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Sample records for solid dispersion technique

  1. 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...

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

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    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.

  3. 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 ...

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

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    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.

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

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    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.

  6. Enhancement of carvedilol solubility by solid dispersion technique using cyclodextrins, water soluble polymers and hydroxyl acid.

    Science.gov (United States)

    Yuvaraja, K; Khanam, Jasmina

    2014-08-05

    Aim of the present work is to enhance aqueous solubility of carvedilol (CV) by solid dispersion technique using wide variety of carriers such as: β-cyclodextrin (βCD), hydroxypropyl-β-cyclodextrin (HPβCD), tartaric acid (TA), polyvinyl pyrrolidone K-30 (PVP K-30) and poloxamer-407 (PLX-407). Various products of 'CV-solid dispersion' had been studied extensively in various pH conditions to check enhancement of solubility and dissolution characteristics of carvedilol. Any physical change upon interaction between CV and carriers was confirmed by instrumental analysis: XRD, DSC, FTIR and SEM. Negative change of Gibb's free energy and complexation constants (Kc, 75-240M(-1), for cyclodextrins and 1111-20,365M(-1), for PVP K-30 and PLX-407) were the evidence of stable nature of the binding between CV and carriers. 'Solubility enhancement factor' of ionized-CV was found high enough (340 times) with HPβCD in presence of TA. TA increases the binding efficiency of cyclodextrin and changing the pH of microenvironment in dissolution medium. In addition, ionization process was used to increase the apparent intrinsic solubility of drug. In vitro, dissolution time of CV was remarkably reduced in the solid dispersion system compared to that of pure drug. This may be attributed to increased wettability, dispersing ability and transformation of crystalline state of drug to amorphous one. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. 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.

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

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    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.

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

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    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.

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

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    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.

  11. Preparation and characterization of fast dissolving flurbiprofen and esomeprazole solid dispersion using spray drying technique.

    Science.gov (United States)

    Pradhan, Roshan; Tran, Tuan Hiep; Kim, Sung Yub; Woo, Kyu Bong; Choi, Yong Joo; Choi, Han-Gon; Yong, Chul Soon; Kim, Jong Oh

    2016-04-11

    We aimed to develop an immediate-release flurbiprofen (FLU) and esomeprazole (ESO) combination formulation with enhanced gastric aqueous solubility and dissolution rate. Aqueous solubility can be enhanced by formulating solid dispersions (SDs) with a polyvinylpyrrolidone (PVP)-K30 hydrophilic carrier, using spray-drying technique. Aqueous and gastric pH dissolution can be achieved by macro-environmental pH modulation using sodium bicarbonate (NaHCO3) and magnesium hydroxide (Mg(OH)2) as the alkaline buffer. FLU/ESO-loaded SDs (FLU/ESO-SDs) significantly improved aqueous solubility of both drugs, compared to each drug powder. Dissolution studies in gastric pH and water were compared with the microenvironmental pH modulated formulations. The optimized FLU/ESO-SD powder formulation consisted of FLU/ESO/PVP-K30/sodium carbonate (Na2CO3) in a weight ratio 1:0.22:1.5:0.3, filled in the inner capsule. The outer capsule consisted of NaHCO3 and Mg(OH)2, which created the macro-environmental pH modulation. Increased aqueous and gastric pH dissolution of FLU and ESO from the SD was attributed to the alkaline buffer effects and most importantly, to drug transformation from crystalline to amorphous SD powder, clearly revealed by scanning electron microscopy, differential scanning calorimetry, and powder X-ray diffraction studies. Thus, the combined FLU and ESO SD powder can be effectively delivered as an immediate-release formulation using the macro-environmental pH modulation concept. Copyright © 2016. Published by Elsevier B.V.

  12. 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

  13. 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.

  14. Application of film-casting technique to investigate drug-polymer miscibility in solid dispersion and hot-melt extrudate.

