Matrix-Solid Phase Dispersion for the Analysis of Fragrance Allergens, Preservatives, Plasticizers, and Musks in Cosmetics

Directory of Open Access Journals (Sweden)

Maria Celeiro

2014-07-01

Full Text Available Fragrance allergens, preservatives, plasticizers, and synthetic musks are usually present in cosmetic and personal care products formulations and many of them are subjected to use restrictions or labeling requirements. Matrix solid-phase dispersion (MSPD is a very suitable analytical technique for the extraction of these compounds providing a simple, low cost sample preparation, and the possibility of performing both extraction and clean-up in one step, reducing possible contamination and analyte losses. This extraction technique has been successfully applied to many cosmetics ingredients allowing obtaining quantitative recoveries. A new very simple micro-MSPD procedure performing the disruption step in a vial is proposed for the gas chromatography-mass spectrometry (GC-MS analysis of 66 chemicals usually present in cosmetics and personal care products. The method was validated showing general recoveries between 80% and 110%, relative standard deviation (RSD values lower than 15%, and limits of detection (LODs below 30 ng·g−1. The validated method was applied to a broad range of cosmetics and personal care products, including several products intended for baby care.

Rare Earth Element Phases in Bauxite Residue

Directory of Open Access Journals (Sweden)

Johannes Vind

2018-02-01

Full Text Available The purpose of present work was to provide mineralogical insight into the rare earth element (REE phases in bauxite residue to improve REE recovering technologies. Experimental work was performed by electron probe microanalysis with energy dispersive as well as wavelength dispersive spectroscopy and transmission electron microscopy. REEs are found as discrete mineral particles in bauxite residue. Their sizes range from <1 μm to about 40 μm. In bauxite residue, the most abundant REE bearing phases are light REE (LREE ferrotitanates that form a solid solution between the phases with major compositions (REE,Ca,Na(Ti,FeO3 and (Ca,Na(Ti,FeO3. These are secondary phases formed during the Bayer process by an in-situ transformation of the precursor bauxite LREE phases. Compared to natural systems, the indicated solid solution resembles loparite-perovskite series. LREE particles often have a calcium ferrotitanate shell surrounding them that probably hinders their solubility. Minor amount of LREE carbonate and phosphate minerals as well as manganese-associated LREE phases are also present in bauxite residue. Heavy REEs occur in the same form as in bauxites, namely as yttrium phosphates. These results show that the Bayer process has an impact on the initial REE mineralogy contained in bauxite. Bauxite residue as well as selected bauxites are potentially good sources of REEs.

Formulation of Fast-Release Gastroretentive Solid Dispersion of ...

African Journals Online (AJOL)

Methods: Hot melt granulation technique was adopted to prepare solid dispersions (SDs) of glibenclamide in .... ml of 0.1M HCl (pH 1.2), stirred at 20 rpm in a water bath (25 ± 0.3 .... cm-1; and SO2 stretching vibration at 1340.43 and 1159.14 ...

Spheroidization behavior of dendritic b.c.c. phase in Zr-based モ-phase composite

Directory of Open Access Journals (Sweden)

Sun Guoyuan

2013-03-01

Full Text Available The spheroidization behavior of the dendritic b.c.c. phase dispersed in a bulk metallic glass (BMG matrix was investigated through applying semi-solid isothermal processing and a subsequent rapid quenching procedure to a Zr-based モ-phase composite. The Zr-based composite with the composition of Zr56.2Ti13.8Nb5.0Cu6.9Ni5.6Be12.5 was prefabricated by a water-cooled copper mold-casting method and characterized by X-ray diffraction (XRD and scanning electron microscope (SEM. The results show that the composite consists of a glassy matrix and uniformly distributed fine dendrites of the モ-Zr solid solution with the body-centered-cubic (b.c.c. structure. Based on the differential scanning calorimeter (DSC examination results, and in view of the b.c.c. モ-Zr to h.c.p. メ-Zr phase transition temperature, a semi-solid holding temperature of 900 ìC was determined. After reheating the prefabricated composite to the semi-solid temperature, followed by an isothermal holding process at this temperature for 5 min, and then quenching the semi-solid mixture into iced-water; the two-phase microstructure composed of a BMG matrix and uniformly dispersed spherical b.c.c. モ-Zr particles with a high degree of sphericity was achieved. The present spheroidization transition is a thermodynamically autonomic behavior, and essentially a diffusion process controlled by kinetic factors; and the formation of the BMG matrix should be attributed to the rapid quenching of the semi-solid mixture as well as the large glass-forming ability of the remaining melt in the semi-solid mixture.

The electron spectrum of UF6 recorded in the gas phase

Science.gov (United States)

Mârtensson, N.; Malmquist, P.-Å.; Svensson, S.; Johansson, B.

1984-06-01

Gas phase core and valence electron spectra from UF6, excited by AlKα monochromatized x rays, in the binding energy range 0-1000 eV are presented. It is shown that the AlKα excited valence electron spectrum can be used to reassign the highest occupied molecular orbital (HOMO) in UF6. Many-body effects on the core levels are discussed and core level lifetimes are determined. The shift between solid phase and gas phase electron binding energies for core lines is used to discuss the U5 f population in UF6.

Preparation and characterization of celecoxib solid dispersions; comparison of poloxamer-188 and PVP-K30 as carriers

Directory of Open Access Journals (Sweden)

Alireza Homayouni

2014-05-01

Full Text Available Objective(s:Solid dispersion formulation is the most promising strategy to improve oral bioavailability of poorly water soluble drugs. The aim of this study was to compare the effect of polyvinylpyrrolidone K30 (PVP and poloxamer-188 (PLX as carrier in solid dispersion formulations of celecoxib (CLX. Materials and Methods: Solid dispersions of CLX:PVP or CLX:PLX were prepared at different ratios (2:1, 1:1, 1:2, 1:4, 1:6 by solvent evaporation and melting methods, respectively. The characterization of samples was performed using differential scanning calorimetery (DSC, X-Ray powder diffraction (XRPD and Fourier transform infrared spectroscopy (FT-IR. The Gordon-Taylor equation was used to estimate the Tg of solid dispersion systems and the possibility of the interaction between CLX and PVP. Also, the dissolution rate of all samples was determined. Results: DSC and XRPD analyses confirmed the presence of amorphous state of drug in solid dispersion systems. FT-IR studies showed CLX could participate in hydrogen bonding with PVP whilst no specific interaction between CLX and PLX was observed. Both PVP and PLX enhanced the dissolution rate of drug in solid dispersion samples. The dissolution rate was dependent on the ratio of drug: carrier. Interestingly, the solid dispersion samples of PLX at 2:1 and 1:1 drug: carrier showed slower dissolution rate than pure CLX, whilst these results were not observed for PVP. Conclusion: The effect of PVP on dissolution rate enhancement was more pronounced compared to the other carrier. Having a higher Tg and more effect on dissolution rate, PVP could be considered as a more suitable carrier compared to PLX in solid dispersion formulation of CLX.

Electron probe micro-analysis of gas bubbles in solids: a novel approach

International Nuclear Information System (INIS)

Verwerft, M.; Vos, B.

1999-01-01

The local analysis of retained noble gas in nuclear fuel is inherently difficult since the physical form under which it is stored varies from atomically dispersed to bubbles with a diameter of several hundreds of nanometers. One of the techniques that has been applied since pore than twenty years is EPMA. Although many important results have been obtained with this technique, its application to the analysis of highly inhomogeneous materials is limited. The EPMA technique is indeed difficult to apply to samples that are not homogeneous on the scale of the electron-solid interaction volume. The paper discusses the development of a method to analyse a system of as bubbles distributed in a solid matrix. This method has been based on a multiple voltage EPMA measurement combined with a scanning Electron Microscopic analysis of the bubble size distribution

Electric field driven plasmon dispersion in AlGaN/GaN high electron mobility transistors

International Nuclear Information System (INIS)

Tan Ren-Bing; Qin Hua; Zhang Xiao-Yu; Xu Wen

2013-01-01

We present a theoretical study on the electric field driven plasmon dispersion of the two-dimensional electron gas (2DEG) in AlGaN/GaN high electron mobility transistors (HEMTs). By introducing a drifted Fermi—Dirac distribution, we calculate the transport properties of the 2DEG in the AlGaN/GaN interface by employing the balance-equation approach based on the Boltzmann equation. Then, the nonequilibrium Fermi—Dirac function is obtained by applying the calculated electron drift velocity and electron temperature. Under random phase approximation (RPA), the electric field driven plasmon dispersion is investigated. The calculated results indicate that the plasmon frequency is dominated by both the electric field E and the angle between wavevector q and electric field E. Importantly, the plasmon frequency could be tuned by the applied source—drain bias voltage besides the gate voltage (change of the electron density)

Solid-solid phase transitions in Fe nanowires induced by axial strain

International Nuclear Information System (INIS)

Sandoval, Luis; Urbassek, Herbert M

2009-01-01

By means of classical molecular-dynamics simulations we investigate the solid-solid phase transition from a bcc to a close-packed crystal structure in cylindrical iron nanowires, induced by axial strain. The interatomic potential employed has been shown to be capable of describing the martensite-austenite phase transition in iron. We study the stress versus strain curves for different temperatures and show that for a range of temperatures it is possible to induce a solid-solid phase transition by axial strain before the elasticity is lost; these transition temperatures are below the bulk transition temperature. The two phases have different (non-linear) elastic behavior: the bcc phase softens, while the close-packed phase stiffens with temperature. We also consider the reversibility of the transformation in the elastic regimes, and the role of the strain rate on the critical strain necessary for phase transition.

Formulation, Characterization, and in Vivo Evaluation of Celecoxib-PVP Solid Dispersion Nanoparticles Using Supercritical Antisolvent Process

Directory of Open Access Journals (Sweden)

Eun-Sol Ha

2014-12-01

Full Text Available The aim of this study was to develop celecoxib-polyvinylpyrrolidone (PVP solid dispersion nanoparticles with and without surfactant using the supercritical antisolvent (SAS process. The effect of different surfactants such as gelucire 44/14, poloxamer 188, poloxamer 407, Ryoto sugar ester L1695, and d-α-tocopheryl polyethylene glycol 1000 succinate (TPGS on nanoparticle formation and dissolution as well as oral absorption of celecoxib-PVP K30 solid dispersion nanoparticles was investigated. Spherical celecoxib solid dispersion nanoparticles less than 300 nm in size were successfully developed using the SAS process. Analysis by differential scanning calorimetry and powder X-ray diffraction showed that celecoxib existed in the amorphous form within the solid dispersion nanoparticles fabricated using the SAS process. The celecoxib-PVP-TPGS solid dispersion nanoparticles significantly enhanced in vitro dissolution and oral absorption of celecoxib relative to that of the unprocessed form. The area under the concentration-time curve (AUC0→24 h and peak plasma concentration (Cmax increased 4.6 and 5.7 times, respectively, with the celecoxib-PVP-TPGS formulation. In addition, in vitro dissolution efficiency was well correlated with in vivo pharmacokinetic parameters. The present study demonstrated that formulation of celecoxib-PVP-TPGS solid dispersion nanoparticles using the SAS process is a highly effective strategy for enhancing the bioavailability of poorly water-soluble celecoxib.

Adsorption factor effect on dispersive ability of polymethylmethylmethacrylate

International Nuclear Information System (INIS)

Gorokhovskij, G.A.; Samsonov, G.V.; Gorshunov, V.P.

1977-01-01

A relationhsip between the rate of polymer macromolecules absorption on some refractory compounds and the dispersion ability of polymer-abrasive compositions was investigated at various contents of the polymethacrylate polymer in an abrasive composition. The solid phase used was powders of Al 2 O 3 , WC, W 2 B 5 , TiB 2 . It was established that the dispersion ability of the polymer-abrasive compositions was a function not only of the cutting properties of the abrasives and the dispersion ability of the polymers, but also of the adsorption properties of the solid phase and of its capacity to transport macromolecules to the surface being worked

Enhanced Supersaturation and Oral Absorption of Sirolimus Using an Amorphous Solid Dispersion Based on Eudragit® E

Directory of Open Access Journals (Sweden)

Youngseok Cho

2015-05-01

Full Text Available The present study aimed to investigate the effect of Eudragit® E/HCl (E-SD on the degradation of sirolimus in simulated gastric fluid (pH 1.2 and to develop a new oral formulation of sirolimus using E-SD solid dispersions to enhance oral bioavailability. Sirolimus-loaded solid dispersions were fabricated by a spray drying process. A kinetic solubility test demonstrated that the sirolimus/E-SD/TPGS (1/8/1 solid dispersion had a maximum solubility of 196.7 μg/mL within 0.5 h that gradually decreased to 173.4 μg/mL after 12 h. According to the dissolution study, the most suitable formulation was the sirolimus/E-SD/TPGS (1/8/1 solid dispersion in simulated gastric fluid (pH 1.2, owing to enhanced stability and degree of supersaturation of E-SD and TPGS. Furthermore, pharmacokinetic studies in rats indicated that compared to the physical mixture and sirolimus/HPMC/TPGS (1/8/1 solid dispersion, the sirolimus/E-SD/TPGS (1/8/1 solid dispersion significantly improved oral absorption of sirolimus. E-SD significantly inhibited the degradation of sirolimus in a dose-dependent manner. E-SD also significantly inhibited the precipitation of sirolimus compared to hydroxypropylmethyl cellulose (HPMC. Therefore, the results from the present study suggest that the sirolimus-loaded E-SD/TPGS solid dispersion has great potential in clinical applications.

Properties of the particulate phase in deep saline groundwater in Laxemar, Sweden

DEFF Research Database (Denmark)

Düker, Anders; Ledin, Anna

1998-01-01

analysis were performed on-line in a field laboratory using measurements of light scattering in combination with photon correlation spectroscopy (PCS). Estimates of the chemical composition of the solid phase were obtained from scanning electron microscopy (SEM) coupled to energy dispersive spectroscopy...

Axial dispersion, holdup and slip velocity of dispersed phase in a pulsed sieve plate extraction column by radiotracer residence time distribution analysis.

Science.gov (United States)

Din, Ghiyas Ud; Chughtai, Imran Rafiq; Inayat, Mansoor Hameed; Khan, Iqbal Hussain

2008-12-01

Axial dispersion, holdup and slip velocity of dispersed phase have been investigated for a range of dispersed and continuous phase superficial velocities in a pulsed sieve plate extraction column using radiotracer residence time distribution (RTD) analysis. Axial dispersion model (ADM) was used to simulate the hydrodynamics of the system. It has been observed that increase in dispersed phase superficial velocity results in a decrease in its axial dispersion and increase in its slip velocity while its holdup increases till a maximum asymptotic value is achieved. An increase in superficial velocity of continuous phase increases the axial dispersion and holdup of dispersed phase until a maximum value is obtained, while slip velocity of dispersed phase is found to decrease in the beginning and then it increases with increase in superficial velocity of continuous phase.

Electron holography for fields in solids: problems and progress.

Science.gov (United States)

Lichte, Hannes; Börrnert, Felix; Lenk, Andreas; Lubk, Axel; Röder, Falk; Sickmann, Jan; Sturm, Sebastian; Vogel, Karin; Wolf, Daniel

2013-11-01

Electron holography initially was invented by Dennis Gabor for solving the problems raised by the aberrations of electron lenses in Transmission Electron Microscopy. Nowadays, after hardware correction of aberrations allows true atomic resolution of the structure, for comprehensive understanding of solids, determination of electric and magnetic nanofields is the most challenging task. Since fields are phase objects in the TEM, electron holography is the unrivaled method of choice. After more than 40 years of experimental realization and steady improvement, holography is increasingly contributing to these highly sophisticated and essential questions in materials science, as well to the understanding of electron waves and their interaction with matter. © 2013 Elsevier B.V. All rights reserved.

Preparation of solid silver nanoparticles for inkjet printed flexible electronics with high conductivity.

Science.gov (United States)

Shen, Wenfeng; Zhang, Xianpeng; Huang, Qijin; Xu, Qingsong; Song, Weijie

2014-01-01

Silver nanoparticles (NPs) which could be kept in solid form and were easily stored without degeneration or oxidation at room temperature for a long period of time were synthesized by a simple and environmentally friendly wet chemistry method in an aqueous phase. Highly stable dispersions of aqueous silver NP inks, sintered at room temperature, for printing highly conductive tracks (∼8.0 μΩ cm) were prepared simply by dispersing the synthesized silver NP powder in water. These inks are stable, fairly homogeneous and suitable for a wide range of patterning techniques. The inks were successfully printed on paper and polyethylene terephthalate (PET) substrates using a common color printer. Upon annealing at 180 °C, the resistivity of the printed silver patterns decreased to 3.7 μΩ cm, which is close to twice that of bulk silver. Various factors affecting the resistivity of the printed silver patterns, such as annealing temperature and the number of printing cycles, were investigated. The resulting high conductivity of the printed silver patterns reached over 20% of the bulk silver value under ambient conditions, which enabled the fabrication of flexible electronic devices, as demonstrated by the inkjet printing of conductive circuits of LED devices.

Analytical electron microscope study of the omega phase transformation in a zirconium--niobium alloy

Energy Technology Data Exchange (ETDEWEB)

Zaluzec, N.J.

1979-06-01

An in-situ study of the as-quenched omega phase transformation in Zr--15% Nb was conducted between the temperatures of 77 and 300/sup 0/K using analytical electron microscopy. The domain size of the omega regions observed in this investigation was on the order of 30 A, consistent with previous observations in this system. No alignment of omega domains along <222> directions of the bcc lattice was observed and in-situ thermal cycling experiments failed to produce a long period structure of alternating ..beta.. and ..omega.. phase regions as predicted by one theory of this transformation. Several techniques of microstructural analysis were developed, refined, and standardized. Grouped under the general classification of Analytical Electron Microscopy (AEM) they provide the experimentalist with a unique tool for the microcharacterization of solids, allowing semiquantitative to quantitative analysis of the morphology, crystallography, elemental composition, and electronic structure of regions as small as 20 A in diameter. These techniques have complications, and it was necessary to study the AEM system used in this work so that instrumental artifacts which invalidate the information produced in the microscope environment might be eliminated. Once these factors had been corrected, it was possible to obtain a wealth of information about the microvolume of material under investigation. The microanalytical techniques employed during this research include: energy dispersive x-ray spectroscopy (EDS) using both conventional and scanning transmission electron microscopy (CTEM, STEM), transmission scanning electron diffraction (TSED), the stationary diffraction pattern technique, and electron energy loss spectroscopy (ELS) using a dedicated scanning transmission electron microscope (DSTEM).

Analytical electron microscope study of the omega phase transformation in a zirconium--niobium alloy

International Nuclear Information System (INIS)

Zaluzec, N.J.

1979-06-01

An in-situ study of the as-quenched omega phase transformation in Zr--15% Nb was conducted between the temperatures of 77 and 300 0 K using analytical electron microscopy. The domain size of the omega regions observed in this investigation was on the order of 30 A, consistent with previous observations in this system. No alignment of omega domains along directions of the bcc lattice was observed and in-situ thermal cycling experiments failed to produce a long period structure of alternating β and ω phase regions as predicted by one theory of this transformation. Several techniques of microstructural analysis were developed, refined, and standardized. Grouped under the general classification of Analytical Electron Microscopy (AEM) they provide the experimentalist with a unique tool for the microcharacterization of solids, allowing semiquantitative to quantitative analysis of the morphology, crystallography, elemental composition, and electronic structure of regions as small as 20 A in diameter. These techniques have complications, and it was necessary to study the AEM system used in this work so that instrumental artifacts which invalidate the information produced in the microscope environment might be eliminated. Once these factors had been corrected, it was possible to obtain a wealth of information about the microvolume of material under investigation. The microanalytical techniques employed during this research include: energy dispersive x-ray spectroscopy (EDS) using both conventional and scanning transmission electron microscopy (CTEM, STEM), transmission scanning electron diffraction (TSED), the stationary diffraction pattern technique, and electron energy loss spectroscopy (ELS) using a dedicated scanning transmission electron microscope

Structural diversity of solid dispersions of acetylsalicylic acid as seen by solid-state NMR

Czech Academy of Sciences Publication Activity Database

Policianová, Olivia; Brus, Jiří; Hrubý, Martin; Urbanová, Martina; Zhigunov, Alexander; Kredatusová, Jana; Kobera, Libor

2014-01-01

Roč. 11, č. 2 (2014), s. 516-530 ISSN 1543-8384 R&D Projects: GA ČR GPP106/11/P426 Institutional support: RVO:61389013 Keywords : solid dispersions * acetylsalicylic acid * polymers Subject RIV: FR - Pharmacology ; Medidal Chemistry Impact factor: 4.384, year: 2014

Superparamagnetic graphene oxide-based dispersive-solid phase extraction for preconcentration and determination of tamsulosin hydrochloride in human plasma by high performance liquid chromatography-ultraviolet detection.

Science.gov (United States)

Pashaei, Yaser; Ghorbani-Bidkorbeh, Fatemeh; Shekarchi, Maryam

2017-05-26

In the present study, superparamagnetic graphene oxide-Fe 3 O 4 nanocomposites were successfully prepared by a modified impregnation method (MGO mi ) and their application as a sorbent in the magnetic-dispersive solid phase extraction (M-dSPE) mode to the preconcentration and determination of tamsulosin hydrochloride (TMS) in human plasma was investigated by coupling with high performance liquid chromatography-ultraviolet detection (HPLC-UV). The structure, morphology and magnetic properties of the prepared nanocomposites were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and vibrating sample magnetometry (VSM). Some factors affecting the extraction efficiency, including the pH value, amount of sorbent, extraction time, elution solvent and its volume, and desorption time were studied and optimized. Magnetic nanocomposites plasma extraction of TMS following HPLC analyses showed a linear calibration curve in the range of 0.5-50.0ngmL -1 with an acceptable correlation coefficient (R 2 =0.9988). The method was sensitive, with a low limit of detection (0.17ngmL -1 ) and quantification (0.48ngmL -1 ). Inter- and intra-day precision expressed as relative standard deviation (n=3) and the preconcentration factor, were found to be 5.6-7.2%, 2.9-4.2% and 10, respectively. Good recoveries (98.1-101.4%) with low relative standard deviations (4.2-5.0%) indicated that the matrices under consideration do not significantly affect the extraction process. Due to its high precision and accuracy, the developed method may be a HPLC-UV alternative with M-dSPE for bioequivalence analysis of TMS in human plasma. Copyright © 2017 Elsevier B.V. All rights reserved.