    Science.gov (United States)

    Parikh, Tapan; Gupta, Simerdeep Singh; Meena, Anuprabha K; Vitez, Imre; Mahajan, Nidhi; Serajuddin, Abu T M

    2015-07-01

    Determination of drug-polymer miscibility is critical for successful development of solid dispersions. This report details a practical method to predict miscibility and physical stability of drug with various polymers in solid dispersion and, especially, in melt extrudates by applying a film-casting technique. Mixtures of itraconazole (ITZ) with hydroxypropylmethylcellulose phthalate (HPMCP), Kollidon(®) VA 64, Eudragit(®) E PO, and Soluplus(®) were film-casted, exposed to 40°C/75% RH for 1 month and then analyzed using differential scanning calorimetry (DSC), powder X-ray diffractometry, and polarized light microscopy (PLM). ITZ had the highest miscibility with HPMCP, being miscible at drug to polymer ratio of 6:4 (w/w). There was a downward trend of lower miscibility with Soluplus(®) (miscible at 3:7, w/w, and a few microcrystals present at 4:6, w/w), Kollidon(®) VA 64 (2:8, w/w) and Eudragit(®) E PO (casting and hot-melt extrusion (HME) using a twin screw extruder. For ITZ-Soluplus(®) mixtures, HME at 4:6 (w/w) resulted in a single phase, whereas drug crystallization was observed at higher drug load. HME of ITZ-Kollidon(®) VA 64 mixtures also correlated well with the miscibility predicted by film casting. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

  15. Enhanced dissolution and oral bioavailability of valsartan solid dispersions prepared by a freeze-drying technique using hydrophilic polymers.

    Science.gov (United States)

    Xu, Wei-Juan; Xie, Hong-Juan; Cao, Qing-Ri; Shi, Li-Li; Cao, Yue; Zhu, Xiao-Yin; Cui, Jing-Hao

    2016-01-01

    This study aimed to improve the dissolution rate and oral bioavailability of valsartan (VAL), a poorly soluble drug using solid dispersions (SDs). The SDs were prepared by a freeze-drying technique with polyethylene glycol 6000 (PEG6000) and hydroxypropylmethylcellulose (HPMC 100KV) as hydrophilic polymers, sodium hydroxide (NaOH) as an alkalizer, and poloxamer 188 as a surfactant without using any organic solvents. In vitro dissolution rate and physicochemical properties of the SDs were characterized using the USP paddle method, differential scanning calorimetry (DSC), X-ray diffractometry (XRD) and Fourier transform-infrared (FT-IR) spectroscopy, respectively. In addition, the oral bioavailability of SDs in rats was evaluated by using VAL (pure drug) as a reference. The dissolution rates of the SDs were significantly improved at pH 1.2 and pH 6.8 compared to those of the pure drug. The results from DSC, XRD showed that VAL was molecularly dispersed in the SDs as an amorphous form. The FT-IR results suggested that intermolecular hydrogen bonding had formed between VAL and its carriers. The SDs exhibited significantly higher values of AUC 0-24 h and Cmax in comparison with the pure drug. In conclusion, hydrophilic polymer-based SDs prepared by a freeze-drying technique can be a promising method to enhance dissolution rate and oral bioavailability of VAL.

  16. 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

  17. Fabrication and evaluation of pH-modulated solid dispersion for telmisartan by spray-drying technique.

    Science.gov (United States)

    Marasini, Nirmal; Tran, Tuan Hiep; Poudel, Bijay Kumar; Cho, Hyuk Jun; Choi, Young Keun; Chi, Sang-Cheol; Choi, Han-Gon; Yong, Chul Soon; Kim, Jong Oh

    2013-01-30

    The present study was undertaken to overcome the problems associated with solubility, dissolution and oral bioavailability of a poorly water-soluble ionizable drug, telmisartan (TMS). For these purposes, a solubility test was carried to select the appropriate formulation composition from various carriers and alkalizers. Solid dispersions (SDs) of TMS were prepared at different drug-to-carrier ratios by the spray-drying technique, and were characterized by dissolution and aqueous solubility studies. The optimum formulation was investigated by dissolution studies at different pH and water media and its solid state characterisations were performed by scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and X-ray diffraction (XRD) studies. In solubility and dissolution tests, all TMS-loaded pH-modulated SDs (pH(M)-SDs) exhibited marked improvement in the dissolution behavior when compared with crystalline TMS powder. The optimum formulation of pH(M)-SD consisted of TMS/PVP (polyvinylpyrrolidone) K30/Na(2)CO(3) at a weight ratio of 2/0.5/3 and showed significant improvement in the aqueous solubility and dissolution rate by approximately 40,000- and 3-fold, respectively, compared to TMS powder. Solid-state characterization revealed the changed in crystallinity of TMS into amorphous state. Furthermore, area under the drug concentration time-curve (AUC) of TMS from the pH(M)-SD increased by 13.4- and 2.1-fold, compared with TMS powder and commercial product, respectively. According to these observations, taken together with dissolution and pharmacokinetic behaviors, pH-modulated SD in the presence of an alkalizer for a poorly water-soluble ionizable drug, TMS, appeared to be efficacious for enhancing its bioavailability. Copyright © 2012 Elsevier B.V. All rights reserved.

  18. 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

  19. Effervescence-assisted dispersive liquid-liquid microextraction using a solid effervescent agent as a novel dispersion technique for the analysis of fungicides in apple juice.

    Science.gov (United States)

    Jiang, Wenqing; Chen, Xiaochu; Liu, Fengmao; You, Xiangwei; Xue, Jiaying

    2014-11-01

    A novel effervescence-assisted dispersive liquid-liquid microextraction method has been developed for the determination of four fungicides in apple juice samples. In this method, a solid effervescent agent is added into samples to assist the dispersion of extraction solvent. The effervescent agent is environmentally friendly and only produces an increase in the ionic strength and a negligible variation in the pH value of the aqueous sample, which does not interfere with the extraction of the analytes. The parameters affecting the extraction efficiency were investigated including the composition of effervescent agent, effervescent agent amount, formulation of effervescent agent, adding mode of effervescent agent, type and volume of extraction solvent, and pH. Under optimized conditions, the method showed a good linearity within the range of 0.05-2 mg/L for pyrimethanil, fludioxonil, and cyprodinil, and 0.1-4 mg/L for kresoxim-methyl, with the correlation coefficients >0.998. The limits of detection for the method ranged between 0.005 and 0.01 mg/L. The recoveries of the target fungicides in apple juice samples were in the range of 72.4-110.8% with the relative standard deviations ranging from 1.2 to 6.8%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. 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 ...

  1. 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 ...

  2. DEVELOPMENT OF SUSTAINED RELEASE TABLETS CONTAINING SOLID DISPERSIONS OF BACLOFEN

    Directory of Open Access Journals (Sweden)

    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.

  3. DEVELOPMENT OF SUSTAINED RELEASE TABLETS CONTAINING SOLID DISPERSIONS OF BACLOFEN

    Directory of Open Access Journals (Sweden)

    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.

  4. 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

  5. Spray drying formulation of amorphous solid dispersions.

    Science.gov (United States)

    Singh, Abhishek; Van den Mooter, Guy

    2016-05-01

    Spray drying is a well-established manufacturing technique which can be used to formulate amorphous solid dispersions (ASDs) which is an effective strategy to deliver poorly water soluble drugs (PWSDs). However, the inherently complex nature of the spray drying process coupled with specific characteristics of ASDs makes it an interesting area to explore. Numerous diverse factors interact in an inter-dependent manner to determine the final product properties. This review discusses the basic background of ASDs, various formulation and process variables influencing the critical quality attributes (CQAs) of the ASDs and aspects of downstream processing. Also various aspects of spray drying such as instrumentation, thermodynamics, drying kinetics, particle formation process and scale-up challenges are included. Recent advances in the spray-based drying techniques are mentioned along with some future avenues where major research thrust is needed. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. 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

  7. 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

    NARCIS (Netherlands)

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

    2006-01-01

    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

  8. 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 ...

  9. 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.

  10. 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, ...

  11. 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...

  12. Fundamental aspects of solid dispersion technology for poorly soluble drugs

    Directory of Open Access Journals (Sweden)

    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.

  13. 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.

  14. 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

  15. 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.