Membranes as separators of dispersed emulsion phases

NARCIS (Netherlands)

Lefferts, A.G.

1997-01-01

The reuse or discharge of industrial waste waters, containing small fractions of dispersed oil, requires a purification treatment for which membranes can be used. If only little oil is present, removal of the dispersed phase might be preferable to the more commonly applied removal of the

Development of a novel mixed hemimicelles dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene for the separation and preconcentration of fluoxetine in different matrices before its determination by fiber optic linear array spectrophotometry and mode-mismatched thermal lens spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Kazemi, Elahe; Haji Shabani, Ali Mohammad [Department of Chemistry, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of); Dadfarnia, Shayessteh, E-mail: sdadfarnia@yazd.ac.ir [Department of Chemistry, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of); Abbasi, Amir [Department of Physics, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of); Rashidian Vaziri, Mohammad Reza [Laser and Optics Research School, 14155-1339, Tehran (Iran, Islamic Republic of); Behjat, Abbas [Department of Physics, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of)

2016-01-28

This study aims at developing a novel, sensitive, fast, simple and convenient method for separation and preconcentration of trace amounts of fluoxetine before its spectrophotometric determination. The method is based on combination of magnetic mixed hemimicelles solid phase extraction and dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene as a sorbent. The magnetic graphene was synthesized by a simple coprecipitation method and characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). The retained analyte was eluted using a 100 μL mixture of methanol/acetic acid (9:1) and converted into fluoxetine-β-cyclodextrin inclusion complex. The analyte was then quantified by fiber optic linear array spectrophotometry as well as mode-mismatched thermal lens spectroscopy (TLS). The factors affecting the separation, preconcentration and determination of fluoxetine were investigated and optimized. With a 50 mL sample and under optimized conditions using the spectrophotometry technique, the method exhibited a linear dynamic range of 0.4–60.0 μg L{sup −1}, a detection limit of 0.21 μg L{sup −1}, an enrichment factor of 167, and a relative standard deviation of 2.1% and 3.8% (n = 6) at 60 μg L{sup −1} level of fluoxetine for intra- and inter-day analyses, respectively. However, with thermal lens spectrometry and a sample volume of 10 mL, the method exhibited a linear dynamic range of 0.05–300 μg L{sup −1}, a detection limit of 0.016 μg L{sup −1} and a relative standard deviation of 3.8% and 5.6% (n = 6) at 60 μg L{sup −1} level of fluoxetine for intra- and inter-day analyses, respectively. The method was successfully applied to determine fluoxetine in pharmaceutical formulation, human urine and environmental water samples. - Graphical abstract: A novel, sensitive, fast, simple and convenient mixed hemimicelles

Development of a novel mixed hemimicelles dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene for the separation and preconcentration of fluoxetine in different matrices before its determination by fiber optic linear array spectrophotometry and mode-mismatched thermal lens spectroscopy

International Nuclear Information System (INIS)

Kazemi, Elahe; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh; Abbasi, Amir; Rashidian Vaziri, Mohammad Reza; Behjat, Abbas

2016-01-01

This study aims at developing a novel, sensitive, fast, simple and convenient method for separation and preconcentration of trace amounts of fluoxetine before its spectrophotometric determination. The method is based on combination of magnetic mixed hemimicelles solid phase extraction and dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene as a sorbent. The magnetic graphene was synthesized by a simple coprecipitation method and characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). The retained analyte was eluted using a 100 μL mixture of methanol/acetic acid (9:1) and converted into fluoxetine-β-cyclodextrin inclusion complex. The analyte was then quantified by fiber optic linear array spectrophotometry as well as mode-mismatched thermal lens spectroscopy (TLS). The factors affecting the separation, preconcentration and determination of fluoxetine were investigated and optimized. With a 50 mL sample and under optimized conditions using the spectrophotometry technique, the method exhibited a linear dynamic range of 0.4–60.0 μg L"−"1, a detection limit of 0.21 μg L"−"1, an enrichment factor of 167, and a relative standard deviation of 2.1% and 3.8% (n = 6) at 60 μg L"−"1 level of fluoxetine for intra- and inter-day analyses, respectively. However, with thermal lens spectrometry and a sample volume of 10 mL, the method exhibited a linear dynamic range of 0.05–300 μg L"−"1, a detection limit of 0.016 μg L"−"1 and a relative standard deviation of 3.8% and 5.6% (n = 6) at 60 μg L"−"1 level of fluoxetine for intra- and inter-day analyses, respectively. The method was successfully applied to determine fluoxetine in pharmaceutical formulation, human urine and environmental water samples. - Graphical abstract: A novel, sensitive, fast, simple and convenient mixed hemimicelles dispersive micro solid

Microencapsulated Comb-Like Polymeric Solid-Solid Phase Change Materials via In-Situ Polymerization

Directory of Open Access Journals (Sweden)

Wei Li

2018-02-01

Full Text Available To enhance the thermal stability and permeability resistance, a comb-like polymer with crystallizable side chains was fabricated as solid-solid phase change materials (PCMs inside the cores of microcapsules and nanocapsules prepared via in-situ polymerization. In this study, the effects on the surface morphology and microstructure of micro/nanocapsules caused by microencapsulating different types of core materials (i.e., n-hexadecane, ethyl hexadecanoate, hexadecyl acrylate and poly(hexadecyl acrylate were systematically studied via field emission scanning electron microscope (FE-SEM and transmission electron microscope (TEM. The confined crystallization behavior of comb-like polymer PCMs cores was investigated via differential scanning calorimeter (DSC. Comparing with low molecular organic PCMs cores, the thermal stability of PCMs microencapsulated comb-like polymer enhanced significantly, and the permeability resistance improved obviously as well. Based on these resultant analysis, the microencapsulated comb-like polymeric PCMs with excellent thermal stability and permeability resistance showed promising foreground in the field of organic solution spun, melt processing and organic coating.

Probing the liquid and solid phases in closely spaced two-dimensional systems

Energy Technology Data Exchange (ETDEWEB)

Zhang, Ding

2014-03-06

Gas, liquid and solid phases are the most common states of matter in our daily encountered 3-dimensional space. The school example is the H{sub 2}O molecule with its phases vapor, water and ice. Interestingly, electrons - with their point-like nature and negative charges - can also organize themselves under certain conditions to bear properties of these three common phases. At relatively high temperature, where Boltzmann statistics prevails, the ensemble of electrons without interactions can be treated as a gas of free particles. Cooling down the system, this electron gas condenses into a Fermi liquid. Finally, as a result of the repulsive Coulomb forces, electrons try to avoid each other by maximizing their distances. When the Coulomb interaction becomes sufficiently strong, a regular lattice emerges - an electron solid. The story however does not end here. Nature has much more in store for us. Electronic systems in fact exhibit a large variety of phases induced by spatial confinement, an external magnetic field, Coulomb interactions, or interactions involving degrees of freedom other than charge such as spin and valley. Here in this thesis, we restrict ourselves to the study of electrons in a 2-dimenisonal (2D) plane. Already in such a 2D electron system (2DES), several distinct states of matter appear: integer and fractional quantum Hall liquids, the 2D Wigner solid, stripe and bubble phases etc. In 2DES it is sufficient to sweep the perpendicular magnetic field to pass from one of these phases into another. Experimentally, many of these phases can be revealed by simply measuring the resistance. For a quantum Hall state, the longitudinal resistance vanishes, while the Hall resistance exhibits a plateau. The quantum Hall plateau is a manifestation of localization induced by the inevitable sample disorder. Coulomb interaction can also play an important role to localize charges. Even in the disorder-free case, electrons - more precisely quasi-particles in the

Probing the liquid and solid phases in closely spaced two-dimensional systems

International Nuclear Information System (INIS)

Zhang, Ding

2014-01-01

Gas, liquid and solid phases are the most common states of matter in our daily encountered 3-dimensional space. The school example is the H 2 O molecule with its phases vapor, water and ice. Interestingly, electrons - with their point-like nature and negative charges - can also organize themselves under certain conditions to bear properties of these three common phases. At relatively high temperature, where Boltzmann statistics prevails, the ensemble of electrons without interactions can be treated as a gas of free particles. Cooling down the system, this electron gas condenses into a Fermi liquid. Finally, as a result of the repulsive Coulomb forces, electrons try to avoid each other by maximizing their distances. When the Coulomb interaction becomes sufficiently strong, a regular lattice emerges - an electron solid. The story however does not end here. Nature has much more in store for us. Electronic systems in fact exhibit a large variety of phases induced by spatial confinement, an external magnetic field, Coulomb interactions, or interactions involving degrees of freedom other than charge such as spin and valley. Here in this thesis, we restrict ourselves to the study of electrons in a 2-dimenisonal (2D) plane. Already in such a 2D electron system (2DES), several distinct states of matter appear: integer and fractional quantum Hall liquids, the 2D Wigner solid, stripe and bubble phases etc. In 2DES it is sufficient to sweep the perpendicular magnetic field to pass from one of these phases into another. Experimentally, many of these phases can be revealed by simply measuring the resistance. For a quantum Hall state, the longitudinal resistance vanishes, while the Hall resistance exhibits a plateau. The quantum Hall plateau is a manifestation of localization induced by the inevitable sample disorder. Coulomb interaction can also play an important role to localize charges. Even in the disorder-free case, electrons - more precisely quasi-particles in the partially

Development of a Laser Dopper Anemometer technique for the measurement of two phase dispersed flow

International Nuclear Information System (INIS)

Srinivasan, J.

1978-05-01

A new optical technique using Laser-Doppler Anemometry is presented for the measurement of the local number densities and two-dimensional velocity probability densities of a turbulent dilute two-phase dispersion which has a distribution of particle size and a predominant direction of flow. This technique establishes that by a suitable scheme of discrimination on the signal amplitude, residence time and frequency of the Doppler signals caused by the scattered light from individual particles in the probing volume, the size distribution of moderately large particles in a dilute dispersed flow can be determined. The newly developed Laser-Doppler Anemometer (LDA) technique was applied to a solid particle-water two-phase flow and a water droplet-air two-phase flow. Particular emphasis was placed on turbulent two-phase water droplet-air flow inside a vertical rectangular channel. At each of nine different measuring locations along the transverse axis (starting at 250μ from the channel wall), over 20,000 Doppler signals were individually examined. The particle size and number density distributions, and the axial and lateral velocity distributions of both phases are reported. The analysis reveals some interesting features of two-phase dispersed flow. A film of water on the channel wall was formed due to the deposition of droplets from the flow. The water droplet entrainment from the wall film and the subsequent breakup of some of these into the flow are discussed. A discussion of the relationship between the particle distributions and turbulent flow characteristics is presented

Taurine zinc solid dispersions attenuate doxorubicin-induced hepatotoxicity and cardiotoxicity in rats.

Science.gov (United States)

Wang, Yu; Mei, Xueting; Yuan, Jingquan; Lu, Wenping; Li, Binglong; Xu, Donghui

2015-11-15

The clinical efficacy of anthracycline anti-neoplastic agents is limited by cardiac and hepatic toxicities. The aim of this study was to assess the hepatoprotective and cardioprotective effects of taurine zinc solid dispersions, which is a newly-synthesized taurine zinc compound, against doxorubicin-induced toxicity in Sprague-Dawley rats intraperitoneally injected with doxorubicin hydrochloride (3mg/kg) three times a week (seven injections) over 28 days. Hemodynamic parameters, levels of liver toxicity markers and oxidative stress were assessed. Taurine zinc significantly attenuated the reductions in blood pressure, left ventricular pressure and ± dp/dtmax, increases in serum alanine aminotransferase and aspartate aminotransferase activities, and reductions in serum Zn(2+) and albumin levels (Ptaurine zinc dose-dependently increased liver superoxide dismutase activity and glutathione concentration, and decreased malondialdehyde level (PTaurine zinc dose-dependently increased liver heme oxygenase-1 and UDP-glucuronyl transferase mRNA and protein expression (Ptaurine zinc inhibited c-Jun N-terminal kinase phosphorylation by upregulating dual-specificity phosphoprotein phosphatase-1. Additionally, taurine zinc inhibited cardiomyocyte apoptosis as there was decreased TUNEL/DAPI positivity and protein expression of caspase-3. These results indicate that taurine zinc solid dispersions prevent the side-effects of anthracycline-based anticancer therapy. The mechanisms might be associated with the enhancement of antioxidant defense system partly through activating transcription to synthesize endogenous phase II medicine enzymes and anti-apoptosis through inhibiting JNK phosphorylation. Copyright © 2015 Elsevier Inc. All rights reserved.

Interaction of dispersed cubic phases with blood components

DEFF Research Database (Denmark)

Bode, J C; Kuntsche, Judith; Funari, S S

2013-01-01

The interaction of aqueous nanoparticle dispersions, e.g. based on monoolein/poloxamer 407, with blood components is an important topic concerning especially the parenteral way of administration. Therefore, the influence of human and porcine plasma on dispersed cubic phases was investigated. Part...... activity of cubic phases based on monoolein and poloxamer 188, on soy phosphatidylcholine, glycerol dioleate and polysorbate 80 or the parenteral fat emulsion Lipofundin MCT 20%....

Enhancement of solubility and bioavailability of ambrisentan by solid dispersion using Daucus carota as a drug carrier: formulation, characterization, in vitro, and in vivo study.

Science.gov (United States)

Deshmane, Subhash; Deshmane, Snehal; Shelke, Santosh; Biyani, Kailash

2018-06-01

Ambrisentan is an US FDA approved drug, it is the second oral endothelin A receptor antagonist known for the treatment of pulmonary arterial hypertension, but its oral administration is limited due to its poor water solubility. Hence, the objective of the investigation was focused on enhancement of solubility and bioavailability of ambrisentan by solid dispersion technique using natural Daucus carota extract as drug carrier. Drug carrier was evaluated for solubility, swelling index, viscosity, angle of repose, hydration capacity, and acute toxicity test (LD 50 ). Ambrisentan was studied for the saturation solubility, phase solubility, and Gibbs free energy change. Compatibility of drug and the natural carrier was confirmed by DSC, FTIR, and XRD. Solid dispersions were evaluated for drug content, solubility, morphology, in vitro, and in vivo study. Screening of the natural carrier showed the desirable properties like water solubility, less swelling index, less viscosity, and acute toxicity study revealed no any clinical symptoms of toxicity. Drug and carrier interaction study confirmed the compatibility to consider its use in the formulation. Formed particles were found to be spherical with smooth surface. In vitro studies revealed higher drug release from the solid dispersion than that of the physical mixture. Bioavailability study confirms the increased absorption and bioavailability by oral administration of solid dispersion. Hence, it can be concluded that the natural Daucus carota extract can be the better alternative source for the preparation of solid dispersion and/or other dosage forms for improving solubility and bioavailability.

Magnetic nanoparticles-nylon 6 composite for the dispersive micro solid phase extraction of selected polycyclic aromatic hydrocarbons from water samples.

Science.gov (United States)

Reyes-Gallardo, Emilia M; Lucena, R; Cárdenas, S; Valcárcel, M

2014-06-06

In this article, the easy synthesis of magnetic nanoparticles-nylon 6 composite is presented, characterized and applied in the microextraction field. The one-step synthesis of the composite is performed by a solvent changeover playing with the different solubility of the polymeric network in formic acid and water. The new material has been characterized by different techniques including infrared spectroscopy, transmission and scanning microscopy. The extraction performance of the composite under a dispersive micro solid phase extraction format has been evaluated by determining four polycyclic aromatic hydrocarbons (benzo[b]fluoranthene, fluoranthene, indeno[1,2,3-cd]pyrene and phenanthrene) in water using ultra performance liquid chromatography (UPLC) combined with photo diode array detection. The developed methodology allows the determination of the analytes with limits of detection in the range from 0.05 μg/L (benzo[b]fluoranthene) to 0.58 μg/L (phenanthrene). The repeatability of the method was better than 6.9% at the limit of quantification level. The relative recoveries varied in the interval 80-111%. Copyright © 2014 Elsevier B.V. All rights reserved.

Investigation into mixing capability and solid dispersion preparation using the DSM Xplore Pharma Micro Extruder.

Science.gov (United States)

Sakai, Toshiro; Thommes, Markus

2014-02-01

The goal of this investigation was to qualify the DSM Xplore Pharma Micro Extruder as a formulation screening tool for early-stage hot-melt extrusion. Dispersive and distributive mixing was investigated using soluplus, copovidone or basic butylated methacrylate copolymer with sodium chloride (NaCl) in a batch size of 5 g. Eleven types of solid dispersions were prepared using various drugs and carriers in batches of 5 g in accordance with the literature. The dispersive mixing was a function of screw speed and recirculation time and the particle size was remarkably reduced after 1 min of processing, regardless of the polymers. An inverse relationship between the particle size and specific mechanical energy (SME) was also found. The SME values were higher than those in large-scale extruders. After 1 min recirculation at 200 rpm, the uniformity of NaCl content met the criteria of the European Pharmacopoeia, indicating that distributive mixing was achieved in this time. For the solid dispersions preparations, the results from different scanning calorimetry, powder X-ray diffractometry and in-vitro dissolution tests confirmed that all solid-dispersion systems were successfully prepared. These findings demonstrated that the extruder is a useful tool to screen solid-dispersion formulations and their material properties on a small scale. © 2013 Royal Pharmaceutical Society.

Characterization of gliclazide-polyethylene glycol solid dispersion and its effect on dissolution

Directory of Open Access Journals (Sweden)

Moreshwar Pandharinath Patil

2011-03-01

Full Text Available The present study was initiated with the objective of studying the in vitro dissolution behavior of gliclazide from its solid dispersion with polyethylene glycol 6000. In this work, a solid dispersion of gliclazide with polyethylene glycol was prepared by the fusion method. In vitro dissolution study of gliclazide, its physical mixture and solid dispersion were carried out to demonstrate the effect of PEG 6000. Analytical techniques of FT-IR spectroscopy, differential scanning calorimetry and X-ray diffractometry were used to characterize the drug in the physical mixtures and solid dispersions. The dissolution studies of solid dispersion and physical mixture showed greater improvement compared to that of the pure drug. The mechanisms for increased dissolution rate may include reduction of crystallite size, a solubilization effect of the carrier, absence of aggregation of drug crystallites, improved wettability and dispersbility of the drug from the dispersion, dissolution of the drug in the hydrophilic carrier or conversion of drug to an amorphous state. The FT-IR spectra suggested that there was no interaction between gliclazide and PEG 6000 when prepared as a solid dispersion. DSC and XRD study indicated that the drug was converted in the amorphous form.O presente trabalho foi realizado com o objetivo de estudar o comportamento in vitro da dissolução da gliclazida a partir da sua dispersão sólida com polietileno glicol 6000. Neste trabalho, as dispersões sólidas de gliclazida com polietileno glicol foram preparadas pelo método de fusão. Os estudo de dissolução in vitro da gliclazida, na mistura física e nas dispersões sólidas foram realizados para demonstrar o efeito de PEG 6000. Técnicas analíticas como espectroscopia FT-IR, calorimetria diferencial de varredura e difração de raios-X foram empregadas para caracterizar o fármaco nas misturas físicas e nas dispersoes sólidas. Os estudos de dissolução demonstraram maior

Jet noise reduction via dispersed phase injection

Science.gov (United States)

Greska, Brent; Krothapalli, Anjaneyulu; Arakeri, Vijay

2001-11-01

A recently developed hot jet aeroacoustics facility at FMRL,FAMU-FSU College of Engineering has been used to study the far field noise characteristics of hot supersonic jets as influenced by the injection of a dispersed phase with low mass loading.The measured SPL from a fully expanded Mach 1.36 hot jet shows a peak value of about 139 dB at 40 deg from the jet axis.By injecting atomized water,the SPL are reduced in the angular region of about 30 deg to 50 deg with the maximum reduction being about 2 dB at 40 deg.However,with the use of non atomized aqueous polymer solution as a dispersed phase the noise levels are reduced over all angular positions by at least 1 dB with the maximum reduction being about 3 dB at 40 deg.The injection of a dispersed phase readily kills the screech; the initial results show promise and optimization studies are underway to find methods of further noise reduction.

Computational design and fabrication of core-shell magnetic molecularly imprinted polymer for dispersive micro-solid-phase extraction coupled with high-performance liquid chromatography for the determination of rhodamine 6G.

Science.gov (United States)

Xie, Jin; Xie, Jie; Deng, Jian; Fang, Xiangfang; Zhao, Haiqing; Qian, Duo; Wang, Hongjuan

2016-06-01

A novel core-shell magnetic nano-adsorbent with surface molecularly imprinted polymer coating was fabricated and then applied to dispersive micro-solid-phase extraction followed by determination of rhodamine 6G using high-performance liquid chromatography. The molecularly imprinted polymer coating was prepared by copolymerization of dopamine and m-aminophenylboronic acid (functional monomers), in the presence of rhodamine 6G (template). The selection of the suitable functional monomers was based on the interaction between different monomers and the template using the density functional theory. The ratios of the monomers to template were further optimized by an OA9 (3(4) ) orthogonal array design. The binding performances of the adsorbent were evaluated by static, kinetic, and selective adsorption experiments. The results reveal that the adsorbent possesses remarkable affinity and binding specificity for rhodamine 6G because of the enhanced Lewis acid-base interaction between the B(Ш) embedded in the imprinted cavities and the template. The nano-adsorbent was successfully applied to dispersive micro-solid-phase extraction coupled to high-performance liquid chromatography for the trace determination of rhodamine 6G in samples with a detection limit of 2.7 nmol/L. Spiked recoveries ranged from 93.0-99.1, 89.5-92.7, and 86.9-105% in river water, matrimony vine and paprika samples, respectively, with relative standard deviations of less than 4.3%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid-phase peptide synthesis

DEFF Research Database (Denmark)

Jensen, Knud Jørgen

2013-01-01

This chapter provides an introduction to and overview of peptide chemistry with a focus on solid-phase peptide synthesis. The background, the most common reagents, and some mechanisms are presented. This chapter also points to the different chapters and puts them into perspective.......This chapter provides an introduction to and overview of peptide chemistry with a focus on solid-phase peptide synthesis. The background, the most common reagents, and some mechanisms are presented. This chapter also points to the different chapters and puts them into perspective....

Electron transfer reactions in microporous solids

Energy Technology Data Exchange (ETDEWEB)

Mallouk, T.E.

1993-01-01

Basic thrust the research program involves use of microporous solids (zeolites, clays, layered and tunnel structure oxide semiconductors) as organizing media for artificial photosynthetic systems. Purpose of the microporous solid is twofold. First, it induces spatial organization of photoactive and electroactive components (sensitizers, semiconductor particles, electron relays, and catalysts) at the solid-solution interface, enhancing the quantum efficiency of charge separation and separating physically the ultimate electron donor and acceptor in the electron transport chain. Second, since the microcrystalline solid admits only molecules of a certain charge and size, it is possible to achieve permanent charge separation by sieving chemical photoproducts (e.g., H[sub 2] and I[sub 3][sup [minus

Recent progress in predicting structural and electronic properties of organic solids with the van der Waals density functional

Energy Technology Data Exchange (ETDEWEB)

Yanagisawa, Susumu, E-mail: shou@sci.u-ryukyu.ac.jp [Department of Physics and Earth Sciences, Faculty of Science, University of the Ryukyus, 1 Senbaru, Nishihara, Okinawa 903-0213 (Japan); Okuma, Koji; Inaoka, Takeshi [Department of Physics and Earth Sciences, Faculty of Science, University of the Ryukyus, 1 Senbaru, Nishihara, Okinawa 903-0213 (Japan); Hamada, Ikutaro, E-mail: Hamada.Ikutaro@nims.go.jp [International Center for Materials Nanoarchitectonics (MANA), National Institute for Materials Science (NIMS), Tsukuba 305-0044 (Japan)

2015-10-01

Highlights: • Review of theoretical studies on organic solids with the density-functional methods. • van der Waals (vdW)-inclusive methods to predict cohesive properties of oligoacenes. • A variant of the vdW density functional describes the structures accurately. • The molecular configuration and conformation crucially affects the band dispersion. - Abstract: We review recent studies on electronic properties of the organic solids with the first-principles electronic structure methods, with the emphasis on the roles of the intermolecular van der Waals (vdW) interaction in electronic properties of the organic semiconductors. After a brief summary of the recent vdW inclusive first-principle theoretical methods, we discuss their performance in predicting cohesive properties of oligoacene crystals as examples of organic crystals. We show that a variant of the van der Waals density functional describes structure and energetics of organic crystals accurately. In addition, we review our recent study on the zinc phthalocyanine crystal and discuss the importance of the intermolecular distance and orientational angle in the band dispersion. Finally, we draw some general conclusions and the future perspectives.

Recent progress in predicting structural and electronic properties of organic solids with the van der Waals density functional

International Nuclear Information System (INIS)

Yanagisawa, Susumu; Okuma, Koji; Inaoka, Takeshi; Hamada, Ikutaro

2015-01-01

Highlights: • Review of theoretical studies on organic solids with the density-functional methods. • van der Waals (vdW)-inclusive methods to predict cohesive properties of oligoacenes. • A variant of the vdW density functional describes the structures accurately. • The molecular configuration and conformation crucially affects the band dispersion. - Abstract: We review recent studies on electronic properties of the organic solids with the first-principles electronic structure methods, with the emphasis on the roles of the intermolecular van der Waals (vdW) interaction in electronic properties of the organic semiconductors. After a brief summary of the recent vdW inclusive first-principle theoretical methods, we discuss their performance in predicting cohesive properties of oligoacene crystals as examples of organic crystals. We show that a variant of the van der Waals density functional describes structure and energetics of organic crystals accurately. In addition, we review our recent study on the zinc phthalocyanine crystal and discuss the importance of the intermolecular distance and orientational angle in the band dispersion. Finally, we draw some general conclusions and the future perspectives.

Enhancement of solubility and oral bioavailability of manidipine by formation of ternary solid dispersion with d-α-tocopherol polyethylene glycol 1000 succinate and copovidone.

Science.gov (United States)

Chamsai, Benchawan; Limmatvapirat, Sontaya; Sungthongjeen, Srisagul; Sriamornsak, Pornsak

2017-12-01

Low bioavailability of oral manidipine (MDP) is due to its low water solubility. The objective of this study was to increase the solubility and bioavailability of MDP by fabricating ternary solid dispersion (tSD) with d-α-tocopherol polyethyleneglycol-1000-succinate and copovidone. In this study, solid ternary phase diagram was applied in order to check the homogeneity of tSD prepared by melting and solidifying with dry ice. The physicochemical properties of different formulations were determined by differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR) and hot stage microscopy. Their solubility, dissolution, stability and bioavailability were also investigated. The results demonstrated that tSD obtained from ternary phase diagram divided into homogeneous and non-homogeneous regions. In the homogenous region, the transparent characteristics of tSD was observed and considered as a glass solution, which have a higher MDP solubility than that in non-homogenous region. The hot stage microscopy, DSC and PXRD confirmed that solid dispersion was formed in which MDP was molecularly dispersed in the carriers, especially in the homogenous region of phase diagram. FTIR analysis demonstrated strong hydrogen bonding between amine groups of MDP and carbonyl groups of copovidone, which supported a higher solubility and dissolution of tSD. The pharmacokinetic study in Wistar rats showed that the tSD had the greatest effect on oral bioavailability. Immediate hypotensive effect of tSD was also observed in vivo. The improvement of stability, dissolution and oral bioavailability of MDP could be achieved by using tSD technique.

Preparation and characterization of a novel polymeric based solid-solid phase change heat storage material

International Nuclear Information System (INIS)

Xi Peng; Gu Xiaohua; Cheng Bowen; Wang Yufei

2009-01-01

Here we reported a two-step procedure for preparing a novel polymeric based solid-solid phase change heat storage material. Firstly, a copolymer monomer containing a polyethylene glycol monomethyl ether (MPEG) phase change unit and a vinyl unit was synthesized via the modification of hydrogen group of MPEG. Secondly, by copolymerization of the copolymer monomer and phenyl ethylene, a novel polymeric based solid-solid phase change heat storage material was prepared. The composition, structure and properties of the novel polymeric based solid-solid phase change material were characterized by IR, 1 H NMR, DSC, WAXD, and POM, respectively. The results show that the novel polymeric based solid-solid phase change material possesses of excellent crystal properties and high phase change enthalpy.

Generation of high harmonic free electron laser with phase-merging effect

Energy Technology Data Exchange (ETDEWEB)

Li, Heting, E-mail: liheting@ustc.edu.cn; Jia, Qika; Zhao, Zhouyu

2017-03-01

An easy-to-implement scheme is proposed to produce the longitudinal electron bunch density modulation with phase-merging phenomenon. In this scheme an electron bunch is firstly transversely dispersed in a modified dogleg to generate the exact dependence of electron energy on the transverse position, then it is modulated in a normal modulator. After travelling through a modified chicane with specially designed transfer matrix elements, the density modulation with phase-merging effect is generated which contains high harmonic components of the seed laser. We present theoretical analysis and numerical simulations for seeded soft x-ray free-electron laser. The results demonstrate that this technique can significantly enhance the frequency up-conversion efficiency and allow a seeded FEL operating at very high harmonics.

Quantum phase transitions of strongly correlated electron systems

International Nuclear Information System (INIS)

Imada, Masatoshi

1998-01-01

Interacting electrons in solids undergo various quantum phase transitions driven by quantum fluctuations. The quantum transitions take place at zero temperature by changing a parameter to control quantum fluctuations rather than thermal fluctuations. In contrast to classical phase transitions driven by thermal fluctuations, the quantum transitions have many different features where quantum dynamics introduces a source of intrinsic fluctuations tightly connected with spatial correlations and they have been a subject of recent intensive studies as we see below. Interacting electron systems cannot be fully understood without deep analyses of the quantum phase transitions themselves, because they are widely seen and play essential roles in many phenomena. Typical and important examples of the quantum phase transitions include metal-insulator transitions, (2, 3, 4, 5, 6, 7, 8, 9) metal-superconductor transitions, superconductor-insulator transitions, magnetic transitions to antiferromagnetic or ferromagnetic phases in metals as well as in Mott insulators, and charge ordering transitions. Here, we focus on three different types of transitions

Molecularly Imprinted Nanomicrospheres as Matrix Solid-Phase Dispersant Combined with Gas Chromatography for Determination of Four Phosphorothioate Pesticides in Carrot and Yacon

Directory of Open Access Journals (Sweden)

Mengchun Zhou

2015-01-01

Full Text Available An efficient, rapid, and selective method for sample pretreatment, namely, molecularly imprinted matrix solid-phase dispersion (MI-MSPD coupled with gas chromatography (GC, was developed for the rapid isolation of four phosphorothioate organophosphorus pesticides (tolclofos-methyl, phoxim, chlorpyrifos, and parathion-methyl from carrot and yacon samples. New molecularly imprinted polymer nanomicrospheres were synthesized by using typical structural analogue tolclofos-methyl as a dummy template via surface grafting polymerization on nanosilica. Then, these four pesticides in carrot and yacon were extracted and adsorbed using the imprinted nanomicrospheres and further determined by gas chromatography. Under the optimized conditions, a good linearity of four pesticides was obtained in a range of 0.05–17.0 ng·g−1 with R varying from 0.9971 to 0.9996, and the detection limit of the method was 0.012~0.026 ng·g−1 in carrot and yacon samples. The recovery rates at two spiked levels were in the range of 85.4–105.6% with RSD ≤9.6%. The presented MI-MSPD method combined the advantages of MSPD for allowing the extraction, dispersion, and homogenization in two steps and the advantages of MIPs for high affinity and selectivity towards four phosphorothioate pesticides, which could be applied to the determination of pesticide residues in complicated vegetal samples.

High throughput screening of phenoxy carboxylic acids with dispersive solid phase extraction followed by direct analysis in real time mass spectrometry.

Science.gov (United States)

Wang, Jiaqin; Zhu, Jun; Si, Ling; Du, Qi; Li, Hongli; Bi, Wentao; Chen, David Da Yong

2017-12-15

A high throughput, low environmental impact methodology for rapid determination of phenoxy carboxylic acids (PCAs) in water samples was developed by combing dispersive solid phase extraction (DSPE) using velvet-like graphitic carbon nitride (V-g-C 3 N 4 ) and direct analysis in real time mass spectrometry (DART-MS). Due to the large surface area and good dispersity of V-g-C 3 N 4 , the DSPE of PCAs in water was completed within 20 s, and the elution of PCAs was accomplished in 20 s as well using methanol. The eluents were then analyzed and quantified using DART ionization source coupled to a high resolution mass spectrometer, where an internal standard was added in the samples. The limit of detection ranged from 0.5 ng L -1 to 2 ng L -1 on the basis of 50 mL water sample; the recovery 79.9-119.1%; and the relative standard deviation 0.23%-9.82% (≥5 replicates). With the ease of use and speed of DART-MS, the whole protocol can complete within mere minutes, including sample preparation, extraction, elution, detection and quantitation. The methodology developed here is simple, fast, sensitive, quantitative, requiring little sample preparation and consuming significantly less toxic organic solvent, which can be used for high throughput screening of PCAs and potentially other contaminants in water. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparison between dispersive solid-phase and dispersive liquid-liquid microextraction combined with spectrophotometric determination of malachite green in water samples based on ultrasound-assisted and preconcentration under multi-variable experimental design optimization.

Science.gov (United States)

Alipanahpour Dil, Ebrahim; Ghaedi, Mehrorang; Asfaram, Arash; Zare, Fahimeh; Mehrabi, Fatemeh; Sadeghfar, Fardin

2017-11-01

The ultrasound-assisted dispersive solid-phase microextraction (USA-DSPME) and the ultrasound-assisted dispersive liquid-liquid microextraction (USA-DLLME) developed for as an ultra preconcentration and/or technique for the determination of malachite green (MG) in water samples. Central composite design based on analysis of variance and desirability function guide finding best operational conditions and represent dependency of response to variables viz. volume of extraction, eluent and disperser solvent, pH, adsorbent mass and ultrasonication time has significant influence on methods efficiency. Optimum conditions was set for USA-DSPME as: 1mg CNTs/Zn:ZnO@Ni 2 P-NCs; 4min sonication time and 130μL eluent at pH 6.0. Meanwhile optimum point for USA-DLLME conditions were fixed at pH 6.0; 4min sonication time and 130, 650μL and 10mL of extraction solvent (CHCl 3 ), disperser solvent (ethanol) and sample volume, respectively. Under the above specified best operational conditions, the enrichment factors for the USA-DSPME and USA-DLLME were 88.89 and 147.30, respectively. The methods has linear response in the range of 20.0 to 4000.0ngmL -1 with the correlation coefficients (r) between 0.9980 to 0.9995, while its reasonable detection limits viz. 1.386 to 2.348ngmL -1 and good relative standard deviations varied from 1.1% to 2.8% (n=10) candidate this method for successful monitoring of analyte from various media. The relative recoveries of the MG dye from water samples at spiking level of 500ngmL -1 were in the range between 94.50% and 98.86%. The proposed methods has been successfully applied to the analysis of the MG dye in water samples, and a satisfactory result was obtained. Copyright © 2017. Published by Elsevier B.V.

Analytical electron microscope based on scanning transmission electron microscope with wavelength dispersive x-ray spectroscopy to realize highly sensitive elemental imaging especially for light elements

International Nuclear Information System (INIS)

Koguchi, Masanari; Tsuneta, Ruriko; Anan, Yoshihiro; Nakamae, Koji

2017-01-01

An analytical electron microscope based on the scanning transmission electron microscope with wavelength dispersive x-ray spectroscopy (STEM-WDX) to realize highly sensitive elemental imaging especially for light elements has been developed. In this study, a large-solid-angle multi-capillary x-rays lens with a focal length of 5 mm, long-time data acquisition (e.g. longer than 26 h), and a drift-free system made it possible to visualize boron-dopant images in a Si substrate at a detection limit of 0.2 atomic percent. (paper)

Graphene oxide decorated with silver nanoparticles as a coating on a stainless-steel fiber for solid-phase microextraction.

Science.gov (United States)

Wang, Licheng; Hou, Xiudan; Li, Jubai; Liu, Shujuan; Guo, Yong

2015-07-01

A novel graphene oxide decorated with silver nanoparticles coating on a stainless-steel fiber for solid-phase microextraction was prepared. Scanning electron microscopy and X-ray photoelectron spectroscopy were used to characterize the coating surface and showed that silver nanoparticles were dispersed on the wrinkled graphene oxide surface. Coupled to gas chromatography with flame ionization detection, the extraction abilities of the fiber for polycyclic aromatic hydrocarbons were examined in the headspace solid-phase microextraction mode. The extraction parameters including adsorption time, adsorption temperature, salt concentration, desorption time and desorption temperature were investigated. Under the optimized condition, wide linearity with low limits of detection from 2 to 10 ng/L was obtained. The relative standard deviations for single-fiber repeatability and fiber-to-fiber reproducibility were less than 10.6 and 17.5%, respectively. The enrichment factors were from 1712.5 to 4503.7, showing the fiber has good extraction abilities. Moreover, the fiber exhibited a good stability and could be reused for more than 120 times. The established method was also applied for determination of polycyclic aromatic hydrocarbons in two real water samples and the recoveries of analytes ranged from 84.4-116.3% with relative standard deviations less than 16.2%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The dissolution enhancement of piroxicam in its physical mixtures and solid dispersion formulations using gluconolactone and glucosamine hydrochloride as potential carriers.

Science.gov (United States)

Al-Hamidi, Hiba; Obeidat, Wasfy M; Nokhodchi, Ali

2015-01-01

The solid dispersion technique is one of the most effective methods for improving the dissolution rate of poorly water-soluble drugs; however this is reliant on a suitable carrier and solvent being selected. The work presented explores amino sugars (d-glucosamine HCl and d-gluconolactone) as potential hydrophilic carriers to improve dissolution rate of a poorly water-soluble drug, piroxicam, from physical mixtures and solid dispersion formulations. Solid dispersions of the drug and carrier were prepared using different ratios by the conventional solvent evaporation method. Acetone was used as solvent in the preparation of solid dispersions. Physical mixtures of piroxicam and carrier were also prepared for comparison. The properties of all solid dispersions and physical mixtures were studied using a dissolution tester, Fourier transform infrared, XRD, SEM and differential scanning calorimetry. These results showed that the presence of glucosamine or gluconolactone can increase dissolution rate of piroxicam compared to pure piroxicam. Glucosamine or Gluconolactone could be used as carrier in solid dispersion formulations and physical mixtures to enhance the dissolution rate. Solid state studies showed that no significant changes occurred for piroxicam in physical mixtures and solid dispersion.

Phase Modulation for postcompensation of dispersion in 160-Gb/s systems

DEFF Research Database (Denmark)

Siahlo, Andrei; Clausen, A. T.; Oxenløwe, Leif Katsuo

2005-01-01

Tunable postcompensation of second-order dispersion by sinusoidal phase modulation is realized for a 160-Gb/s optical transmission system. Accumulated dispersions with magnitudes up to 4 ps/nm are compensated in the receiver end.......Tunable postcompensation of second-order dispersion by sinusoidal phase modulation is realized for a 160-Gb/s optical transmission system. Accumulated dispersions with magnitudes up to 4 ps/nm are compensated in the receiver end....

Extending the random-phase approximation for electronic correlation energies: the renormalized adiabatic local density approximation

DEFF Research Database (Denmark)

Olsen, Thomas; Thygesen, Kristian S.

2012-01-01

The adiabatic connection fluctuation-dissipation theorem with the random phase approximation (RPA) has recently been applied with success to obtain correlation energies of a variety of chemical and solid state systems. The main merit of this approach is the improved description of dispersive forces...... while chemical bond strengths and absolute correlation energies are systematically underestimated. In this work we extend the RPA by including a parameter-free renormalized version of the adiabatic local-density (ALDA) exchange-correlation kernel. The renormalization consists of a (local) truncation...... of the ALDA kernel for wave vectors q > 2kF, which is found to yield excellent results for the homogeneous electron gas. In addition, the kernel significantly improves both the absolute correlation energies and atomization energies of small molecules over RPA and ALDA. The renormalization can...

Solid Phase Equilibrium Relations in the CaO-SiO2-Nb2O5-La2O3 System at 1273 K

Science.gov (United States)

Qiu, Jiyu; Liu, Chengjun

2018-02-01

Silicate slag system with additions Nb and RE formed in the utilization of REE-Nb-Fe ore deposit resources in China has industrial uses as a metallurgical slag system. The lack of a phase diagram, theoretical, and thermodynamic information for the multi-component system restrict the comprehensive utilization process. In the current work, solid phase equilibrium relations in the CaO-SiO2-Nb2O5-La2O3 quaternary system at 1273 K (1000 °C) were investigated experimentally by the high-temperature equilibrium experiment followed by X-ray diffraction, scanning electron microscope, and energy dispersive spectrometer. Six spatial independent tetrahedron fields in the CaO-SiO2-Nb2O5-La2O3 system phase diagram were determined by the Gibbs Phase Rule. The current work combines the mass fraction of equilibrium phase and corresponding geometric relation. A determinant method was deduced to calculate the mass fraction of equilibrium phase in quaternary system according to the Mass Conservation Law, the Gibbs Phase Rule, the Lever's Rule, and the Cramer Law.

Mechanism and microstructures in Ga2O3 pseudomartensitic solid phase transition.

Science.gov (United States)

Zhu, Sheng-Cai; Guan, Shu-Hui; Liu, Zhi-Pan

2016-07-21

Solid-to-solid phase transition, although widely exploited in making new materials, challenges persistently our current theory for predicting its complex kinetics and rich microstructures in transition. The Ga2O3α-β phase transformation represents such a common but complex reaction with marked change in cation coordination and crystal density, which was known to yield either amorphous or crystalline products under different synthetic conditions. Here we, via recently developed stochastic surface walking (SSW) method, resolve for the first time the atomistic mechanism of Ga2O3α-β phase transformation, the pathway of which turns out to be the first reaction pathway ever determined for a new type of diffusionless solid phase transition, namely, pseudomartensitic phase transition. We demonstrate that the sensitivity of product crystallinity is caused by its multi-step, multi-type reaction pathway, which bypasses seven intermediate phases and involves all types of elementary solid phase transition steps, i.e. the shearing of O layers (martensitic type), the local diffusion of Ga atoms (reconstructive type) and the significant lattice dilation (dilation type). While the migration of Ga atoms across the close-packed O layers is the rate-determining step and yields "amorphous-like" high energy intermediates, the shearing of O layers contributes to the formation of coherent biphase junctions and the presence of a crystallographic orientation relation, (001)α//(201[combining macron])β + [120]α//[13[combining macron]2]β. Our experiment using high-resolution transmission electron microscopy further confirms the theoretical predictions on the atomic structure of biphase junction and the formation of (201[combining macron])β twin, and also discovers the late occurrence of lattice expansion in the nascent β phase that grows out from the parent α phase. By distinguishing pseudomartensitic transition from other types of mechanisms, we propose general rules to predict the

Development and characterization of solid dispersion of piroxicam for improvement of dissolution rate using hydrophilic carriers

Directory of Open Access Journals (Sweden)

Mohammad Barzegar-jalali

2014-09-01

Full Text Available Introduction: The main objective of this study was preparation and characterization of solid dispersion of piroxicam to enhance its dissolution rate. Methods: Solid dispersion formulations with different carriers including crospovidone, microcrystalline cellulose and Elaeagnus angustifolia fruit powder and with different drug: carrier ratios were prepared employing cogrinding method. Dissolution study of the piroxicam powders, physical mixtures and solid dispersions was performed in simulated gastric fluid and simulated intestinal fluid using USP Apparatus type II. The physical characterization of formulations were analyzed using powder X ray diffraction (PXRD, particle size analyzer and differential scanning calorimetry (DSC. Interactions between the drug and carriers were evaluated by Fourier transform infrared (FT-IR spectroscopic method. Results: It was revealed that all of three carriers increase the dissolution rate of piroxicam from physical mixtures and especially in solid dispersions compared to piroxicam pure and treated powders. PXRD and DSC results were confirmed the reduction of crystalline form of piroxicam. FT-IR analysis did not show any physicochemical interaction between drug and carriers in the solid dispersion formulations. Conclusion: Dissolution rate was dependent on the type and ratio of drug: carrier as well as pH of dissolution medium. Dissolution data of formulations were fitted well in to the linear Weibull as well as non-linear logistic and a suggested models.