  16. Cefuroxime axetil solid dispersions prepared using solution enhanced dispersion by supercritical fluids.

    Science.gov (United States)

    Jun, Seoung Wook; Kim, Min-Soo; Jo, Guk Hyun; Lee, Sibeum; Woo, Jong Soo; Park, Jeong-Sook; Hwang, Sung-Joo

    2005-12-01

    Cefuroxime axetil (CA) solid dispersions with HPMC 2910/PVP K-30 were prepared using solution enhanced dispersion by supercritical fluids (SEDS) in an effort to increase the dissolution rate of poorly water-soluble drugs. Their physicochemical properties in solid state were characterized by differential scanning calorimeter (DSC), powder X-ray diffraction (PXRD), Fourier transform infrared spectrometry (FT-IR) and scanning electron microscopy. No endothermic and characteristic diffraction peaks corresponding to CA were observed for the solid dispersions in DSC and PXRD. FTIR analysis demonstrated the presence of intermolecular hydrogen bonds between CA and HPMC 2910/PVP K-30 in solid dispersions, resulting in the formation of amorphous or non-crystalline CA. Dissolution studies indicated that the dissolution rates were remarkably increased in solid dispersions compared with those in the physical mixture and drug alone. In conclusion, an amorphous or non-crystalline CA solid dispersion prepared using SEDS could be very useful for the formulation of solid dosage forms.

  17. Magnetic nanoparticles based dispersive micro-solid-phase extraction as a novel technique for coextraction of acidic and basic drugs from biological fluids and waste water.

    Science.gov (United States)

    Asgharinezhad, Ali Akbar; Mollazadeh, Narges; Ebrahimzadeh, Homeira; Mirbabaei, Fatemeh; Shekari, Nafiseh

    2014-04-18

    The coextraction of acidic and basic drugs from different samples is a considerable and disputable concept in sample preparation strategies. In this study, for the first time, simultaneous extraction of acidic and basic drugs with magnetic nanoparticles based dispersive micro-solid phase extraction followed by high performance liquid chromatography-ultraviolet detection was introduced. Cetyltrimethyl ammonium bromide-coated Fe3O4@decanoic acid as an efficient sorbent was successfully applied to adsorb diclofenac (DIC) as an acidic and diphenhydramine (DPH) as a basic model compound. First, appropriate amount of synthetic Fe3O4@decanoic acid nanoparticles was added to aqueous solution of drugs. After adjusting the pH of the solution, cetyltrimethyl ammonium bromide (CTAB) was added to the mixture being stirred at a constant rate. After the adsorption of drugs and decantation of supernatant with a magnetic field, the sorbent was eluted with methanol by fierce vortex. The parameters affecting the extraction efficiency were optimized and obtained as: pH of the sample=9, concentration of CTAB=0.2mmolL(-1), amount of sorbent=10mg, extraction time=5min, no salt addition to sample, type and volume of the eluent=50μL methanol, and desorption time=1min. Under the optimum conditions detection limits and linear dynamic ranges were achieved in the range of 1.8-3.0, 5-1500μgL(-1) for DPH and 1.5-3.5, 5-1500μgL(-1) for DIC, respectively. The percent of extraction recovery and relative standard deviations (n=5) were in the range of 47.3-60, 5.2-9.0 for DPH and 64-76.7, 5.1-5.8 for DIC, respectively. Ultimately, the applicability of the method was successfully confirmed by the extraction and determination of DIC and DPH in human urine, plasma and waste water samples in the range of microgram per liter and satisfactory results were obtained. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. Solubilization of poorly water-soluble drugs using solid dispersions.

    Science.gov (United States)

    Tran, Thao T-D; Tran, Phuong H-L; Khanh, Tran N; Van, Toi V; Lee, Beom-Jin

    2013-08-01

    Many new drugs have been discovered in pharmaceutical industry and exposed their surprised potential therapeutic effects. Unfortunately, these drugs possess low absorption and bioavailability since their solubility limitation in water. Solid dispersion (SD) is the current technique gaining so many attractions from scientists due to its effect on improving solubility and dissolution rate of poorly water-soluble drugs. A number of patents including the most recent inventions have been undertaken in this review to address various respects of this strategy in solubilization of poorly watersoluble drugs including type of carriers, preparation methods and view of technologies used to detect SD properties and mechanisms with the aim to accomplish a SD not only effective on enhanced bioavailability but also overcome difficulties associated with stability and production. Future prospects are as well discussed with an only hope that many developments and researches in this field will be successfully reached and contributed to commercial use for treatment as much as possible.