Dissolution-modulating mechanism of pH modifiers in solid dispersion containing weakly acidic or basic drugs with poor water solubility.

Science.gov (United States)

Tran, Phuong Ha-Lien; Tran, Thao Truong-Dinh; Lee, Kyoung-Ho; Kim, Dong-Jin; Lee, Beom-Jin

2010-05-01

Although the solid dispersion method has been known to increase the dissolution rate of poorly water-soluble drugs by dispersing them in hydrophilic carriers, one obstacle of the solid dispersion method is its limited solubilization capacity, especially for pH-dependent soluble drugs. pH-modified solid dispersion, in which pH modifiers are incorporated, may be a useful method for increasing the dissolution rate of weakly acidic or basic drugs. Sufficient research, including the most recent reports, was undertaken in this review. How could the inclusion of the pH the pH modifiers in the solid dispersion system change drug structural behaviors, molecular interactions, microenvironmental pH, and/or release rate of pH modifiers, relating with the enhanced dissolution of weakly acidic or weakly basic drugs with poor water solubility? These questions have been investigated to determine the dissolution-modulating mechanism of pH modifiers in solid dispersion containing weakly acidic or basic drugs. It is believed that step-by-step mechanistic approaches could provide the ultimate solution for solubilizing several poorly water-soluble drugs with pH-dependent solubility from a solid dispersion system, as well as provide ideas for developing future dosage systems.

Multiplexed Colorimetric Solid-Phase Extraction

Science.gov (United States)

Gazda, Daniel B.; Fritz, James S.; Porter, Marc D.

2009-01-01

Multiplexed colorimetric solid-phase extraction (MC-SPE) is an extension of colorimetric solid-phase extraction (C-SPE) an analytical platform that combines colorimetric reagents, solid phase extraction, and diffuse reflectance spectroscopy to quantify trace analytes in water. In CSPE, analytes are extracted and complexed on the surface of an extraction membrane impregnated with a colorimetric reagent. The analytes are then quantified directly on the membrane surface using a handheld diffuse reflectance spectrophotometer. Importantly, the use of solid-phase extraction membranes as the matrix for impregnation of the colorimetric reagents creates a concentration factor that enables the detection of low concentrations of analytes in small sample volumes. In extending C-SPE to a multiplexed format, a filter holder that incorporates discrete analysis channels and a jig that facilitates the concurrent operation of multiple sample syringes have been designed, enabling the simultaneous determination of multiple analytes. Separate, single analyte membranes, placed in a readout cartridge create unique, analyte-specific addresses at the exit of each channel. Following sample exposure, the diffuse reflectance spectrum of each address is collected serially and the Kubelka-Munk function is used to quantify each water quality parameter via calibration curves. In a demonstration, MC-SPE was used to measure the pH of a sample and quantitate Ag(I) and Ni(II).

Optimization of a method based on micro-matrix solid-phase dispersion (micro-MSPD for the determination of PCBs in mussel samples

Directory of Open Access Journals (Sweden)

Nieves Carro

2017-03-01

Full Text Available This paper reports the development and optimization of micro-matrix solid-phase dispersion (micro-MSPD of nine polychlorinated biphenyls (PCBs in mussel samples (Mytilus galloprovincialis by using a two-level factorial design. Four variables (amount of sample, anhydrous sodium sulphate, Florisil and solvent volume were considered as factors in the optimization process. The results suggested that only the interaction between the amount of anhydrous sodium sulphate and the solvent volume was statistically significant for the overall recovery of a trichlorinated compound, CB 28. Generally most of the considered species exhibited a similar behaviour, the sample and Florisil amounts had a positive effect on PCBs extractions and solvent volume and sulphate amount had a negative effect. The analytical determination and confirmation of PCBs were carried out by using GC-ECD and GC-MS/MS, respectively. The method was validated having satisfactory precision and accuracy with RSD values below 6% and recoveries between 81 and 116% for all congeners. The optimized method was applied to the extraction of real mussel samples from two Galician Rías.

Enhanced bioavailability of sirolimus via preparation of solid dispersion nanoparticles using a supercritical antisolvent process

Directory of Open Access Journals (Sweden)

Kim MS

2011-11-01

Full Text Available Min-Soo Kim1, Jeong-Soo Kim1, Hee Jun Park1, Won Kyung Cho1,3, Kwang-Ho Cha1,3, Sung-Joo Hwang2,31College of Pharmacy, Chungnam National University, Daejeon, Republic of Korea, 2College of Pharmacy, 3Yonsei Institute of Pharmaceutical Sciences, Yonsei University, Incheon, Republic of KoreaBackground: The aim of this study was to improve the physicochemical properties and bioavailability of poorly water-soluble sirolimus via preparation of a solid dispersion of nanoparticles using a supercritical antisolvent (SAS process.Methods: First, excipients for enhancing the stability and solubility of sirolimus were screened. Second, using the SAS process, solid dispersions of sirolimus-polyvinylpyrrolidone (PVP K30 nanoparticles were prepared with or without surfactants such as sodium lauryl sulfate (SLS, tocopheryl propylene glycol succinate, Sucroester 15, Gelucire 50/13, and Myrj 52. A mean particle size of approximately 250 nm was obtained for PVP K30-sirolimus nanoparticles. Solid state characterization, kinetic solubility, powder dissolution, stability, and pharmacokinetics were analyzed in rats.Results: X-ray diffraction, differential scanning calorimetry, and high-pressure liquid chromatography indicated that sirolimus existed in an anhydrous amorphous form within a solid dispersion of nanoparticles and that no degradation occurred after SAS processing. The improved supersaturation and dissolution of sirolimus as a solid dispersion of nanoparticles appeared to be well correlated with enhanced bioavailability of oral sirolimus in rats. With oral administration of a solid dispersion of PVP K30-SLS-sirolimus nanoparticles, the peak concentration and AUC0→12h of sirolimus were increased by approximately 18.3-fold and 15.2-fold, respectively.Conclusion: The results of this study suggest that preparation of PVP K30-sirolimus-surfactant nanoparticles using the SAS process may be a promising approach for improving the bioavailability of sirolimus

Density-functional theory for fluid-solid and solid-solid phase transitions.

Science.gov (United States)

Bharadwaj, Atul S; Singh, Yashwant

2017-03-01

We develop a theory to describe solid-solid phase transitions. The density functional formalism of classical statistical mechanics is used to find an exact expression for the difference in the grand thermodynamic potentials of the two coexisting phases. The expression involves both the symmetry conserving and the symmetry broken parts of the direct pair correlation function. The theory is used to calculate phase diagram of systems of soft spheres interacting via inverse power potentials u(r)=ε(σ/r)^{n}, where parameter n measures softness of the potential. We find that for 1/nfcc) structure while for 1/n≥0.154 the body-centred-cubic (bcc) structure is preferred. The bcc structure transforms into the fcc structure upon increasing the density. The calculated phase diagram is in good agreement with the one found from molecular simulations.

Electron stimulated reactions of methyl iodide coadsorbed with amorphous solid water

International Nuclear Information System (INIS)

Perry, C. C.; Faradzhev, N. S.; Madey, T. E.; Fairbrother, D. H.

2007-01-01

The electron stimulated reactions of methyl iodide (MeI) adsorbed on and suspended within amorphous solid water (ice) were studied using a combination of postirradiation temperature programmed desorption and reflection absorption infrared spectroscopy. For MeI adsorbed on top of amorphous solid water (ice), electron beam irradiation is responsible for both structural and chemical transformations within the overlayer. Electron stimulated reactions of MeI result principally in the formation of methyl radicals and solvated iodide anions. The cross section for electron stimulated decomposition of MeI is comparable to the gas phase value and is only weakly dependent upon the local environment. For both adsorbed MeI and suspended MeI, reactions of methyl radicals within MeI clusters lead to the formation of ethane, ethyl iodide, and diiodomethane. In contrast, reactions between the products of methyl iodide and water dissociation are responsible for the formation of methanol and carbon dioxide. Methane, formed as a result of reactions between methyl radicals and either parent MeI molecules or hydrogen atoms, is also observed. The product distribution is found to depend on the film's initial chemical composition as well as the electron fluence. Results from this study highlight the similarities in the carbon-containing products formed when monohalomethanes coadsorbed with amorphous solid water are irradiated by either electrons or photons

Encapsulation of solid dispersion in solid lipid particles for dissolution enhancement of poorly water-soluble drug.

Science.gov (United States)

Tran, Khanh Thi My; Vo, Toi Van; Tran, Phuong Ha-Lien; Lee, Beom-Jin; Duan, Wei; Tran, Thao Truong-Dinh

2017-06-05

The aim of this research was to engineer solid dispersion lipid particles (SD-SLs) in which a solid dispersion (SD) was encapsulated to form the core of solid lipid particles (SLs), thereby achieving an efficient enhancement in the dissolution of a poorly water-soluble drug. Ultrasonication was introduced into the process to obtain micro/nanoscale SLs. The mechanism of dissolution enhancement was investigated by analysing the crystalline structure, molecular interactions, and particle size of the formulations. The drug release from the SD-SLs was significantly greater than that from the SD or SLs alone. This enhancement in drug release was dependent on the preparation method and the drug-to-polymer ratio of the SD. With an appropriate amount of polymer in the SD, the solidification method had the potential to alter the drug crystallinity to an amorphous state, resulting in particle uniformity and molecular interactions in the SD-SLs. The proposed system provides a new strategy for enhancing the dissolution rate of poorly water-soluble drugs and further improving their bioavailability. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Long-wave equivalent viscoelastic solids for porous rocks saturated by two-phase fluids

Science.gov (United States)

Santos, J. E.; Savioli, G. B.

2018-04-01

Seismic waves traveling across fluid-saturated poroelastic materials with mesoscopic-scale heterogeneities induce fluid flow and Biot's slow waves generating energy loss and velocity dispersion. Using Biot's equations of motion to model these type of heterogeneities would require extremely fine meshes. We propose a numerical upscaling procedure to determine the complex and frequency dependent P-wave and shear moduli of an effective viscoelastic medium long-wave equivalent to a poroelastic solid saturated by a two-phase fluid. The two-phase fluid is defined in terms of capillary pressure and relative permeability flow functions. The P-wave and shear effective moduli are determined using harmonic compressibility and shear experiments applied on representative samples of the bulk material. Each experiment is associated with a boundary value problem that is solved using the finite element method. Since a poroelastic solid saturated by a two-phase fluid supports the existence of two slow waves, this upscaling procedure allows to analyze their effect on the mesoscopic-loss mechanism in hydrocarbon reservoir formations. Numerical results show that a two-phase Biot medium model predicts higher attenuation than classic Biot models.

First principles electronic band structure and phonon dispersion curves for zinc blend beryllium chalcogenide

Energy Technology Data Exchange (ETDEWEB)

Dabhi, Shweta, E-mail: venu.mankad@gmail.com; Mankad, Venu, E-mail: venu.mankad@gmail.com; Jha, Prafulla K., E-mail: venu.mankad@gmail.com [Department of Physics, Maharaja Krishnakumasinhji Bhavnagar University, Bhavnagar-364001 (India)

2014-04-24

A detailed theoretical study of structural, electronic and Vibrational properties of BeX compound is presented by performing ab-initio calculations based on density-functional theory using the Espresso package. The calculated value of lattice constant and bulk modulus are compared with the available experimental and other theoretical data and agree reasonably well. BeX (X = S,Se,Te) compounds in the ZB phase are indirect wide band gap semiconductors with an ionic contribution. The phonon dispersion curves are represented which shows that these compounds are dynamically stable in ZB phase.

Quantitative energy-dispersive electron probe X-ray microanalysis ...

Indian Academy of Sciences (India)

Abstract. An energy-dispersive electron probe X-ray microanalysis (ED-EPMA) technique us- ing an energy-dispersive X-ray detector with an ultra-thin window, designated as low-Z particle. EPMA, has been developed. The low-Z particle EPMA allows the quantitative determination of concentrations of low-Z elements such ...

Natural polymers: Best carriers for improving bioavailability of poorly water soluble drugs in solid dispersions

OpenAIRE

Sandip Sapkal; Mahesh Narkhede; Mukesh Babhulkar; Gautam Mehetre; Ashish Rathi

2013-01-01

ABSTRACTNatural polymers and its modified forms can be used as best alternative for improving bioavailabilityof poorly water soluble drugs in solid dispersion. Most of the natural polymersare hydrophilic and having high swelling capacity. Recent trend towards the use of naturalpolymer demands the replacement of synthetic additives with natural ones. Many plant derivednatural polymers are studied for use in solid dispersion systems, out of which naturalgums, cyclodextrin and carbohydrate are m...

Gas phase dispersion in a small rotary kiln

International Nuclear Information System (INIS)

Spencer, B.B.

1981-07-01

A study was made of nonideal flow of gas in a rotary kiln reactor. A rotating tube 0.165 m in diameter by 2.17 m long, with internal lifting flights, was operated at room temperature. Rotational speeds from 2.0 to 7.0 rpm, air flow rates from 0.351 to 4.178 m 3 /h, and solid contents of 0.0, 5.1, and 15.3% of tube volume were studied. Residence time distribution of the gas was measured by means of the pulse injection technique using a helium tracer. A model was developed based on dispersive flow that exchanges with a deadwater region. Two parameters, a dispersion number describing bulk gas flow and an interchange factor describing exchange between the flow region and the gas trapped in the solids bed, were sufficient to correlate the data, but these parameters are sensitive to experimental error. The model is applicable to analysis of other flow systems, such as packed beds

THE ROLE OF 4-HYDROXYPHENYLPYRUVATE DIOXYGENASE IN ENHANCEMENT OF SOLID-PHASE ELECTRON TRANSFER BY SHEWANELLA ONEIDENSIS MR-1

Energy Technology Data Exchange (ETDEWEB)

Turick, C; Amy Ekechukwu, A

2007-06-01

While mechanistic details of dissimilatory metal reduction are far from being understood, it is postulated that the electron transfer to solid metal oxides is mediated by outer membrane-associated c-type cytochromes and redox active electron shuttling compounds. This study focuses on the production of homogensitate in Shewanella oneidensis MR-1, an intermediate of tyrosine degradation pathway, which is a precursor of a redox cycling metabolite, pyomelanin. In this study, we determined that two enzymes involved in this pathway, 4-hydroxyphenylpyruvate dioxygenase (4HPPD) and homogentisate 1,2-dioxygenase are responsible for homogentisate production and oxidation, respectively. Inhibition of 4-HPPD activity with the specific inhibitor sulcotrione (2-(2-chloro-4-methane sulfonylbenzoyl)-1,3-cyclohexanedione), and deletion of melA, a gene encoding 4-HPPD, resulted in no pyomelanin production by S. oneidensis MR-1. Conversely, deletion of hmgA which encodes the putative homogentisate 1,2-dioxygenase, resulted in pyomelanin overproduction. The efficiency and rates, with which MR-1 reduces hydrous ferric oxide, were directly linked to the ability of mutant strains to produce pyomelanin. Electrochemical studies with whole cells demonstrated that pyomelanin substantially increases the formal potential (E{sup o}{prime}) of S. oneidensis MR-1. Based on this work, environmental production of pyomelanin likely contributes to an increased solid-phase metal reduction capacity in Shewanella oneidensis.

Investigating the effect of moisture protection on solid-state stability and dissolution of fenofibrate and ketoconazole solid dispersions using PXRD, HSDSC and Raman microscopy.

Science.gov (United States)

Kanaujia, Parijat; Lau, Grace; Ng, Wai Kiong; Widjaja, Effendi; Schreyer, Martin; Hanefeld, Andrea; Fischbach, Matthias; Saal, Christoph; Maio, Mario; Tan, Reginald B H

2011-09-01

Enhanced dissolution of poorly soluble active pharmaceutical ingredients (APIs) in amorphous solid dispersions often diminishes during storage due to moisture-induced re-crystallization. This study aims to investigate the influence of moisture protection on solid-state stability and dissolution profiles of melt-extruded fenofibrate (FF) and ketoconazole (KC) solid dispersions. Samples were kept in open, closed and Activ-vials(®) to control the moisture uptake under accelerated conditions. During 13-week storage, changes in API crystallinity were quantified using powder X-ray diffraction (PXRD) (Rietveld analysis) and high sensitivity differential scanning calorimetry (HSDSC) and compared with any change in dissolution profiles. Trace crystallinity was observed by Raman microscopy, which otherwise was undetected by PXRD and HSDSC. Results showed that while moisture protection was ineffective in preventing the re-crystallization of amorphous FF, KC remained X-ray amorphous despite 5% moisture uptake. Regardless of the degree of crystallinity increase in FF, the enhanced dissolution properties were similarly diminished. Moisture uptake above 10% in KC samples also led to re-crystallization and significant decrease in dissolution rates. In conclusion, eliminating moisture sorption may not be sufficient in ensuring the stability of solid dispersions. Analytical quantification of API crystallinity is crucial in detecting subtle increase in crystallinity that can diminish the enhanced dissolution properties of solid dispersions.

Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

Science.gov (United States)

Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

2015-08-01

A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L- 1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L- 1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract.

Solid-solid phase change thermal storage application to space-suit battery pack

Science.gov (United States)

Son, Chang H.; Morehouse, Jeffrey H.

1989-01-01

High cell temperatures are seen as the primary safety problem in the Li-BCX space battery. The exothermic heat from the chemical reactions could raise the temperature of the lithium electrode above the melting temperature. Also, high temperature causes the cell efficiency to decrease. Solid-solid phase-change materials were used as a thermal storage medium to lower this battery cell temperature by utilizing their phase-change (latent heat storage) characteristics. Solid-solid phase-change materials focused on in this study are neopentyl glycol and pentaglycerine. Because of their favorable phase-change characteristics, these materials appear appropriate for space-suit battery pack use. The results of testing various materials are reported as thermophysical property values, and the space-suit battery operating temperature is discussed in terms of these property results.

Development of an elevated temperature aluminum alloy containing Al3X-type dispersed phases

International Nuclear Information System (INIS)

Zedalis, M.S.

1985-01-01

The extents of solid solubility in the equilibrium, tetragonal Al 3 X-type dispersed phases (X represents binary and ternary combinations of Hf, Ti, V, and Zr) were examined using powder x-ray diffraction methods. Minimum lattice disregistry (delta) with the Al(ss) matrix was achieved by maximizing the amount of Ti or V added to the Al 3 Hf and/or Al 3 Zr phases without forming a co-intermetallic compound exhibiting a DO 22 crystal structure. In comparison to Al 3 Zr, with a (delta) equal to 2.88%, the addition of V to Al 3 Zr in the ratio 7:1, i.e., Al 3 (v/sub 0.875/Zr/sub 0.125/), results in a decrease in (delta) by approximately 17%. Electron diffraction revealed that the addition of V to the metastable cubic (L1 2 ) Al 3 Zr phase also resulted in a reduction in the lattice disregistry across the precipitate/matrix boundary. In comparison with the cubic Al 3 Zr phase, with a (delta) of approximately 1.0%, the Al 3 (V/sub 0.875/Zr/sub 0.125/) phase exhibits a mismatch of approximately -0.14%. The cubic Al 3 (V/sub 0.875/Zr/sub 0.125/) phase was observed by TEM to be substantially more stable, i.e., resist transformation to the equilibrium tetragonal phase, when compared to the cubic Al 3 Zr phase. It is proposed that a reduction in lattice disregistry results in a decrease in the strain energy component of the system's total free energy. A systematic decrease in the coarsening rate with a reduction in the lattice disregistry for the cubic Al 3 Zr, Al 3 (V/sub 0.725/Zr/sub 0.275/) and Al 3 (V/sub 0.875/Zr/sub 0.125/) and tetragonal Al 3 Zr and Al 3 (V/sub 0.875/Zr/sub 0.125/) phases is proposed to be representative of a decrease in the interfacial energy across the precipitate/matrix boundary

A Molecular-Level View of the Physical Stability of Amorphous Solid Dispersions

Science.gov (United States)

Yuan, Xiaoda

Many pharmaceutical compounds being developed in recent years are poorly soluble in water. This has led to insufficient oral bioavailability of many compounds in vitro. The amorphous formulation is one of the promising techniques to increase the oral bioavailability of these poorly water-soluble compounds. However, an amorphous drug substance is inherently unstable because it is a high energy form. In order to increase the physical stability, the amorphous drug is often formulated with a suitable polymer to form an amorphous solid dispersion. Previous research has suggested that the formation of an intimately mixed drug-polymer mixture contributes to the stabilization of the amorphous drug compound. The goal of this research is to better understand the role of miscibility, molecular interactions and mobility on the physical stability of amorphous solid dispersions. Methods were developed to detect different degrees of miscibility on nanometer scale and to quantify the extent of hydrogen-bonding interactions between the drug and the polymer. Miscibility, hydrogen-bonding interactions and molecular mobility were correlated with physical stability during a six-month period using three model systems. Overall, this research provides molecular-level insights into many factors that govern the physical stability of amorphous solid dispersions which can lead to a more effective design of stable amorphous formulations.

Solid phase assays

International Nuclear Information System (INIS)

Reese, M.G.; Johnson, L.R.; Ransom, D.K.

1980-01-01

In a solid phase assay for quantitative determination of biological and other analytes, a sample such as serum is contacted with a receptor for the analyte being assayed, the receptor being supported on a solid support. No tracer for the analyte is added to the sample before contacting with the receptor; instead the tracer is contacted with the receptor after unbound analyte has been removed from the receptor. The assay can be otherwise performed in a conventional manner but can give greater sensitivity. (author)

Fast determination of seven synthetic pigments from wine and soft drinks using magnetic dispersive solid-phase extraction followed by liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

Chen, Xiao-Hong; Zhao, Yong-Gang; Shen, Hao-Yu; Zhou, Li-Xin; Pan, Sheng-Dong; Jin, Mi-Cong

2014-06-13

A novel, simple and sensitive method based on the use of magnetic dispersive solid-phase extraction (M-dSPE) procedure combined with ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) was developed to determine seven synthetic pigments (tartrazine, amaranth, carmine, sunset yellow, allura red, brilliant blue and erythrosine) in wines and soft drinks. An amino-functionalized low degrees of cross-linking magnetic polymer (NH2-LDC-MP) was synthesized via suspension polymerization, and characterized by transmission electron microscopy (TEM). The NH2-LDC-MP was used as the M-dSPE sorbent to remove the matrix from the solution, and the main factors affecting the extraction were investigated in detail. The obtained results demonstrated the higher extraction capacity of NH2-LDC-MP with recoveries between 84.0 and 116.2%. The limits of quantification (LOQs) for the seven synthetic pigments were between 1.51 and 5.0μg/L in wines and soft drinks. The developed M-dSPE UFLC-MS/MS method had been successfully applied to the real wines and soft drinks for food-safety risk monitoring in Zhejiang Province, China. The results showed that sunset yellow was in three out of thirty soft drink samples (2.95-42.6μg/L), and erythrosine in one out of fifteen dry red wine samples (3.22μg/L), respectively. It was confirmed that the NH2-LDC-MP was a kind of highly effective M-dSPE materials for the pigments analyses. Copyright © 2014 Elsevier B.V. All rights reserved.

Directed Acceleration of Electrons from a Solid Surface by Sub-10-fs Laser Pulses

International Nuclear Information System (INIS)

Brandl, F.; Hidding, B.; Osterholz, J.; Hemmers, D.; Pretzler, G.; Karmakar, A.; Pukhov, A.

2009-01-01

Electrons have been accelerated from solid target surfaces by sub-10-fs laser pulses of 120 μJ energy which were focused to an intensity of 2x10 16 W/cm 2 . The electrons have a narrow angular distribution, and their observed energies exceed 150 keV. We show that these energies are not to be attributed to collective plasma effects but are mainly gained directly via repeated acceleration in the transient field pattern created by incident and reflected laser, alternating with phase-shift-generating scattering events in the solid.

Identification of phases in zinc alloy powders using electron backscatter diffraction

Energy Technology Data Exchange (ETDEWEB)

Perez, Martin G. [Graduate Center for Materials Research, University of Missouri-Rolla, Rolla, MO 65409 (United States); Kenik, Edward A. [Oak Ridge National Laboratory, 100 Bethel Valley Rd., Bldg. 4515, MS-6064, P.O. Box 2008, Oak Ridge, TN 37831 (United States); O' Keefe, Matthew J. [Graduate Center for Materials Research, University of Missouri-Rolla, Rolla, MO 65409 (United States)]. E-mail: mjokeefe@umr.edu; Miller, F. Scott [Graduate Center for Materials Research, University of Missouri-Rolla, Rolla, MO 65409 (United States); Johnson, Benedict [Graduate Center for Materials Research, University of Missouri-Rolla, Rolla, MO 65409 (United States)

2006-05-25

Scanning electron microscopy and electron backscatter diffraction (EBSD) were used for the structural characterization of phases in Zn alloy powders. Commercial Zn alloy powders contained additions of <1000 ppm of Bi, In, Al or Mg. Bismuth and In have extremely low solubility in Zn and form intermetallic Bi-In compounds which segregate to the Zn grain boundaries. The Bi-In phases were <0.3 {mu}m in size, had low melting points, and were not abundant enough for EBSD analysis. Increasing the alloying additions 20-40-fold resulted in Bi-In phases >1 {mu}m that could be used for EBSD analysis for phase characterization. Deformation-free microstructures were obtained by mechanical polishing and ion milling. The Zn matrix was characterized as Zn via EBSD. A BiIn{sub 2} phase was identified in the powder microstructures via EBSD. An In phase with 8-9 wt.% Bi was identified using low voltage energy dispersive spectroscopy and closely matched the composition predicted by the Bi-In phase diagram.

Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

Directory of Open Access Journals (Sweden)

Helena Prosen

2014-05-01

Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

Applications of liquid-phase microextraction in the sample preparation of environmental solid samples.

Science.gov (United States)

Prosen, Helena

2014-05-23

Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several innovative liquid-phase microextraction (LPME) techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME). Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

Preparation and evaluation of carvacrol pellets based on PVP solid-dispersion by extrusion-spheronization technique

Directory of Open Access Journals (Sweden)

Z. Taghizadeh*

2017-11-01

Full Text Available Background and objectives: Carvacrol is one of the main pharmacologically active components of Thymus vulgaris essential oil which has shown several therapeutic effects. There are few works regarding the formulation of essential oils as oral solid dosage forms due to their liquid nature, stability and technical problems. The aim of this study was to combine the solid-dispersion approach and extrusion-spheronization technique to produce pellets with desirable physico-mechanical and release properties. Methods: Solid dispersion matrix (30% of carvacrol in polyvinylpyrrolidone K30 was prepared by solvent evaporation. The matrix was mixed with Avicel and lactose and granulated by water. The wet mass was transformed into pellets by extrusion-spheronization. In order to compare the solid dispersion method with the classic approaches, another pellet formulation was prepared by absorption of carvacrol on Aerosil. The pellets were characterized for size (sieve analysis, shape factors (image analysis, mechanical strength, carvacrol content, and release rate (dissolution test. Accelerated stability test of formulations was also carried out. Results: Using suitable composition of solid dispersion matrix and granulation fluid, the pellets with desirable size and shape and mechanical properties could be produced. PVP-based pellets had higher mechanical strength, slower release rate and improved content and stability. The PVP ratio showed considerable effect on release properties of the pellets. Conclusion: Overall, the results revealed the feasibility of preparing desirable pellets containing carvacrol with acceptable content, stability and release properties which can be administered as hard gelatin capsules.

Microwave-assisted synthesis of reduced graphene oxide decorated with magnetite and gold nanoparticles, and its application to solid-phase extraction of organochlorine pesticides

International Nuclear Information System (INIS)

Mehdinia, Ali; Rouhani, Shirin; Mozaffari, Shahla

2016-01-01

An agent-free microwave-assisted method was developed for the preparation of a reduced graphene oxide/Fe_3O_4-gold nanocomposite. This material was used as an adsorbent for magnetic solid-phase extraction of organochlorine pesticides (OCPs) from water samples. The nanocomposite was characterized by transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy and energy-dispersive X-ray spectroscopy. The effects of sample volume, amount of sorbent, eluent volume, extraction and desorption time, and the effect of salt on the extraction efficiency were optimized. The linear response range of GC analysis extends from 0.05 to 500 μg L"−"1 of OCPs, the limits of detection range from 0.4 to 4.1 ng L"−"1, relative standard deviations from 1.7 to 7.3 %, and recoveries (from spiked seawater samples) from 69 to 114 %. (author)

Solid-phase zirconium and fluoride species in alkaline zircaloy cladding waste at Hanford.

Science.gov (United States)

Reynolds, Jacob G; Huber, Heinz J; Cooke, Gary A; Pestovich, John A

2014-08-15

The United States Department of Energy Hanford Site, near Richland, Washington, USA, processed plutonium between 1944 and 1987. Fifty-six million gallons of waste of various origins remain, including waste from removing zircaloy fuel cladding using the so-called Zirflex process. The speciation of zirconium and fluoride in this waste is important because of the corrosivity and reactivity of fluoride as well as the (potentially) high density of Zr-phases. This study evaluates the solid-phase speciation of zirconium and fluoride using X-ray diffraction (XRD) and scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS). Two waste samples were analyzed: one waste sample that is relatively pure zirconium cladding waste from tank 241-AW-105 and another that is a blend of zirconium cladding wastes and other high-level wastes from tank 241-C-104. Villiaumite (NaF) was found to be the dominant fluoride species in the cladding waste and natrophosphate (Na7F[PO4]2 · 19H2O) was the dominant species in the blended waste. Most zirconium was present as a sub-micron amorphous Na-Zr-O phase in the cladding waste and a Na-Al-Zr-O phase in the blended waste. Some zirconium was present in both tanks as either rounded or elongated crystalline needles of Na-bearing ZrO2 that are up to 200 μm in length. These results provide waste process planners the speciation data needed to develop disposal processes for this waste. Copyright © 2014 Elsevier B.V. All rights reserved.

Systematic study on intermolecular valence-band dispersion in molecular crystalline films

International Nuclear Information System (INIS)

Yamane, Hiroyuki; Kosugi, Nobuhiro

2015-01-01

Highlights: • Intermolecular valence-band dispersion of crystalline films of phthalocyanines. • Intermolecular transfer integral versus lattice constant. • Site-specific intermolecular interaction and resultant valence-band dispersion. • Band narrowing effect induced by elevated temperature. - Abstract: Functionalities of organic semiconductors are governed not only by individual properties of constituent molecules but also by solid-state electronic states near the Fermi level such as frontier molecular orbitals, depending on weak intermolecular interactions in various conformations. The individual molecular property has been widely investigated in detail; on the other hand, the weak intermolecular interaction is difficult to investigate precisely due to the presence of the structural and thermal energy broadenings in organic solids. Here we show quite small but essential intermolecular valence band dispersions and their temperature dependence of sub-0.1-eV scale in crystalline films of metal phthalocyanines (H_2Pc, ZnPc, CoPc, MnPc, and F_1_6ZnPc) by using angle-resolved photoemission spectroscopy (ARPES) with synchrotron radiation. The observed bands show intermolecular and site dependent dispersion widths, phases, and periodicities, for different chemical substitution of terminal groups and central metals in the phthalocyanine molecule. The precise and systematic band-dispersion measurement would be a credible approach toward the comprehensive understanding of intermolecular interactions and resultant charge transport properties as well as their tuning by substituents in organic molecular systems.

Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

Science.gov (United States)

Krawczyk-Coda, Magdalena

2017-03-01

In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

Electron holography for fields in solids: Problems and progress

International Nuclear Information System (INIS)

Lichte, Hannes; Börrnert, Felix; Lenk, Andreas; Lubk, Axel; Röder, Falk; Sickmann, Jan; Sturm, Sebastian; Vogel, Karin; Wolf, Daniel

2013-01-01

Electron holography initially was invented by Dennis Gabor for solving the problems raised by the aberrations of electron lenses in Transmission Electron Microscopy. Nowadays, after hardware correction of aberrations allows true atomic resolution of the structure, for comprehensive understanding of solids, determination of electric and magnetic nanofields is the most challenging task. Since fields are phase objects in the TEM, electron holography is the unrivaled method of choice. After more than 40 years of experimental realization and steady improvement, holography is increasingly contributing to these highly sophisticated and essential questions in materials science, as well to the understanding of electron waves and their interaction with matter. - Highlights: • We review the development of the method of electron holography. • We outline the role of information content as guideline. • We outline the improvements of the method. • We sketch the future instrumental development. • We summarize the still existing problems to solve

The removal of fatty acids from edible oil : removal of the dispersed phase of a water-in-oil dispersion by a hydrophilic membrane

NARCIS (Netherlands)

Keurentjes, J.T.F.; Doornbusch, G.I.; Riet, van 't K.

1991-01-01

Fatty acids can be extracted from an oil phase by forming a dispersed phase of saponified fatty acids/water/isopropanol in oil. This dispersion can be separated in the two phases by two membranes of opposite polarity in series. In this study the separation of the water phase from the dispersion by a

All-PM monolithic fs Yb-fiber laser, dispersion-managed with all-solid photonic bandgap fiber

DEFF Research Database (Denmark)

Liu, Xiaomin; Lægsgaard, Jesper; Turchinovich, Dmitry

2009-01-01

All-in-fiber SESAM-modelocked self-starting fiber laser is demonstrated. Cavity dispersion is managed by a spliced-in PM all-solid photonic bandgap fiber. The laser directly delivers 1.25 nJ pulses of 280 fs duration.......All-in-fiber SESAM-modelocked self-starting fiber laser is demonstrated. Cavity dispersion is managed by a spliced-in PM all-solid photonic bandgap fiber. The laser directly delivers 1.25 nJ pulses of 280 fs duration....

Unipolar time-differential charge sensing in non-dispersive amorphous solids

International Nuclear Information System (INIS)

Goldan, A. H.; Rowlands, J. A.; Tousignant, O.; Karim, K. S.

2013-01-01

The use of high resistivity amorphous solids as photodetectors, especially amorphous selenium, is currently of great interest because they are readily produced over large area at substantially lower cost compared to grown crystalline solids. However, amorphous solids have been ruled out as viable radiation detection media for high frame-rate applications, such as single-photon-counting imaging, because of low carrier mobilities, transit-time-limited photoresponse, and consequently, poor time resolution. To circumvent the problem of poor charge transport in amorphous solids, we propose unipolar time-differential charge sensing by establishing a strong near-field effect using an electrostatic shield within the material. For the first time, we have fabricated a true Frisch grid inside a solid-state detector by evaporating amorphous selenium over photolithographically prepared multi-well substrates. The fabricated devices are characterized with optical, x-ray, and gamma-ray impulse-like excitations. Results prove the proposed unipolar time-differential property and show that time resolution in non-dispersive amorphous solids can be improved substantially to reach the theoretical limit set by spatial spreading of the collected Gaussian carrier cloud.

Enhancement of in-vitro drug dissolution of ketoconazole for its optimal in-vivo absorption using Nanoparticles and Solid Dispersion forms of the drug

Science.gov (United States)

Syed, Mohammed Irfan

was modified to include 0.02%, 0.05% and 0.1% sodium lauryl sulfate. Here, after 2 hours, the amount of drug dissolved was calculated to be 10% from controls, 21% from solid dispersion and 36% from nanoparticles in SIF with 0.02% SLS. Drug release was 20% from controls, 41% from solid dispersion and 52% from nanoparticle formulation in SIF with 0.05% SLS. Whereas amount of drug released in SIF with 0.1% SLS showed 21% from the control, 62% from solid dispersion and 85% from Nanoparticles respectively. This data supports that the ketoconazole Nanoparticles and its solid-dispersion exhibit many fold increase in dissolution of the drug, which could lead to a less variable and enhanced in-vivo drug absorption profiles. In addition, the data from the Physical Characterization (DSC, XRD and FTIR) supports that there were no interaction within the ingredients occurred in Nanoparticles and solid-dispersion formulations of the drug sample. Wet Bead Milling and Hot Melt methods proved useful in developing the Nanoparticles and solid dispersion form of ketoconazole. Results from particle size analysis were in correlation with data obtained from Scanning electron Microscopy and size of the nanoparticles was below 100nm. The dissolution studies with the modified simulated intestinal fluid (SIF) exhibited several fold increase in the dissolution of the drug compared to the pure drug powder and the commercial products used as the control. Also, the results from the physical characterization studies clearly support the stability of ketoconazole in both of these formulations.

Frequency doubling in poled polymers using anomalous dispersion phase-matching

Energy Technology Data Exchange (ETDEWEB)

Kowalczyk, T.C.; Singer, K.D. [Case Western Reserve Univ., Cleveland, OH (United States). Dept. of Physics; Cahill, P.A. [Sandia National Labs., Albuquerque, NM (United States)

1995-10-01

The authors report on a second harmonic generation in a poled polymer waveguide using anomalous dispersion phase-matching. Blue light ({lambda} = 407 nm) was produced by phase-matching the lowest order fundamental and harmonic modes over a distance of 32 {micro}m. The experimental conversion efficiency was {eta} = 1.2 {times} 10{sup {minus}4}, in agreement with theory. Additionally, they discuss a method of enhancing the conversion efficiency for second harmonic generation using anomalous dispersion phase-matching to optimize Cerenkov second harmonic generation. The modeling shows that a combination of phase-matching techniques creates larger conversion efficiencies and reduces critical fabrication requirements of the individual phase-matching techniques.

Introduction to solid state electronics

CERN Document Server

Wang, FFY

1989-01-01

This textbook is specifically tailored for undergraduate engineering courses offered in the junior year, providing a thorough understanding of solid state electronics without relying on the prerequisites of quantum mechanics. In contrast to most solid state electronics texts currently available, with their generalized treatments of the same topics, this is the first text to focus exclusively and in meaningful detail on introductory material. The original text has already been in use for 10 years. In this new edition, additional problems have been added at the end of most chapters. These proble

Optical properties of solids

CERN Document Server

Wooten, Frederick

1972-01-01

Optical Properties of Solids covers the important concepts of intrinsic optical properties and photoelectric emission. The book starts by providing an introduction to the fundamental optical spectra of solids. The text then discusses Maxwell's equations and the dielectric function; absorption and dispersion; and the theory of free-electron metals. The quantum mechanical theory of direct and indirect transitions between bands; the applications of dispersion relations; and the derivation of an expression for the dielectric function in the self-consistent field approximation are also encompassed.

Combinatorial Solid-Phase Synthesis of Balanol Analogues

DEFF Research Database (Denmark)

Nielsen, John; Lyngsø, Lars Ole

1996-01-01

The natural product balanol has served as a template for the design and synthesis of a combinatorial library using solid-phase chemistry. Using a retrosynthetic analysis, the structural analogues have been assembled from three relatively accessible building blocks. The solid-phase chemistry inclu...

Preconcentration of uranium in water samples using dispersive ...

African Journals Online (AJOL)

Preconcentration of uranium in water samples using dispersive liquid-liquid micro- extraction coupled with solid-phase extraction and determination with inductively coupled plasma-optical emission spectrometry.

Selective ionic liquid ferrofluid based dispersive-solid phase extraction for simultaneous preconcentration/separation of lead and cadmium in milk and biological samples.

Science.gov (United States)

Fasih Ramandi, Negin; Shemirani, Farzaneh

2015-01-01

For the first time, a selective ionic liquid ferrofluid has been used in dispersive solid phase extraction (IL-FF-D-SPE) for simultaneous preconcentration and separation of lead and cadmium in milk and biological samples combined with flame atomic absorption spectrometry. To improve the selectivity of the ionic liquid ferrofluid, the surface of TiO2 nanoparticles with a magnetic core as sorbent was modified by loading 1-(2-pyridylazo)-2-naphtol. Due to the rapid injection of an appropriate amount of ionic liquid ferrofluid into the aqueous sample by a syringe, extraction can be achieved within a few seconds. In addition, based on the attraction of the ionic liquid ferrofluid to a magnet, no centrifugation step is needed for phase separation. The experimental parameters of IL-FF-D-SPE were optimized using a Box-Behnken design (BBD) after a Plackett-Burman screening design. Under the optimum conditions, the relative standard deviations of 2.2% and 2.4% were obtained for lead and cadmium, respectively (n=7). The limit of detections were 1.21 µg L(-1) for Pb(II) and 0.21 µg L(-1) for Cd(II). The preconcentration factors were 250 for lead and 200 for cadmium and the maximum adsorption capacities of the sorbent were 11.18 and 9.34 mg g(-1) for lead and cadmium, respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

Stability of nanoscale secondary phases in an oxide dispersion strengthened Fe-12Cr alloy

International Nuclear Information System (INIS)

Castro, V. de; Marquis, E.A.; Lozano-Perez, S.; Pareja, R.; Jenkins, M.L.

2011-01-01

Transmission electron microscopy and atom-probe tomography were used to characterize on a near-atomic scale the microstructure and oxide and carbide phases that form during thermo-mechanical treatments of a model oxide dispersion strengthened Fe-12 wt.% Cr-0.4 wt.% Y 2 O 3 alloy. It was found that some of the Y-rich nanoparticles retained their initial crystallographic structure but developed a Cr-enriched shell, while others evolved into ternary oxide phases during the initial processing. The Y- and Cr-rich oxide phases formed remained stable after annealing at 1023 K for 96 h. However, the number of Cr-rich carbides appeared to increase, inducing Cr depletion in the matrix.

Stability of nanoscale secondary phases in an oxide dispersion strengthened Fe-12Cr alloy

Energy Technology Data Exchange (ETDEWEB)

Castro, V. de, E-mail: vanessa.decastro@uc3m.es [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom); Marquis, E.A.; Lozano-Perez, S. [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom); Pareja, R. [Departamento de Fisica, Universidad Carlos III de Madrid, Avda. de la Universidad 30, 28911 Leganes, Madrid (Spain); Jenkins, M.L. [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom)

2011-06-15

Transmission electron microscopy and atom-probe tomography were used to characterize on a near-atomic scale the microstructure and oxide and carbide phases that form during thermo-mechanical treatments of a model oxide dispersion strengthened Fe-12 wt.% Cr-0.4 wt.% Y{sub 2}O{sub 3} alloy. It was found that some of the Y-rich nanoparticles retained their initial crystallographic structure but developed a Cr-enriched shell, while others evolved into ternary oxide phases during the initial processing. The Y- and Cr-rich oxide phases formed remained stable after annealing at 1023 K for 96 h. However, the number of Cr-rich carbides appeared to increase, inducing Cr depletion in the matrix.

Surface phase transitions in cu-based solid solutions

Science.gov (United States)

Zhevnenko, S. N.; Chernyshikhin, S. V.