  6. Solid dispersions enhance solubility, dissolution, and permeability of thalidomide.

    Science.gov (United States)

    Barea, Silvana A; Mattos, Cristiane B; Cruz, Ariadne C C; Chaves, Vitor C; Pereira, Rafael N; Simões, Claudia M O; Kratz, Jadel M; Koester, Letícia S

    2017-03-01

    Thalidomide (THD) is a BCS class II drug with renewed and growing therapeutic applicability. Along with the low aqueous solubility, additional poor biopharmaceutical properties of the drug, i.e. chemical instability, high crystallinity, and polymorphism, lead to a slow and variable oral absorption. In this view, we developed solid dispersions (SDs) containing THD dispersed in different self-emulsifying carriers aiming at an enhanced absorption profile for the drug. THD was dispersed in lauroyl macrogol-32 glycerides (Gelucire ® 44/14) and α-tocopherol polyethylene glycol succinate (Kolliphor ® TPGS), in the presence or absence of the precipitation inhibitor polyvinylpyrrolidone K30 (PVP K30), by means of the solvent method. Physicochemical analysis revealed the formation of semicrystalline SDs. X-ray diffraction and infrared spectroscopy analyses suggest that the remaining crystalline fraction of the drug in the SDs did not undergo polymorphic transition. The impact of the solubility-enhancing formulations on the THD biopharmaceutical properties was evaluated by several in vitro techniques. The developed SDs were able to increase the apparent solubility of the drug (up to 2-3x the equilibrium solubility) for a least 4 h. Dissolution experiments (paddle method, 75 rpm) in different pHs showed that around 80% of drug dissolved after 120 min (versus 40% of pure crystalline drug). Additionally, we demonstrated the enhanced solubility obtained via SDs could be translated into increased flux in a parallel artificial membrane permeability assay (PAMPA). In summary, the results demonstrate that SDs could be considered an interesting and unexplored strategy to improve the biopharmaceutical properties of THD, since SDs of this important drug have yet to be reported.

  7. 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.

  8. 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.

  9. Dispersive solid-phase imprinting of proteins for the production of plastic antibodies

    DEFF Research Database (Denmark)

    Ashley, Jon; Feng, Xiaotong; Halder, Arnab

    2018-01-01

    We describe a novel dispersive solid-phase imprinting technique for the production of nano-sized molecularly imprinted polymers (nanoMIPs) as plastic antibodies. The template was immobilized on in-house synthesized magnetic microspheres instead of conventional glass beads. As a result, high...

  10. 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.

  11. 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.

  12. Solid-phase extraction versus matrix solid-phase dispersion: Application to white grapes.

    Science.gov (United States)

    Dopico-García, M S; Valentão, P; Jagodziñska, A; Klepczyñska, J; Guerra, L; Andrade, P B; Seabra, R M

    2007-11-15

    The use of matrix solid-phase dispersion (MSPD) was tested to, separately, extract phenolic compounds and organic acids from white grapes. This method was compared with a more conventional analytical method previously developed that combines solid liquid extraction (SL) to simultaneously extract phenolic compounds and organic acids followed by a solid-phase extraction (SPE) to separate the two types of compounds. Although the results were qualitatively similar for both techniques, the levels of extracted compounds were in general quite lower on using MSPD, especially for organic acids. Therefore, SL-SPE method was preferred to analyse white "Vinho Verde" grapes. Twenty samples of 10 different varieties (Alvarinho, Avesso, Asal-Branco, Batoca, Douradinha, Esganoso de Castelo Paiva, Loureiro, Pedernã, Rabigato and Trajadura) from four different locations in Minho (Portugal) were analysed in order to study the effects of variety and origin on the profile of the above mentioned compounds. Principal component analysis (PCA) was applied separately to establish the main sources of variability present in the data sets for phenolic compounds, organic acids and for the global data. PCA of phenolic compounds accounted for the highest variability (77.9%) with two PCs, enabling characterization of the varieties of samples according to their higher content in flavonol derivatives or epicatechin. Additionally, a strong effect of sample origin was observed. Stepwise linear discriminant analysis (SLDA) was used for differentiation of grapes according to the origin and variety, resulting in a correct classification of 100 and 70%, respectively.

  13. Dissolution and oral bioavailability enhancement of praziquantel by solid dispersions.

    Science.gov (United States)

    Liu, Yanyan; Wang, Tianzi; Ding, Wenya; Dong, Chunliu; Wang, Xiaoting; Chen, Jianqing; Li, Yanhua

    2018-06-01

    The aim of the present investigation was to enhance the solubility, dissolution, and oral bioavailability of praziquantel (PZQ), a poorly water-soluble BCS II drug (Biopharmaceutical Classification System), using a solid dispersion (SD) technique involving hydrophilic copolymers. The SD formulations were prepared by a solvent evaporation method with PZQ and PEG 4000 (polyethylene glycol 4000), PEG 6000, or P 188 polymers at various weight ratios or a combination of PEG 4000/P 188. The optimized SD formulation, which had the highest solubility in distilled water, was further characterized by its surface morphology, crystallinity, and dissolution in 0.1 M HCl with 0.2% w/v of sodium dodecyl sulfate (SDS). X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) revealed the amorphous form of PZQ in the SDs. Moreover, at an oral dosage of 5 mg/kg PZQ, the SDs had higher C max values and areas under the curve (AUCs) compared to those of commercial PZQ tablets. Preparation of PZQ-loaded SDs using PEG 4000/P 188 is a promising strategy to improve the oral bioavailability of PZQ.

  14. 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.

  15. Thermodynamic phase behavior of API/polymer solid dispersions.

    Science.gov (United States)

    Prudic, Anke; Ji, Yuanhui; Sadowski, Gabriele

    2014-07-07

    To improve the bioavailability of poorly soluble active pharmaceutical ingredients (APIs), these materials are often integrated into a polymer matrix that acts as a carrier. The resulting mixture is called a solid dispersion. In this work, the phase behaviors of solid dispersions were investigated as a function of the API as well as of the type and molecular weight of the carrier polymer. Specifically, the solubility of artemisinin and indomethacin was measured in different poly(ethylene glycol)s (PEG 400, PEG 6000, and PEG 35000). The measured solubility data and the solubility of sulfonamides in poly(vinylpyrrolidone) (PVP) K10 and PEG 35000 were modeled using the perturbed-chain statistical associating fluid theory (PC-SAFT). The results show that PC-SAFT predictions are in a good accordance with the experimental data, and PC-SAFT can be used to predict the whole phase diagram of an API/polymer solid dispersion as a function of the kind of API and polymer and of the polymer's molecular weight. This remarkably simplifies the screening process for suitable API/polymer combinations.

  16. New Information Dispersal Techniques for Trustworthy Computing

    Science.gov (United States)

    Parakh, Abhishek

    2011-01-01

    Information dispersal algorithms (IDA) are used for distributed data storage because they simultaneously provide security, reliability and space efficiency, constituting a trustworthy computing framework for many critical applications, such as cloud computing, in the information society. In the most general sense, this is achieved by dividing data…

  17. 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.

  18. 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

  19. 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

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

    Science.gov (United States)

    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

  1. Solid lipid dispersions: potential delivery system for functional ingredients in foods.

    Science.gov (United States)

    Asumadu-Mensah, Aboagyewa; Smith, Kevin W; Ribeiro, Henelyta S

    2013-07-01

    Structured solid lipid (SL) systems have the advantages of long-term physical stability, low surfactant concentrations, and may exhibit controlled release of active ingredients. In this research work, the potential use of high-melting SLs for the production of the above structured SL carrier systems was investigated. Dispersions containing either SL or blend of solid lipid and oil (SL+O) were produced by a hot melt high-pressure homogenization method. Experiments involved the use of 3 different SLs for the disperse phase: stearic acid, candelilla wax and carnauba wax. Sunflower oil was incorporated in the disperse phase for the production of the dispersions containing lipid and oil. In order to evaluate the practical aspects of structured particles, analytical techniques were used including: static light scattering to measure particle sizes, transmission electron microscopy (TEM) for investigating particle morphology and differential scanning calorimetry (DSC) to investigate the crystallization behavior of lipids in bulk and in dispersions. Results showed different mean particle sizes depending on the type of lipid used in the disperse phase. Particle sizes for the 3 lipids were: stearic acid (SL: 195 ± 2.5 nm; SL+O: 138 ± 6.0 nm); candelilla wax (SL: 178 ± 1.7 nm; SL+O: 144 ± 0.6 nm); carnauba wax (SL: 303 ± 1.5 nm; SL+O: 295 ± 5.0 nm). TEM results gave an insight into the practical morphology, showing plate-like and needle-like structures. DSC investigations also revealed that SL dispersions melted and crystallized at lower temperatures than the bulk. This decrease can be explained by the small particle sizes of the dispersion, the high-specific surface area, and the presence of a surfactant. © 2013 Institute of Food Technologists®

  2. 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.