2017-11-01

We have measured surface energy in two-component Cu-based systems in H2 + Ar gas atmosphere. The experiments on solid Cu [Ag] and Cu [Co] solutions show presence of phase transitions on the surfaces. Isotherms of the surface energy have singularities (the minimum in the case of copper solid solutions with silver and the maximum in the case of solid solutions with cobalt). In both cases, the surface phase transitions cause deficiency of surface miscibility: formation of a monolayer (multilayer) (Cu-Ag) or of nanoscale particles (Cu-Co). At the same time, according to the volume phase diagrams, the concentration and temperature of the surface phase transitions correspond to the solid solution within the volume. The method permits determining the rate of diffusional creep in addition to the surface energy. The temperature and concentration dependence of the solid solutions' viscosity coefficient supports the fact of the surface phase transitions and provides insights into the diffusion properties of the transforming surfaces.

Studies on keV and eV electrons in solids

International Nuclear Information System (INIS)

Schou, J.

1979-10-01

The interaction between keV or eV electrons and solids was studied. The results presented mostly concern problems in connection with electron irradiation of solids, but to some extent they also include ion-induced secondary electron emission. The experiments were mainly performed on solidified gases using 1 - 3 keV electrons. The projected range of electrons was determined in solid hydrogen, deuterium and nitrogen. The true secondary electron emission coefficient and the electron reflection coefficient of solid hydrogen, deuterium and nitrogen were measured. The escape depth of the true secondary electrons in nitrogen was determined. The angular dependence of both the reflection coefficient and the true secondary electron emission coefficient of solid hydrogen and deuterium was investigated. Both ion- and electron-induced secondary electron emission were treated theoretically on the basis of ionization cascade theory. (Auth.)

Transmission electron microscopy characterization of irradiated U-7Mo/Al-2Si dispersion fuel

International Nuclear Information System (INIS)

Gan, J.; Keiser, D.D.; Wachs, D.M.; Robinson, A.B.; Miller, B.D.; Allen, T.R.

2010-01-01

The plate-type dispersion fuels, with the atomized U(Mo) fuel particles dispersed in the Al or Al alloy matrix, are being developed for use in research and test reactors worldwide. It is found that the irradiation performance of a plate-type dispersion fuel depends on the radiation stability of the various phases in a fuel plate. Transmission electron microscopy was performed on a sample (peak fuel mid-plane temperature ∼109 deg. C and fission density ∼4.5 x 10 27 f m -3 ) taken from an irradiated U-7Mo dispersion fuel plate with Al-2Si alloy matrix to investigate the role of Si addition in the matrix on the radiation stability of the phase(s) in the U-7Mo fuel/matrix interaction layer. A similar interaction layer that forms in irradiated U-7Mo dispersion fuels with pure Al matrix has been found to exhibit poor irradiation stability, likely as a result of poor fission gas retention. The interaction layer for both U-7Mo/Al-2Si and U-7Mo/Al fuels is observed to be amorphous. However, unlike the latter, the amorphous layer for the former was found to effectively retain fission gases in areas with high Si concentration. When the Si concentration becomes relatively low, the fission gas bubbles agglomerate into fewer large pores. Within the U-7Mo fuel particles, a bubble superlattice ordered as fcc structure and oriented parallel to the bcc metal lattice was observed where the average bubble size and the superlattice constant are 3.5 nm and 11.5 nm, respectively. The estimated fission gas inventory in the bubble superlattice correlates well with the fission density in the fuel.

Sulfonated nanocellulose for the efficient dispersive micro solid-phase extraction and determination of silver nanoparticles in food products.

Science.gov (United States)

Ruiz-Palomero, Celia; Soriano, M Laura; Valcárcel, Miguel

2016-01-08

This paper reports a simple approach to Analytical Nanoscience and Nanotechnology (AN&N) that integrates the nanotool, sulfonated nanocellulose (s-NC), and nanoanalyte, silver nanoparticles (AgNPs), in the same analytical process by using an efficient, environmentally friendly dispersive micro solid-phase extraction (D-μSPE) capillary electrophoresis (CE) method with s-NC as sorbent material. Introducing negatively charged sulfate groups onto the surface of cellulose enhances its surface chemistry and enables the extraction and preconcentration of AgNPs of variable diameter (10, 20 and 60nm) and shell composition (citrate and polyvinylpyrrolidone coatings) from complex matrices into a cationic surfactant. In this way, AgNPs of diverse nature were successfully extracted onto the s-NC sorbent and then desorbed into an aqueous solution containing thiotic acid (TA) prior to CE without the need for any labor-intensive cleanup. The ensuing eco-friendly D-μSPE method exhibited a linear response to AgNPs with a limit of detection (LOD) of 20μg/L. Its ability to specifically recognize AgNPs of different sizes was checked in orange juice and mussels, which afforded recoveries of 70.9-108.4%. The repeatability of the method at the limit of quantitation (LOQ) level was 5.6%. Based on the results, sulfonated nanocellulose provides an efficient, cost-effective analytical nanotool for the extraction of AgNPs from food products. Copyright © 2015 Elsevier B.V. All rights reserved.

Phase Transformation in Cast Superaustenitic Stainless Steels

Energy Technology Data Exchange (ETDEWEB)

Lee Phillips, Nathaniel Steven [Iowa State Univ., Ames, IA (United States)

2006-01-01

Superaustenitic stainless steels constitute a group of Fe-based alloys that are compositionally balanced to have a purely austenitic matrix and exhibit favorable pitting and crevice corrosion resistant properties and mechanical strength. However, intermetallic precipitates such as sigma and Laves can form during casting or exposure to high-temperature processing, which degrade the corrosion and mechanical properties of the material. The goal of this study was to accurately characterize the solid-solid phase transformations seen in cast superaustenitic stainless steels. Heat treatments were performed to understand the time and temperature ranges for intermetallic phase formations in alloys CN3MN and CK3MCuN. Microstructures were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy and wavelength dispersive spectroscopy (EDS, WDS). The equilibrium microstructures, composed primarily of sigma and Laves within purely austenitic matrices, showed slow transformation kinetics. Factors that determine the extent of transformation, including diffusion, nucleation, and growth, are discussed.

Profiling the Fatty Acids Content of Ornamental Camellia Seeds Cultivated in Galicia by an Optimized Matrix Solid-Phase Dispersion Extraction

Directory of Open Access Journals (Sweden)

Carmen Garcia-Jares

2017-10-01

Full Text Available Camellia (genus of flowering plants of fam. Theaceae is one of the main crops in Asia, where tea and oil from leaves and seeds have been utilized for thousands of years. This plant is excellently adapted to the climate and soil of Galicia (northwestern Spain and northern Portugal where it is grown not only as an ornamental plant, but to be evaluated as a source of bioactive compounds. In this work, the main fatty acids were extracted from Camellia seeds of four varieties of Camellia: sasanqua, reticulata, japonica and sinensis, by means of matrix-solid phase dispersion (MSPD, and analyzed by gas chromatography (GC with MS detection of the corresponding methyl esters. MSPD constitutes an efficient and greener alternative to conventional extraction techniques, moreover if it is combined with the use of green solvents such as limonene. The optimization of the MSPD extraction procedure has been conducted using a multivariate approach based on strategies of experimental design, which enabled the simultaneous evaluation of the factors influencing the extraction efficiency as well as interactions between factors. The optimized method was applied to characterize the fatty acids profiles of four Camellia varieties seeds, allowing us to compare their fatty acid composition.

Profiling the Fatty Acids Content of Ornamental Camellia Seeds Cultivated in Galicia by an Optimized Matrix Solid-Phase Dispersion Extraction

Science.gov (United States)

Garcia-Jares, Carmen; Sanchez-Nande, Marta; Lamas, Juan Pablo; Lores, Marta

2017-01-01

Camellia (genus of flowering plants of fam. Theaceae) is one of the main crops in Asia, where tea and oil from leaves and seeds have been utilized for thousands of years. This plant is excellently adapted to the climate and soil of Galicia (northwestern Spain) and northern Portugal where it is grown not only as an ornamental plant, but to be evaluated as a source of bioactive compounds. In this work, the main fatty acids were extracted from Camellia seeds of four varieties of Camellia: sasanqua, reticulata, japonica and sinensis, by means of matrix-solid phase dispersion (MSPD), and analyzed by gas chromatography (GC) with MS detection of the corresponding methyl esters. MSPD constitutes an efficient and greener alternative to conventional extraction techniques, moreover if it is combined with the use of green solvents such as limonene. The optimization of the MSPD extraction procedure has been conducted using a multivariate approach based on strategies of experimental design, which enabled the simultaneous evaluation of the factors influencing the extraction efficiency as well as interactions between factors. The optimized method was applied to characterize the fatty acids profiles of four Camellia varieties seeds, allowing us to compare their fatty acid composition. PMID:29039745

Evaluation and enhancement of physical stability of semi-solid dispersions containing piroxicam into hard gelatin capsules.

Science.gov (United States)

Karataş, Ayşegül; Bekmezci, Serife

2013-01-01

The aim of the study was to investigate the physical stability of the semi-solid dispersions into the hard gelatine capsules prepared with Gelucire 44/14, Labrasol and different additives such as microcrystalline cellulose (MCC), mannitol and lactose (alpha-monohydrate) used for enhancing the stability of the formulations. The master dispersion prepared with only Gelucire 44/14 (20% w/w) and Labrasol (80% w/w) was stored in a refrigerator (5 +/- 3 degrees C), while the modified dispersions with the additives (2% w/w) were kept in a climatic chamber (25 +/- 2 degrees C / 60 +/- 5% RH) for 12 months. Dissolution tests of the semi-solid dispersions were performed in media with different pH's immediatly after preparation and after 3, 6 and 12 months of storage. FTIR and DSC studies were also carried out at the same time points. The ideal storage condition for the master dispersion was found to be at 5 degrees C. The addition of MCC, mannitol and lactose (alpha-monohydrate) to the original dispersion afforded a solidification effect on the formulation at room temperature and showed the same dissolution behavior (not less than 85% of piroxicam within 30 min in pH 1.2, 4.5 and 6.8; and water) with the master. The dispersion including lactose was stable at 25 degrees C for 12 months. However, the ideal period of storage for the modified dispersions including MCC and mannitol was 6 months at 25 degrees C. FTIR and DSC results both confirmed the amorphous state of piroxicam in all semi-solid dispersions under storage conditions for 12 months.

Auroral electron time dispersion

International Nuclear Information System (INIS)

Kletzing, C.A.

1989-01-01

A sounding rocket flight was launched from Greenland in 1985 to study high latitude, early morning auroral physics. The payload was instrumented with electron and ion detectors, AC and DC electric field experiments, a plasma density experiment, and a magnetometer to measure the ambient field. The rocket was launched during disturbed conditions, when the polar cap was in a contracted state with visible aurora overhead. The electron data contained numerous signatures indicative of time-of-flight energy dispersion characterized by a coherent structure in which lower energy electrons arrived at the rocket after higher energy electrons. A model was constructed to explain this phenomena by the sudden application of a region of parallel electric field along a length of magnetic field line above the rocket. The model incorporates detector response and uses an altitudinal density profile based on auroral zone measurements. Three types of potential structures were tried: linear, quadratic and cubic. Of the three it was found that the cubic (electric field growing in a quadratic manner moving up the field line) produced the best fit to the data. The potential region was found to be approximately 1-2 R e in extent with the lower edge 3000-4000 km away from the rocket. The background electron temperature in the model which produced the best fit to the data was of the order of 15 eV

Synthesis of novel high-voltage cathode material LiCoPO4 via rheological phase method

International Nuclear Information System (INIS)

Tan, Long; Luo, Zhimei; Liu, Haowen; Yu, Ying

2010-01-01

For the first time, rheological phase method, a simple and effective route, is applied to synthesize novel cathode material LiCoPO 4 . X-ray diffraction spectrometer (XRD), X-ray photoelectron spectrometer (XPS), transmission electron microscope (TEM) and electrochemical impedance spectroscopy (EIS) are taken to investigate this material, respectively. XRD figure shows that the rheological sample is better crystallized than the solid-state one. XPS result of the rheological sample exhibits that the valence of Co is 2+. TEM images show that better dispersed particles with smaller size can be formed by rheological method comparing to the solid-state route. Charge-discharge test is carried out in the range of 3.0-5.0 V at 0.2 mA cm -2 . The initial discharge capacity for rheological phase and solid-state powder is 71.5 and 30.9 mAh g -1 , respectively. The better electrochemical property should be ascribed to the better crystallized rheological phase production with better dispersed and smaller particles, which can greatly facilitate the diffusion of Li + .

Solubility and dissolution performances of spray-dried solid dispersion of Efavirenz in Soluplus.

Science.gov (United States)

Lavra, Zênia Maria Maciel; Pereira de Santana, Davi; Ré, Maria Inês

2017-01-01

Efavirenz (EFV), a first-line anti-HIV drug largely used as part of antiretroviral therapies, is practically insoluble in water and belongs to BCS class II (low solubility/high permeability). The aim of this study was to improve the solubility and dissolution performances of EFV by formulating an amorphous solid dispersion of the drug in polyvinyl caprolactam-polyvinyl acetate-polyethylene glycol graft copolymer (Soluplus ® ) using spray-drying technique. To this purpose, spray-dried dispersions of EFV in Soluplus ® at different mass ratios (1:1.25, 1:7, 1:10) were prepared and characterized using particle size measurements, SEM, XRD, DSC, FTIR and Raman microscopy mapping. Solubility and dissolution were determined in different media. Stability was studied at accelerated conditions (40 °C/75% RH) and ambient conditions for 12 months. DSC and XRD analyses confirmed the EFV amorphous state. FTIR spectroscopy analyses revealed possible drug-polymer molecular interaction. Solubility and dissolution rate of EFV was enhanced remarkably in the developed spray-dried solid dispersions, as a function of the polymer concentration. Spray-drying was concluded to be a proper technique to formulate a physically stable dispersion of amorphous EFV in Soluplus ® , when protected from moisture.

Comparison of ethylcellulose matrix characteristics prepared by solid dispersion technique or physical mixing

Directory of Open Access Journals (Sweden)

Fatemeh Sadeghi

2003-07-01

Full Text Available The characteristics of ethylcellulose matrices prepared from solid dispersion systems were compared with those prepared from physical mixture of drug and polymer. Sodium diclofenac was used as a model drug and the effect of the drug:polymer ratio and the method of matrix production on tablet crushing strength, friability, drug release profile and drug release mechanism were evaluated. The results showed that increasing the polymer content in matrices increased the crushing strengths of tablets. However the friability of tablets was independent of polymer content. Drug release rate was greatly affected by the amount of polymer in the matrices and considerable decrease in release rate was observed by increasing the polymer content. It was also found that the type of mixture used for matrix production had great influence on the tablet crushing strength and drug release rate. Matrices prepared from physical mixtures of drug and polymer was harder than those prepared from solid dispersion systems, but their release rates were considerably faster. This phenomenon was attributed to the encapsulation of drug particles by polymer in matrices prepared from solid dispersion system which caused a great delay in diffusion of the drug through polymer and made diffusion as a rate retarding process in drug release mechanism.

Solid phase transformations

CERN Document Server

Čermák, J

2008-01-01

This special-topic book, devoted to ""Solid Phase Transformations"" , covers a broad range of phenomena which are of importance in a number of technological processes. Most commercial alloys undergo thermal treatment after casting, with the aim of imparting desired compositions and/or optimal morphologies to the component phases. In spite of the fact that the topic has lain at the center of physical metallurgy for a long time, there are numerous aspects which are wide open to potential investigative breakthroughs. Materials with new structures also stimulate research in the field, as well as n

Controlled release systems containing solid dispersions: strategies and mechanisms.

Science.gov (United States)

Tran, Phuong Ha-Lien; Tran, Thao Truong-Dinh; Park, Jun Bom; Lee, Beom-Jin

2011-10-01

In addition to a number of highly soluble drugs, most new chemical entities under development are poorly water-soluble drugs generally characterized by an insufficient dissolution rate and a small absorption window, leading to the low bioavailability. Controlled-release (CR) formulations have several potential advantages over conventional dosage forms, such as providing a uniform and prolonged therapeutic effect to improve patient compliance, reducing the frequency of dosing, minimizing the number of side effects, and reducing the strength of the required dose while increasing the effectiveness of the drug. Solid dispersions (SD) can be used to enhance the dissolution rate of poorly water-soluble drugs and to sustain the drug release by choosing an appropriate carrier. Thus, a CR-SD comprises both functions of SD and CR for poorly water-soluble drugs. Such CR dosage forms containing SD provide an immediately available dose for an immediate action followed by a gradual and continuous release of subsequent doses to maintain the plasma concentration of poorly water-soluble drugs over an extended period of time. This review aims to summarize all currently known aspects of controlled release systems containing solid dispersions, focusing on the preparation methods, mechanisms of action and characterization of physicochemical properties of the system.

Coordinate, Momentum and Dispersion operators in Phase space representation

International Nuclear Information System (INIS)

Rakotoson, H.; Raoelina Andriambololona; Ranaivoson, R.T.R.; Raboanary, R.

2017-07-01

The aim of this paper is to present a study on the representations of coordinate, momentum and dispersion operators in the framework of a phase space representation of quantum mechanics that we have introduced and studied in previous works. We begin in the introduction section with a recall about the concept of representation of operators on wave function spaces. Then, we show that in the case of the phase space representation the coordinate and momentum operators can be represented either with differential operators or with matrices. The explicit expressions of both the differential operators and matrices representations are established. Multidimensional generalization of the obtained results are performed and phase space representation of dispersion operators are given.

An integrated electron and optical metallographic procedure for the identification of precipitate phases in type 316 stainless steel

International Nuclear Information System (INIS)

Slattery, G.F.; O'Riordan, P.; Lambert, M.E.; Green, S.M.

1981-01-01

A sequential and integrated metallographic procedure has been developed and successfully employed to differentiate between carbide, sigma, chi, Laves and ferrite phases which are commonly encountered in type 316 austenitic steel. The experimental techniques of optical and electron microscopy to identify these phases have been outlined and provide a rapid and convenient method of characterizing the microstructure of the steel. The techniques sequence involves selective metallographic etching, Nomarski interference microscopy, scanning electron microscopy, energy dispersive microanalysis, transmission electron microscopy and electron diffraction. (author)

Nonlinear Dispersive Elastic Waves in Solids: Exact, Approximate, and Numerical Solutions

Science.gov (United States)

Khajehtourian, Romik

Wave motion lies at the heart of many disciplines in the physical sciences and engineering. For example, problems and applications involving light, sound, heat, or fluid flow are all likely to involve wave dynamics at some level. A particular class of problems is concerned with the propagation of elastic waves in a solid medium, such as a fiber-reinforced composite material responding to vibratory excitations, or soil and rock admitting seismic waves moments after the onset of an earthquake, or phonon transport in a semiconducting crystal like silicon. Regardless of the type of wave, the dispersion relation provides a fundamental characterization of the elastodynamic properties of the medium. The first part of the dissertation examines the propagation of a large-amplitude elastic wave in a one-dimensional homogeneous medium with a focus on the effects of inherent nonlinearities on the dispersion relation. Considering a thin rod, where the thickness is small compared to the wavelength, an exact, closed-form formulation is presented for the treatment of two types of nonlinearity in the strain-displacement gradient relation: Green-Lagrange and Hencky. The derived relation is then verified by direct time-domain simulations, examining both instantaneous dispersion (by direct observation) and short-term, pre-breaking dispersion (by Fourier transformation). A high-order perturbation analysis is also conducted yielding an explicit analytical space-time solution, which is shown to be spectrally accurate. The results establish a perfect match between theory and simulation and reveal that regardless of the strength of the nonlinearity, the dispersion relation fully embodies all information pertaining to the nonlinear harmonic generation mechanism that unfolds as an arbitrary-profiled wave evolves in the medium. In the second part of the dissertation, the analysis is extended to a continuous periodic thin rod exhibiting multiple phases or embedded local resonators. The

Quantitative vs. qualitative approaches to the electronic structure of solids

International Nuclear Information System (INIS)

Oliva, J.M.; Llunell, Miquel; Alemany, Pere; Canadell, Enric

2003-01-01

The usefulness of qualitative and quantitative theoretical approaches in solid state chemistry is discussed by considering three different types of problems: (a) the distribution of boron and carbon atoms in MB 2 C 2 (M=Ca, La, etc.) phases, (b) the band structure and Fermi surface of low-dimensional transition metal oxides and bronzes, and (c) the correlation between the crystal and electronic structure of the ternary nitride Ca 2 AuN

Solid dispersions of Myricetin with enhanced solubility: Formulation, characterization and crystal structure of stability-impeding Myricetin monohydrate crystals

Science.gov (United States)

Mureşan-Pop, M.; Pop, M. M.; Borodi, G.; Todea, M.; Nagy-Simon, T.; Simon, S.

2017-08-01

Three solid dispersion forms of Myricetin combined with the Polyvinylpyrrolidone were successfully prepared by spray drying method, and characterized by X-ray powder diffraction, thermal analysis, infrared spectroscopy and optical microscopy. Zeta potential measurements provided indications on solid dispersions stability in aqueous suspension related to their storage at elevated temperature and relative humidity, which depends on the Myricetin load. By increase of Myricetin load, the stability of the solid dispersion is impeded due to growth of Myricetin monohydrate crystals. The amorphous dispersions with 10% and 50% Myricetin load are stable and, compared to pure Myricetin, their aqueous solubility is enhanced by a factor of 47 and 13, respectively. The dispersion with 80% Myricetin load is unstable on storage, and this behavior acts in conjunction with the development of Myricetin monohydrate crystals. Single-crystal X-ray diffraction results obtained for Myricetin monohydrate reveal a structure of an infinite 2D network of hydrogen-bonded molecules involving all six hydroxyl groups of Myricetin. The water molecules are positioned in between the infinite chains, and contribute via H-bonds to robust crystal packing. The calculated needle-like morphology of monohydrate form is in agreement with the optical microscopy results. The study shows that the solid amorphous dispersions with up to 50% Myricetin load are a viable option for achieving substantial solubility improvement of Myricetin, and supports their potential use in pharmaceutical applications.

Solid-Solid Vacuum Regolith Heat-Exchanger for Oxygen Production, Phase I

Data.gov (United States)

National Aeronautics and Space Administration — This SBIR Phase-1 project will demonstrate the feasibility of using a novel coaxial counterflow solid-solid heat exchanger to recover heat energy from spent regolith...

Ranges, Reflection and Secondary Electron Emission for keV Hydrogen Ions Incident on Solid N2

DEFF Research Database (Denmark)

Børgesen, P.; Sørensen, H.; Hao-Ming, Chen

1983-01-01

Ranges were measured for 0.67–3.3 keV/amu hydrogen and deuterium ions in solid N2. Comparisons with similar results for N2-gas confirm the previously observed large phase effect in the stopping cross section. Measurements of the secondary electron emission coefficient for bulk solid N2 bombarded...... by 0.67–9 keV/amu ions also seem to support such a phase effect. It is argued that we may also extract information about the charge state of reflected projectiles....

[Pharmacokinetics and relative bioavailability of THC and THC-solid dispersion orally to mice at single dose].

Science.gov (United States)

Liao, Li; Hua, Hua; Zhao, Jun-Ning; Luo, Heng; Yang, An-Dong

2014-03-01

To establish a fast sensitive, reproducible LC-MS/MS method to study pharmacokinetic properties of THC, and compare relative bioavailability of THC and its solid dispersion in mice. 200 mice were divided randomly into two groups, and administered orally with THC and THC-solid dispersion after fasting (calculate on THC:400 mg x kg(-1)), used HPLC-MS/MS method to determine the THC concentration of each period at the following times: baseline ( predose ), 15, 30, 45 min, 1, 1.5, 2, 3, 4, 6, 24 h after dosing. Calculating the pharmacokinetic parameters according to the C-t curv, and then use the Phoenix WinNonlin software for data analysis. The calibration curves were linear over the range 9.06-972 microg x L(-1) for THC (R2 = 0.999). The limit of detection (LOD) was 0.7 microg x L(-1), respectively. The average extraction recoveries for THC was above 75%, The methodology recoveries were between 79% and 108%. The intra-day and inter-day RSD were less than 13%, the stability test showed that the plasma samples was stable under different conditions (RSD THC and THC-solid dispersion orally to mice shows as fllows: T(max), were 60 and 15 min, AUC(0-t) were 44 500.43 and 57 497.81 mg x L(-1) x min, AUC(0-infinity) were 51 226.00 and 68 031.48 mg x L(-1) x min, MRT(0-infinity) were 596.915 6, 661.747 7 min, CL(z)/F were 0.007 809 and 0.005 88 L x min(-1) x kg(-1). Compared with THC, the MRT and t1/2 of the THC-solid dispersion were all slightly extended, the t(max) was significantly reduced, AUC(0-24 h), AUC(0-infinity) and C(max) were all significantly higher, the relative bioavailability of THC-solid dispersion is 1.34 times of THC. The results of the experiment shows that the precision, accuracy, recovery and applicability were found to be adequate for the pharmacokinetic studies. After oral administration to mice, the relative bioavailability of THC-solid dispersion show significant improvement compared to THC.

The Chemistry, Crystallization, Physicochemical Properties and Behavior of Sodium Aluminosilicate Solid Phases: Final Report

International Nuclear Information System (INIS)

Rosencrance, S.

2003-01-01

The synthesis of sodium aluminosilicate solids phases precipitated from NO 2 /NO 3 -free and NO 2 /NO 3 -rich liquors has been performed. Four sodium aluminosilicate precipitation products were formed. These are (1) X-ray/electron diffraction-indifferent amorphous phase; (2) crystalline zeolite A; (3)NO 2 /NO 3 -rich crystalline sodalite; and (4) NO 2 /NO 3 -rich crystalline cancrinite phase. Characterization of the physicochemical properties for these phases has been performed under conditions simulating Westinghouse Savannah River Company liquid waste processing

Development of clinical dosage forms for a poorly water-soluble drug II: formulation and characterization of a novel solid microemulsion preconcentrate system for oral delivery of a poorly water-soluble drug.

Science.gov (United States)

Li, Ping; Hynes, Sara R; Haefele, Thomas F; Pudipeddi, Madhu; Royce, Alan E; Serajuddin, Abu T M

2009-05-01

The solution of a poorly water-soluble drug in a liquid lipid-surfactant mixture, which served as a microemulsion preconcentrate, was converted into a solid form by incorporating it in a solid polyethylene glycol (PEG) matrix. The solid microemulsion preconcentrates thus formed consisted of Capmul PG8 (propylene glycol monocaprylate) as oil, Cremophor EL (polyoxyl 35 castor oil) as surfactant, and hydrophilic polymer PEG 3350 as solid matrix. The drug (aqueous solubility: 0.17 microg/mL at pH 1-8 and 25 degrees C) was dissolved in a melt of the mixture at 65-70 degrees C and then the hot solution was filled into hard gelatin capsules; the liquid gradually solidified upon cooling below 55 degrees C. The solid system was characterized by differential scanning calorimetry (DSC), scanning electron microscopy (SEM), confocal Raman microscopy (CRM), and the dispersion testing in water. It was confirmed that a solid microemulsion preconcentrate is a two-phase system, where clusters of crystalline PEG 3350 formed the solid structure (m.p. 55-60 degrees C) and the liquid microemulsion preconcentrate dispersed in between PEG 3350 crystals as a separate phase. The drug remained dissolved in the liquid phase. In vitro release testing showed that the preconcentrate dispersed readily in water forming a microemulsion with the drug dissolved in the oil particles (PEG 3350 did not interfere with the process of self-microemulsification.

Solid-phase spectrophotometry

International Nuclear Information System (INIS)

Brykina, G.D.; Marchenko, D.Yu.; Shpigun, O.A.

1995-01-01

Solid-phase spectrophotometry (SPS), which is based on the direct measurement of light absorption of an ion exchanger containing a substance of interest, was reviewed. Since 1976, it has been known that aborbance of an ion exchanger is directly proportional to the concentration of a particular ion in solution. A similar dependence can also be followed for other sorbents, as well as for foams, membranes, films, etc., which do not exhibit ion exchange properties. One can use absorption, diffuse reflection, and luminescence spectra parameters as an analytical signal. Thus, SPS of ion exchangers is among the analytical techniques that combine the sorption concentration and surface determination of the substance of interest. This review summarizes the advancements in SPS over the last six years and demonstrates the prospects for its development. Special attention is paid to experimental methods for measuring solid-phase absorption and to the basic procedures of sample preparation, including new ones. These two facets are of great importance for obtaining precise results and extending the capabilities of SPS

Ultrasound-assisted leaching-dispersive solid-phase extraction followed by liquid-liquid microextraction for the determination of polybrominated diphenyl ethers in sediment samples by gas chromatography-tandem mass spectrometry.

Science.gov (United States)

Fontana, Ariel R; Lana, Nerina B; Martinez, Luis D; Altamirano, Jorgelina C

2010-06-30

Ultrasound-assisted leaching-dispersive solid-phase extraction followed by dispersive liquid-liquid microextraction (USAL-DSPE-DLLME) technique has been developed as a new analytical approach for extracting, cleaning up and preconcentrating polybrominated diphenyl ethers (PBDEs) from sediment samples prior gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis. In the first place, PBDEs were leached from sediment samples by using acetone. This extract was cleaned-up by DSPE using activated silica gel as sorbent material. After clean-up, PBDEs were preconcentrated by using DLLME technique. Thus, 1 mL acetone extract (disperser solvent) and 60 microL carbon tetrachloride (extraction solvent) were added to 5 mL ultrapure water and a DLLME technique was applied. Several variables that govern the proposed technique were studied and optimized. Under optimum conditions, the method detection limits (MDLs) of PBDEs calculated as three times the signal-to-noise ratio (S/N) were within the range 0.02-0.06 ng g(-1). The relative standard deviations (RSDs) for five replicates were or =0.9991. Validation of the methodology was carried out by standard addition method at two concentration levels (0.25 and 1 ng g(-1)) and by comparing with a reference Soxhlet technique. Recovery values were > or =80%, which showed a satisfactory robustness of the analytical methodology for determination of low PBDEs concentration in sediment samples. Copyright 2010 Elsevier B.V. All rights reserved.

Dispersed-fringe-accumulation-based left-subtract-right method for fine co-phasing of a dispersed fringe sensor.

Science.gov (United States)

Li, Yang; Wang, Shengqian; Rao, Changhui

2017-05-20

In this paper, a dispersed-fringe-accumulation (DFA)-based left-subtract-right (LSR) piston estimation method (DFA-LSR), in which the dispersed fringe image is accumulated in the dispersed direction, and then the LSR method is used to estimate the piston error, is proposed for dispersed fringe sensors (DFS) in the fine co-phasing stage. The DFS is usually used to detect the piston errors (optical path difference) between different segmented mirrors or synthetic aperture telescopes. The DFA-LSR makes up for the shortcomings of the main peak position (MPP) method, which suffers from the constant offset in the pixel counts. The analysis and experiment results show that the proposed method can keep relatively better performance even at the condition of poor signal-to-noise ratio, compared with the MPP method in fine co-phasing stage.

Combinational approach using solid dispersion and semi-solid matrix technology to enhance in vitro dissolution of telmisartan

Directory of Open Access Journals (Sweden)

Syed Faisal Ali

2016-02-01

Full Text Available The present investigation was focused to formulate semi-solid capsules (SSCs of hydrophobic drug telmisartan (TLMS by encapsulating semi-solid matrix of its solid dispersion (SD in HPMC capsules. The combinational approach was used to reduce the lag time in drug release and improvise its dissolution. SDs of TLMS was prepared using hot fusion method by varying the combinations of Pluronic-F68, Gelucire 50/13 and Plasdone S630. A total of nine batches (SD1-SD9 were characterized for micromeritic properties, in vitro dissolution behavior and surface characterization. SD4 with 52.43% cumulative drug release (CDR in phosphate buffer, pH 7.4, in 120 min, t50% 44.2 min and DE30min 96.76% was selected for the development of semi-solid capsules. Differential scanning calorimetry of SD4 revealed molecular dispersion of TLMS in Pluronic-F68. SD4 was formulated into SSCs using Gelucire 44/14 and PEG 400 as semi-solid components and PEG 6000 as a suspending agent to achieve reduction in lag time for effective drug dissolution. SSC6 showed maximum in vitro drug dissolution 97.49 % in phosphate buffer, pH 7.4 with in 20 min that was almost a three folds reduction in the time required to achieve similar dissolution by SD. Thus, SSCs present an excellent approach to enhance in vitro dissolution as well as to reduce the lag time of dissolution for poorly water soluble drugs especially to those therapeutic classes that are intended for faster onset of action. Developed approach based on HPMC capsules provided a better alternative to target delivery of telmisartan to the vegetarian population.

Phonon dispersion curves determination in (delta)-phase Pu-Ga alloys

Energy Technology Data Exchange (ETDEWEB)

Wong, J; Clatterbuck, D; Occelli, F; Farber, D; Schwartz, A; Wall, M; Boro, C; Krisch, M; Beraud, A; Chiang, T; Xu, R; Hong, H; Zschack, P; Tamura, N

2006-02-07

We have designed and successfully employed a novel microbeam on large grain sample concept to conduct high resolution inelastic x-ray scattering (HRIXS) experiments to map the full phonon dispersion curves of an fcc {delta}-phase Pu-Ga alloy. This approach obviates experimental difficulties with conventional inelastic neutron scattering due to the high absorption cross section of the common {sup 239}Pu isotope and the non-availability of large (mm size) single crystal materials for Pu and its alloys. A classical Born von-Karman force constant model was used to model the experimental results, and no less than 4th nearest neighbor interactions had to be included to account for the observation. Several unusual features including, a large elastic anisotropy, a small shear elastic modulus, (C{sub 11}-C{sub 12})/2, a Kohn-like anomaly in the T{sub 1}[011] branch, and a pronounced softening of the T[111] branch towards the L point in the Brillouin are found. These features may be related to the phase transitions of plutonium and to strong coupling between the crystal structure and the 5f valence instabilities. Our results represent the first full phonon dispersions ever obtained for any Pu-bearing material, thus ending a 40-year quest for this fundamental data. The phonon data also provide a critical test for theoretical treatments of highly correlated 5f electron systems as exemplified by recent dynamical mean field theory (DMFT) calculations for {delta}-plutonium. We also conducted thermal diffuse scattering experiments to study the T(111) dispersion at low temperatures with an attempt to gain insight into bending of the T(111) branch in relationship to the {delta} {yields} {alpha}{prime} transformation.

Phase I Trial of 2-Methoxyestradiol (2ME2, Panzem®) NanoCrystal® Dispersion (NCD®) in Advanced Solid Malignancies

Science.gov (United States)

Tevaarwerk, Amye J.; Holen, Kyle D.; Alberti, Dona B.; Sidor, Carolyn; Arnott, Jamie; Quon, Check; Wilding, George; Liu, Glenn

2010-01-01

Purpose 2-methoxyestradiol (2ME2, Panzem®) is an endogenous, estradiol-17β metabolite which at pharmacological doses exerts antimitotic and antiangiogenic activities. Studies with a 2ME2 capsule formulation showed limited oral bioavailability. We report the results of a phase I study using a NanoCrystal® Dispersion formulation of 2ME2 (2ME2 NCD). Experimental Design Patients with refractory solid tumors received 2ME2 NCD orally. Patients received drug either every six hours (Part A) or every eight hours (Part B). Doses were escalated in successive cohorts until the maximum-tolerated dose (MTD) was identified. The primary objective was identifying the MTD. Secondary objectives were to evaluate the plasma pharmacokinetics of 2ME2 and efficacy. Results In Part A, 16 patients received a median of 4 cycles of 2ME2 NCD. DLTs included fatigue (2), hypophosphatemia (2), increased ALT (1) and muscle weakness (1). Trough levels at steady state reached the minimum effective concentration in all cohorts. The MTD was determined to be 1000 mg orally every 6 hours. In Part B, 10 patients received a median of 1 cycle. DLTs included elevated γ‐glutamyltransferase (1), hyponatremia (1), fatigue (1), and anorexia (1). An MTD could not be defined for Part B, because 4/10 patients had DLTs at the initial dose level and dose reduction was not pursued. Thirteen patients had stable disease (A: 11, B: 2); there were no confirmed responses. Conclusion For 2ME2 NCD, the MTD and recommended phase II regimen is 1000 mg orally every 6 hours. Treatment was generally well tolerated. PMID:19228747

Simultaneous in situ derivatization and ultrasound-assisted dispersive magnetic solid phase extraction for thiamine determination by spectrofluorimetry.

Science.gov (United States)

Tarigh, Ghazale Daneshvar; Shemirani, Farzaneh

2014-06-01

A simple and rapid method for the simultaneous in situ derivatizaion, preconcentration and extraction of thiamine (vitamin B1) as a model analyte was developed by a novel quantitative method, namely ultrasound-assisted dispersive magnetic solid phase extraction spectrofluorimetry (USA-DMSPE-FL) from different real samples. This method consists of sample preparation, in situ derivatization, exhaustive extraction and clean up by a single process. High extraction efficiency and in situ derivatization in a short period of time is the main advantages of this procedure. For this purpose, the reusable magnetic multi-wall carbon nanotube (MMWCNT) nanocomposite was used as an adsorbent for preconcentration and determination of thiamine. Thiamine was, simultaneously, in situ derivatized as thiochrome by potassium hexacyanoferrate (III) and adsorbed on MMWCNT in an ultrasonic water bath. The MMWCNTs were then collected using an external magnetic field. Subsequently, the extracted thiochrome was washed from the surface of the adsorbent and determined by spectrofluorimetry. The developed method, which has been analytically characterized under its optimal operating conditions, allows the detection of the analyte in the samples with method detection limits of 0.37 µg L(-1). The repeatability of the method, expressed as the relative standard deviation (RSD, n=6), varies between 2.0% and 4.8% in different real samples, while the enhancement factor is 197. The proposed procedure has been applied for the determination of thiamine in biological (serum and urine), pharmaceutical (multivitamin tablet and B complex syrup) and foodstuff samples (cereal, wheat flour, banana and honey) with the good recoveries in the range from 90% to 105%. Copyright © 2014 Elsevier B.V. All rights reserved.

Enhanced systemic exposure of saquinavir via the concomitant use of curcumin-loaded solid dispersion in rats.

Science.gov (United States)

Kim, Su-A; Kim, Sung-Whan; Choi, Hoo-Kyun; Han, Hyo-Kyung

2013-08-16

The present study aimed to evaluate the effect of curcumin-loaded solid dispersion on the pharmacokinetics of saquinavir in rats. Solid dispersion (SD) formulation was prepared with Solutol® HS15 to improve the solubility and bioavailability of curcumin. Subsequently, its inhibition effect on P-gp mediated cellular efflux was examined by using NCI/ADR-RES cells overexpressing P-gp. Compared to the untreated curcumin, SD formulation enhanced the cellular uptake of rhodamine-123, a P-gp substrate by approximately 3 folds in NCI/ADR-RES cells. The oral and intravenous pharmacokinetics of saquinavir were also determined in rats with/without curcumin in the different formulations. Compared to the control given saquinavir alone, curcumin-loaded solid dispersion significantly (p<0.05) increased the oral exposure of saquinavir in rats, while it did not affect the intravenous pharmacokinetics of saquinavir. The AUC and Cmax of oral saquinavir increased by 3.8- and 2.7-folds, respectively in the presence of curcumin-loaded solid dispersion. In contrast, the untreated curcumin did not affect the oral pharmacokinetics of saquinavir. These results suggest that SD formulation of curcumin should be effective to improve the in vivo effectiveness of curcumin as an absorption enhancer, leading to the improved oral exposure of saquinavir. Copyright © 2013 Elsevier B.V. All rights reserved.

Synthesis of surface Cr (VI)-imprinted magnetic nanoparticles for selective dispersive solid-phase extraction and determination of Cr (VI) in water samples.

Science.gov (United States)

Qi, Xue; Gao, Shuang; Ding, Guosheng; Tang, An-Na

2017-01-01

A facile, rapid and selective magnetic dispersed solid-phase extraction (dSPE) method for the extraction and enrichment of Cr (VI) prior to flame atomic absorption spectrometry (AAS) was introduced. For highly selective and efficient extraction, magnetic Cr (VI)-imprinted nanoparticles (Fe 3 O 4 @ Cr (VI) IIPs) were prepared by hyphenating surface ion-imprinted with sol-gel techniques. In the preparation process, chromate (Cr(VI)) was used as the template ion; vinylimidazole and 3-aminopropyltriethoxysilane were selected as organic functional monomer and co-monomer respectively. Another reagent, methacryloxypropyltrimethoxysilane was adopted as coupling agent to form the stable covalent bonding between organic and inorganic phases. The effects of various parameters on the extraction efficiency, such as pH of sample solution, the amount of adsorbent, extraction time, the type and concentration of eluent were systematically investigated. Furthermore, the thermodynamic and kinetic properties of the adsorption process were studied to explore the internal adsorption mechanism. Under optimized conditions, the preconcentration factor, limit of detection and linear range of the established dSPE-AAS method for Cr (VI) were found to be 98, 0.29μgL -1 and 4-140μgL -1 , respectively. The developed method was also successfully applied to the analysis of Cr (VI) in different water samples with satisfactory results, proving its reliability and feasibility in real sample analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

Secondary electron emission from solid HD and a solid H2-D2 mixture

DEFF Research Database (Denmark)

Sørensen, H.; Børgesen, P.; Hao-Ming, Chen

1983-01-01

Secondary electron emission from solid HD and a solid 0.6 H2 + 0.4 D2 mixture has been studied for electron and hydrogen ion bombardment at primary energies from 0.5 to 3 keV and 2 to 10 keV/amu, respectively. The yield for solid HD is well explained by a simple stoichiometric model of the low...

5' modification of duplex DNA with a ruthenium electron donor-acceptor pair using solid-phase DNA synthesis

Science.gov (United States)

Frank, Natia L.; Meade, Thomas J.

2003-01-01

Incorporation of metalated nucleosides into DNA through covalent modification is crucial to measurement of thermal electron-transfer rates and the dependence of these rates with structure, distance, and position. Here, we report the first synthesis of an electron donor-acceptor pair of 5' metallonucleosides and their subsequent incorporation into oligonucleotides using solid-phase DNA synthesis techniques. Large-scale syntheses of metal-containing oligonucleotides are achieved using 5' modified phosporamidites containing [Ru(acac)(2)(IMPy)](2+) (acac is acetylacetonato; IMPy is 2'-iminomethylpyridyl-2'-deoxyuridine) (3) and [Ru(bpy)(2)(IMPy)](2+) (bpy is 2,2'-bipyridine; IMPy is 2'-iminomethylpyridyl-2'-deoxyuridine) (4). Duplexes formed with the metal-containing oligonucleotides exhibit thermal stability comparable to the corresponding unmetalated duplexes (T(m) of modified duplex = 49 degrees C vs T(m) of unmodified duplex = 47 degrees C). Electrochemical (3, E(1/2) = -0.04 V vs NHE; 4, E(1/2) = 1.12 V vs NHE), absorption (3, lambda(max) = 568, 369 nm; 4, lambda(max) = 480 nm), and emission (4, lambda(max) = 720 nm, tau = 55 ns, Phi = 1.2 x 10(-)(4)) data for the ruthenium-modified nucleosides and oligonucleotides indicate that incorporation into an oligonucleotide does not perturb the electronic properties of the ruthenium complex or the DNA significantly. In addition, the absence of any change in the emission properties upon metalated duplex formation suggests that the [Ru(bpy)(2)(IMPy)](2+)[Ru(acac)(2)(IMPy)](2+) pair will provide a valuable probe for DNA-mediated electron-transfer studies.