  3. 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.

  4. 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.

  5. [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.

  6. 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.

  7. 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.

  8. 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.

  9. Volume reduction techniques for solid radioactive wastes

    International Nuclear Information System (INIS)

    Clarke, J.H.

    1980-01-01

    This report gives an account of some of the techniques in current use in the UK for the treatment of solid radioactive wastes to reduce their volume prior to storage or disposal. Reference is also made to current research and development projects. It is based on a report presented at a recent International Atomic Energy Agency Technical Committee when this subject was the main theme. An IAEA Technical Series report covering techniques in use in all parts of the world should be published within the next two years. (author)

  10. Axial dispersion of gas and solid phases in a gas—solid packed column at trickle flow

    NARCIS (Netherlands)

    Roes, A.W.M.; van Swaaij, Willibrordus Petrus Maria

    1979-01-01

    Axial dispersion of gas and solid phases in a gas—solid packed column at trickle flow, a promising new countercurrent operation, was evaluated using residence time distribution (RTD) experiments. The column was packed with dumped Pall rings, the gas phase was air at ambient conditions and the solid

  11. Acoustic and Seismic Dispersion in Complex Fluids and Solids

    Science.gov (United States)

    Goddard, Joe

    2017-04-01

    The first part of the present paper is the continuation of a previous work [3] on the effects of higher spatial gradients and temporal relaxation on stress and heat flux in complex fluids. In particular, the general linear theory is applied to acoustic dispersion, extending a simpler model proposed by Davis and Brenner [2]. The theory is applied to a linearized version of the Chapman-Enskog fluid [1] valid to terms of Burnett order and including Maxwell-Cataneo relaxation of stress and heat flux on relaxation time scales τ. For this model, the dispersion relation k(ω) giving spatial wave number k as function of temporal frequency ω is a cubic in k2, in contrast to the quadratic in k2 given by the classical model and the recently proposed modification [2]. The cubic terms are shown to be important only for ωτ = O(1) where Maxwell-Cataneo relaxation is also important. As a second part of the present work, it is shown how the above model can also be applied to isotropic solids, where both shear and pressure waves are important. Finally, consideration is given to hyperstress in micro- polar continua, including both graded and micro-morphic varieties. [1]S. Chapman and T. Cowling. The mathematical theory of non-uniform gases. Cambridge University Press, [Cambridge, UK], 1960. [2]A. M.J. Davis and H. Brenner. Thermal and viscous effects on sound waves: revised classical theory. J. Acoust. Soc. Am., 132(5):2963-9, 2012. [3] J.D. Goddard. On material velocities and non-locality in the thermo-mechanics of continua. Int. J. Eng. Sci., 48(11):1279-88, 2010.

  12. Combination of (M)DSC and surface analysis to study the phase behaviour and drug distribution of ternary solid dispersions.

    Science.gov (United States)

    Meeus, Joke; Scurr, David J; Chen, Xinyong; Amssoms, Katie; Davies, Martyn C; Roberts, Clive J; Van den Mooter, Guy

    2015-04-01

    Miscibility of the different compounds that make up a solid dispersion based formulation play a crucial role in the drug release profile and physical stability of the solid dispersion as it defines the phase behaviour of the dispersion. The standard technique to obtain information on phase behaviour of a sample is (modulated) differential scanning calorimetry ((M)DSC). However, for ternary mixtures (M)DSC alone is not sufficient to characterize their phase behaviour and to gain insight into the distribution of the active pharmaceutical ingredient (API) in a two-phased polymeric matrix. MDSC was combined with complementary surface analysis techniques, specifically time-of-flight secondary ion mass spectrometry (ToF-SIMS) and atomic force microscopy (AFM). Three spray-dried model formulations with varying API/PLGA/PVP ratios were analyzed. MDSC, TOF-SIMS and AFM provided insights into differences in drug distribution via the observed surface coverage for 3 differently composed ternary solid dispersions. Combining MDSC and surface analysis rendered additional insights in the composition of mixed phases in complex systems, like ternary solid dispersions.