Wax Precipitation Modeled with Many Mixed Solid Phases

DEFF Research Database (Denmark)

Heidemann, Robert A.; Madsen, Jesper; Stenby, Erling Halfdan

2005-01-01

The behavior of the Coutinho UNIQUAC model for solid wax phases has been examined. The model can produce as many mixed solid phases as the number of waxy components. In binary mixtures, the solid rich in the lighter component contains little of the heavier component but the second phase shows sub......-temperature and low-temperature forms, are pure. Model calculations compare well with the data of Pauly et al. for C18 to C30 waxes precipitating from n-decane solutions. (C) 2004 American Institute of Chemical Engineers....

Electron backscatter diffraction as a useful method for alloys microstructure characterization

Energy Technology Data Exchange (ETDEWEB)

Klimek, Leszek; Pietrzyk, Bozena

2004-11-17

Microstructure examination of cast Co-Cr-Mo alloy is presented in this paper. The surface morphology and chemical composition of the alloy were investigated by means of scanning electron microscopy (SEM) and energy dispersive X-ray microanalysis (EDX). An identification of alloy phases was carried out using electron backscatter diffraction (EBSD). Two different kinds of precipitates in metallic matrix were found. They were identified as MC and M{sub 23}C{sub 6} type of carbides in Co-lattice solid solution. The advantages and limits of the EBSD method are described. It is presented that EBSD, as excellent tool for phase identification, is a valuable supplementary method for materials research.

The Extraction and Determination of Ellagic Acid Content in the Peels of Six Iranian Pomegranates Cultivars Using a New Miniaturized Matrix Solid-Phase Dispersion Method

Directory of Open Access Journals (Sweden)

Fariba Nazari Serenjeh

2017-03-01

Full Text Available Background and Aim:The peels of six Iranian pomegranates (Punica granatum L. cultivars, as a traditional medicine, were treated with a new miniaturized matrix solid-phase dispersion (MSPD method for the HPLC determination of ellagic acid (EA. Materials and Methods:In the proposed method, only 10mg of the sample powder was ground and blended with an equal amount of C18 sorbent in an agate mortar. The use of the agate mortar with smooth surface facilitated the sample transfer into a cartridge and reduced the required amount of sample and sorbent. Micro volumes of dichloromethane, n-hexane and methanol were used as modifier, washing and elution solvents, respectively. The eluate was injected into an HPLC-UV system for the analysis. Results:Several factors such as the type and amount of dispersing sorbent, modifier, washing solvent and eluent were carefully studied and optimized. Six replicated analyses at the optimized conditions resulted in a recovery of 96.7% and a relative standard deviation of 5.87%. The proposed method was successfully applied to the extraction and determination of EA in the peels samples. Conclusion:According to the ultimate results, the MSPD method is an efficient technique for the quantitative extraction of EA from the peels of pomegranate. Malas cultivar has the highest amount (18.1 g kg-1 of ellagic acid content compared to the other studied pomegranate cultivars.

Ultra-sensitive speciation analysis of mercury by CE-ICP-MS together with field-amplified sample stacking injection and dispersive solid-phase extraction.

Science.gov (United States)

Chen, YiQuan; Cheng, Xian; Mo, Fan; Huang, LiMei; Wu, Zujian; Wu, Yongning; Xu, LiangJun; Fu, FengFu

2016-04-01

A simple dispersive solid-phase extraction (DSPE) used to extract and preconcentrate ultra-trace MeHg, EtHg and Hg(2+) from water sample, and a sensitive method for the simultaneous analysis of MeHg, EtHg and Hg(2+) by using capillary electrophoresis-inductively coupled plasma mass spectrometry (CE-ICP-MS) with field-amplified sample stacking injection (FASI) were first reported in this study. The DSPE used thiol cotton particles as adsorbent, and is simple and effective. It can be used to extract and preconcentrate ultra-trace mercury compounds in water samples within 30 min with a satisfied recovery and no mercury species alteration during the process. The FASI enhanced the sensitivity of CE-ICP-MS with 25-fold, 29-fold and 27-fold for MeHg, EtHg and Hg(2+) , respectively. Using FASI-CE-ICP-MS together with DSPE, we have successfully determined ultra-trace MeHg, EtHg and Hg(2+) in tap water with a limits of quantification (LOQs) of 0.26-0.45 pg/mL, an RSD (n = 3) mercury. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A simple and sensitive approach to quantify methyl farnesoate in whole arthropods by matrix-solid phase dispersion and gas chromatography-mass spectrometry.

Science.gov (United States)

Montes, Rosa; Rodil, Rosario; Neuparth, Teresa; Santos, Miguel M; Cela, Rafael; Quintana, José Benito

2017-07-28

Methyl farnesoate (MF) is an arthropod hormone that plays a key role in the physiology of several arthropods' classes being implicated in biological processes such as molting and reproduction. The development of an analytical technique to quantify the levels of this compound in biological tissues can be of major importance for the field of aquaculture/apiculture conservation and in endocrine disruption studies. Therefore, the aim of this study was to develop a simple and sensitive method to measure native levels of MF in the tissue of three representative species from different arthropods classes with environmental and/or economic importance. Thus, a new approach using whole organisms and the combination of matrix solid-phase dispersion with gas chromatography coupled to mass spectrometry was developed. This method allows quantifying endogenous MF at low levels (LOQs in the 1.2-3.1ng/g range) in three arthropod species, and could be expanded to additional arthropod classes. The found levels ranged between 2 and 12ng/g depending on the studied species and gender. The overall recovery of the method was evaluated and ranged between 69 and 96%. Copyright © 2017 Elsevier B.V. All rights reserved.

Observation of strongly forbidden solid effect dynamic nuclear polarization transitions via electron-electron double resonance detected NMR

Energy Technology Data Exchange (ETDEWEB)

Smith, Albert A.; Corzilius, Björn; Haze, Olesya; Swager, Timothy M.; Griffin, Robert G., E-mail: rgg@mit.edu [Department of Chemistry and Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States)

2013-12-07

We present electron paramagnetic resonance experiments for which solid effect dynamic nuclear polarization transitions were observed indirectly via polarization loss on the electron. This use of indirect observation allows characterization of the dynamic nuclear polarization (DNP) process close to the electron. Frequency profiles of the electron-detected solid effect obtained using trityl radical showed intense saturation of the electron at the usual solid effect condition, which involves a single electron and nucleus. However, higher order solid effect transitions involving two, three, or four nuclei were also observed with surprising intensity, although these transitions did not lead to bulk nuclear polarization—suggesting that higher order transitions are important primarily in the transfer of polarization to nuclei nearby the electron. Similar results were obtained for the SA-BDPA radical where strong electron-nuclear couplings produced splittings in the spectrum of the indirectly observed solid effect conditions. Observation of high order solid effect transitions supports recent studies of the solid effect, and suggests that a multi-spin solid effect mechanism may play a major role in polarization transfer via DNP.

In situ electron holography of electric potentials inside a solid-state electrolyte: Effect of electric-field leakage

Energy Technology Data Exchange (ETDEWEB)

Aizawa, Yuka; Yamamoto, Kazuo; Sato, Takeshi [Nanostructures Research Laboratory, Japan Fine Ceramics Center, 2-4-1 Mutsuno, Atsuta-ku, Nagoya, Aichi 456-8587 (Japan); Murata, Hidekazu [Faculty of Science and Technology, Meijo University, 1-501 Shiogamaguchi, Tempaku-ku, Nagoya, Aichi 468-8502 (Japan); Yoshida, Ryuji; Fisher, Craig A.J. [Nanostructures Research Laboratory, Japan Fine Ceramics Center, 2-4-1 Mutsuno, Atsuta-ku, Nagoya, Aichi 456-8587 (Japan); Kato, Takehisa; Iriyama, Yasutoshi [Department of Materials, Physics and Energy Engineering, Nagoya University, Furo-cho, Chikusa-ku, Nagoya, Aichi 464-8601 (Japan); Hirayama, Tsukasa, E-mail: t-hirayama@jfcc.or.jp [Nanostructures Research Laboratory, Japan Fine Ceramics Center, 2-4-1 Mutsuno, Atsuta-ku, Nagoya, Aichi 456-8587 (Japan)

2017-07-15

In situ electron holography is used to observe changes of electric-potential distributions in an amorphous lithium phosphorus oxynitride (LiPON) solid-state electrolyte when different voltages are applied. 2D phase images are simulated by integrating the 3D potential distribution along the electron trajectory through a thin Cu/LiPON/Cu region. Good agreement between experimental and simulated phase distributions is obtained when the influence of the external electric field is taken into account using the 3D boundary-charge method. Based on the precise potential changes, the lithium-ion and lithium-vacancy distributions inside the LiPON layer and electric double layers (EDLs) are inferred. The gradients of the phase drops at the interfaces in relation to EDL widths are discussed. - Highlights: • Solid-state electrolyte LiPON has been observed by in situ electron holography. • Observed phase distributions are compared with those simulated numerically. • 3D electric fields around the specimen are taken into account in the simulation. • Electric-potential distributions inside LiPON have been obtained. • The lithium-ion and lithium-vacancy distributions inside the LiPON are inferred.

Effect of silica nanoparticles on the phase inversion of liquid-liquid dispersions

International Nuclear Information System (INIS)

Asadabadi, Maliheh Raji; Abolghasemi, Hossein; Nasab, Payman Davoodi; Maragheh, Mohammad Ghannadi

2013-01-01

The effect of silica nanoparticles on phase inversion of liquid-liquid dispersions in a stirred vessel was investigated. The studied systems were toluene dispersed in water and vice versa. In the first set of experiments, phase inversion behavior of systems without Silica nanoparticles was evaluated and subsequent experiments were conducted in the presence of the nanoparticles. For this purpose, Silica nanoparticles of different concentrations (0.01, 0.03, 0.05, 0.07 wt%) were dispersed in water. The nanofluid stability was examined using an ultraviolet-visible (UV-vis) spectrophotometer. The results indicated that increase in silica nanoparticle concentrations up to 0.07 wt% led to increase in agitation speed of phase inversion 43-53.5% and 38.5-45% in the case of O/W and W/O dispersions, respectively. Consequently, the tendency of dispersions to inversion diminished as nanoparticle concentrations increased. Finally, 0.05 wt% of silica nanoparticle was selected as the optimum on the range studied

Convoy electron production by heavy ions in solids

International Nuclear Information System (INIS)

Sellin, I.A.

1984-01-01

The term convoy electron refers to those electrons ejected in fast ion-atom and ion-solid collisions closely matched in vector velocity to that of the incident heavy particles responsible for their ejection. Similarities and differences among electrons ejected into such states through binary electron capture to continuum and electron loss to continuum processes in single ion-atom encounters are compared and contrasted to more complex ejection processes occurring in solid targets. Puzzles posed by the apparent strong projectile Z dependence but weak emergent ion charge dependence of the yield in the case of solid targets are reviewed. Very recent progress in resolving these puzzles has been made by recent observations that the apparent mean free path for electron scattering out of the forward direction within the target is observed to be an order of magnitude greater than that for free electrons of equal velocity provided the projectile charge is high. 13 references, 2 figures, 1 table

Solid - solid and solid - liquid phase transitions of iron and iron alloys under laser shock compression

Science.gov (United States)

Harmand, M.; Krygier, A.; Appel, K.; Galtier, E.; Hartley, N.; Konopkova, Z.; Lee, H. J.; McBride, E. E.; Miyanishi, K.; Nagler, B.; Nemausat, R.; Vinci, T.; Zhu, D.; Ozaki, N.; Fiquet, G.

2017-12-01

An accurate knowledge of the properties of iron and iron alloys at high pressures and temperatures is crucial for understanding and modelling planetary interiors. While Earth-size and Super-Earth Exoplanets are being discovered in increasingly large numbers, access to detailed information on liquid properties, melting curves and even solid phases of iron and iron at the pressures and temperatures of their interiors is still strongly limited. In this context, XFEL sources coupled with high-energy lasers afford unique opportunities to measure microscopic structural properties at far extreme conditions. Also the achievable time resolution allows the shock history and phase transition mechanisms to be followed during laser compression, improving our understanding of the high pressure and high strain experiments. Here we present recent studies devoted to investigate the solid-solid and solid-liquid transition in laser-shocked iron and iron alloys (Fe-Si, Fe-C and Fe-O alloys) using X-ray diffraction and X-ray diffuse scattering. Experiment were performed at the MEC end-station of the LCLS facility at SLAC (USA). Detection of the diffuse scattering allowed the identification of the first liquid peak position along the Hugoniot, up to 4 Mbar. The time resolution shows ultrafast (between several tens and several hundreds of picoseconds) solid-solid and solid-liquid phase transitions. Future developments at XFEL facilities will enable detailed studies of the solid and liquid structures of iron and iron alloys as well as out-of-Hugoniot studies.

A four phases model to simulate the dispersion of 226Ra, 238U and 232Th in an estuary affected by phosphate rock processing

International Nuclear Information System (INIS)

Perianez, R.; Abril, J.M.; Garcia-Leon, M.

1997-01-01

A numerical model to simulate the dispersion of non conservative radionuclides in tidal waters has been developed. The model includes four phases: water, suspended matter and two grain size sediment fractions. Ionic exchanges between water and the solid phases have been formulated in terms of kinetic transfer coefficients instead of distribution coefficients, because the model was developed for nonequilibrium conditions. The model simultaneously solves the shallow water hydrodynamic equations, the suspended matter dispersion equation and the four equations which give the time evolution of specific activity in each phase. The model has been applied to the Odiel river (southwest Spain), where a phosphate complex releases its wastes. It gives good results in predicting concentrations of 226 Ra, 238 U and 232 Th in water, suspended matter, distribution coefficients and Th/U mass rations. (author)

Streamlined sample cleanup using combined dispersive solid-phase extraction and in-vial filtration for analysis of pesticides and environmental pollutants in shrimp

Energy Technology Data Exchange (ETDEWEB)

Han, Lijun [College of Science, China Agricultural University, Beijing (China); Sapozhnikova, Yelena [U.S. Dept. of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA 19038 (United States); Lehotay, Steven J., E-mail: Steven.Lehotay@ars.usda.gov [U.S. Dept. of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA 19038 (United States)

2014-05-01

Highlights: • The first report that combines in-vial filtration and dispersive-SPE for sample cleanup. • The unique application of ammonium formate for salting-out partitioning in QuEChERS. • Evaluations of a new zirconium-based and a non-friable GCB sorbent for d-SPE cleanup. • A new analytical method for 59 pesticides and environmental pollutants in shrimp. Abstract: A new method of sample preparation was developed and is reported for the first time. The approach combines in-vial filtration with dispersive solid-phase extraction (d-SPE) in a fast and convenient cleanup of QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts. The method was applied to simultaneous analysis of 42 diverse pesticides and 17 environmental contaminants, including polycyclic aromatic hydrocarbons, polychlorinated biphenyls (PCBs), and flame retardants, in shrimp as the sample matrix. Final extracts were analyzed by both low-pressure gas chromatography – triple quadrupole tandem mass spectrometry (LPGC-MS/MS), and high-performance liquid chromatography – triple quadrupole tandem mass spectrometry (HPLC-MS/MS) to provide a wide scope of analysis for targeted analytes. During method development, several different commercial sorbents for d-SPE were investigated and compared with respect to analyte recoveries. The method was validated at 10, 50, and 100 ng g⁻¹ spiking levels (10-fold lower for PCBs), and the results for nearly all analytes were between 70 and 115% recoveries with ≤17% relative standard deviations. The method was shown to be simple, fast, and effective for multi-application analysis of chemical residues in the representative food and environmental marker matrix.

A Simple Vortex-Assisted Magnetic Dispersive Solid Phase Microextraction System for Preconcentration and Separation of Triazine Herbicides from Environmental Water and Vegetable Samples Using Fe₃O₄@MIL-100(Fe) Sorbent.

Science.gov (United States)

Nasrollahpour, Atefe; Moradi, Seyyed Ershad

2018-04-04

A vortex-assisted magnetic dispersive solid phase microextraction coupled with high-performance liquid chromatography has been developed for the extraction and determination of triazine herbicides by using magnetic metal organic frameworks [Fe₃O₄@MIL-100(Fe)] in environmental water and vegetable samples. The Fe₃O₄@MIL-100(Fe) composite has been characterized by using X-ray diffraction spectroscopy, tunneling electron microscopy, thermogravimetric measurement, and Brunauer-Emmett-Teller analysis. The method is based on the sorption of triazine herbicides on Fe₃O₄@MIL-100(Fe) because of the complex formation between iron oxide nanoparticles and triazine herbicides beside π-π interactions between organic parts of Fe₃O₄@MIL-100(Fe) and triazine herbicides. The experimental parameters for the preconcentration of triazine herbicides, such as the type and volume of the eluent, pH, time of the sorption and desorption, and the amount of the sorbent, were optimized. Under the optimized conditions, the method was linear over the concentration range of 0.0061 to 70 ng/mL for each triazine herbicide, and the correlation coefficients ranged from 0.9988 to 0.9997. The limit of detection of the method at a signal-to-noise ratio of 3 was 2.0 to 5.3 ng/mL. The relative standard deviations for inter- and intraday assays were in the range of 5.8 to 10.2% and 3.8 to 6.3%, respectively.

Multiple solid-phase microextraction

NARCIS (Netherlands)

Koster, EHM; de Jong, GJ

2000-01-01

Theoretical aspects of multiple solid-phase microextraction are described and the principle is illustrated with the extraction of lidocaine from aqueous solutions. With multiple extraction under non-equilibrium conditions considerably less time is required in order to obtain an extraction yield that

Solid dispersions in oncology: a solution to solubility-limited oral drug absorption

NARCIS (Netherlands)

Sawicki, Emilia

2017-01-01

This thesis discusses the formulation method solid dispersion and how it works to resolve solubility-limited absorption of orally dosed anticancer drugs. Dissolution in water is essential for drug absorption because only dissolved drug molecules are absorbed. The problem is that half of the arsenal

Understanding the generation and maintenance of supersaturation during the dissolution of amorphous solid dispersions using modulated DSC and 1H NMR.

Science.gov (United States)

Baghel, Shrawan; Cathcart, Helen; O'Reilly, Niall J

2018-01-30

In this study, the dissolution behaviour of dipyridamole (DPM) and cinnarizine (CNZ) spray-dried amorphous solid dispersions (ASDs) using polyvinyl pyrrolidone (PVP) and polyacrylic acid (PAA) as a carrier matrix were evaluated and compared. The drug concentrations achieved from the dissolution of PVP and PAA solid dispersions were significantly greater than the equilibrium solubility of crystalline DPM and CNZ in phosphate buffer pH 6.8 (PBS 6.8). The maximum drug concentration achieved by dissolution of PVP and PAA solid dispersions did not exceed the theoretically calculated apparent solubility of amorphous DPM and CNZ. However, the degree of supersaturation of DPM and CNZ increased considerably as the polymer weight fraction within the solid dispersion increased. In addition, the supersaturation profile of DPM and CNZ were studied in the presence and absence of the polymers. PAA was found to maintain a higher level of supersaturation compared to PVP. The enhanced drug solution concentration following dissolution of ASDs can be attributed to the reduced crystal growth rates of DPM and CNZ at an equivalent supersaturation. We have also shown that, for drugs having high crystallization tendency and weak drug-polymer interaction, the feasible way to increase dissolution might be increase the polymer weight fraction in the ASD. Solution 1 H NMR spectra were used to understand dissolution mechanism and to identify drug-polymer interaction. The change in electron densities of proton attached to different groups in DPM and CNZ suggested drug-polymer interaction in solution. The relative intensities of peak shift and nature of interaction between drug and polymer in different systems are different. These different effects suggest that DPM and CNZ interacts in a different way with PVP and PAA in solution which goes some way towards explaining the different polymeric effect, particularly in terms of inhibition of drug recrystallization and dissolution of DPM and CNZ ASDs

Mechanical and Tribological Characteristics of TIG Hardfaced Dispersive Layer by Reinforced with Particles Extruded Aluminium

Directory of Open Access Journals (Sweden)

R. Dimitrova

2017-05-01

Full Text Available The article presents the results of the implemented technology for generation of hardfaced dispersive layers obtained by additive material containing reinforcing phase of non-metal particles. The wear resistant coatings are deposited on pure aluminium metal matrix by shielded gas metal-arc welding applying tungsten inert gas (TIG with extruded aluminium wire reinforced by particles as additive material. Wire filler is produced by extrusion of a pack containing metalized and plated by flux micro/nano SiC particles. The metalized particles implanting in the metal matrix and its dispersive hardfacing are realized by solid-state welding under conditions of hot plastic deformation. Tribological characteristics are studied of the hardfaced layers of dispersive reinforced material on pure aluminium metal matrix with and without flux. Hardness profiles of the hardfaced layers are determined by nanoindentation. The surface layers are studied by means of Scanning Electron Microscopy (SEM and Energy Dispersive X-ray (EDX analysis. Increase by 15-31 % of the wear resistance of the hardfaced layers and 30-40 % of their hardness was found, which is due to the implanted in the layer reinforcing phase of metalized micro/nano SiC particles.

Hydrodynamic and thermal modeling of solid particles in a multi-phase, multi-component flow

International Nuclear Information System (INIS)

Tentner, A.M.; Wider, H.U.

1984-01-01

This paper presents the new thermal hydraulic models describing the hydrodynamics of the solid fuel/steel chunks during an LMFBR hypothetical core disruptive accident. These models, which account for two-way coupling between the solid and fluid phases, describe the mass, momentum and energy exchanges which occur when the chunks are present at any axial location. They have been incorporated in LEVITATE, a code for the analysis of fuel and cladding dynamics under Loss-of-Flow (LOF) conditions. Their influence on fuel motion is presented in the context of the L6 TREAT experiment analysis. It is shown that the overall hydrodynamic behavior of the molten fuel and solid fuel chunks is dependent on both the size of the chunks and the power level. At low and intermediate power levels the fuel motion is more dispersive when small chunks, rather than large ones, are present. At high power levels the situation is reversed

Electron emission from solids induced by swift heavy ions

International Nuclear Information System (INIS)

Xiao Guoqing