  13. [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.

  14. 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...

  15. Physical stability of API/polymer-blend amorphous solid dispersions.

    Science.gov (United States)

    Lehmkemper, Kristin; Kyeremateng, Samuel O; Bartels, Mareike; Degenhardt, Matthias; Sadowski, Gabriele

    2018-03-01

    The preparation of amorphous solid dispersions (ASDs) is a well-established strategy for formulating active pharmaceutical ingredients by embedding them in excipients, usually amorphous polymers. Different polymers can be combined for designing ASDs with desired properties like an optimized dissolution behavior. One important criterion for the development of ASD compositions is the physical stability. In this work, the physical stability of API/polymer-blend ASDs was investigated by thermodynamic modeling and stability studies. Amorphous naproxen (NAP) and acetaminophen (APAP) were embedded in blends of hydroxypropyl methylcellulose acetate succinate (HPMCAS) and either poly(vinylpyrrolidone) (PVP) or poly(vinylpyrrolidone-co-vinyl acetate) (PVPVA64). Parameters for modeling the API solubility in the blends and the glass-transition temperature curves of the water-free systems with Perturbed-Chain Statistical Associating Fluid Theory and Kwei equation, respectively, were correlated to experimental data. The phase behavior for standardized storage conditions (0%, 60% and 75% relative humidity (RH)) was predicted and compared to six months-long stability studies. According to modeling and experimental results, the physical stability was reduced with increasing HPMCAS content and increasing RH. This trend was observed for all investigated systems, with both APIs (NAP and APAP) and both polymer blends (PVP/HPMCAS and PVPVA64/HPMCAS). PC-SAFT and the Kwei equation turned out to be suitable tools for modeling and predicting the physical stability of the investigated API/polymer-blends ASDs. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. 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.

  17. Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD) and Dispersive Solid Phase Extraction (d-SPE) of Plant Samples

    Science.gov (United States)

    Sowa, Ireneusz; Wójciak-Kosior, Magdalena; Strzemski, Maciej; Sawicki, Jan; Staniak, Michał; Dresler, Sławomir; Szwerc, Wojciech; Mołdoch, Jarosław; Latalski, Michał

    2018-01-01

    Polyaniline (PANI) is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME). In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI) was used for dispersive solid phase extraction (d-SPE) and matrix solid–phase extraction (MSPD). The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD) quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples. PMID:29565297

  18. Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD and Dispersive Solid Phase Extraction (d-SPE of Plant Samples

    Directory of Open Access Journals (Sweden)

    Ireneusz Sowa

    2018-03-01

    Full Text Available Polyaniline (PANI is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME. In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI was used for dispersive solid phase extraction (d-SPE and matrix solid–phase extraction (MSPD. The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples.

  19. Investigating the Dissolution Performance of Amorphous Solid Dispersions Using Magnetic Resonance Imaging and Proton NMR

    Directory of Open Access Journals (Sweden)

    Francesco Tres

    2015-09-01

    Full Text Available We have investigated the dissolution performance of amorphous solid dispersions of poorly water-soluble bicalutamide in a Kollidon VA64 polymeric matrix as a function of the drug loading (5% vs. 30% bicalutamide. A combined suite of state-of-the-art analytical techniques were employed to obtain a clear picture of the drug release, including an integrated magnetic resonance imaging UV-Vis flow cell system and 1H-NMR. Off-line 1H-NMR was used for the first time to simultaneously measure the dissolution profiles and rates of both the drug and the polymer from a solid dispersion. MRI and 1H-NMR data showed that the 5% drug loading compact erodes linearly, and that bicalutamide and Kollidon VA64 are released at approximately the same rate from the molecular dispersion. For the 30% extrudate, data indicated a slower water ingress into the compact which corresponds to a slower dissolution rate of both bicalutamide and Kollidon VA64.

  20. 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.)

  1. 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.

  2. 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.

  3. 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

  4. Flexible continuous manufacturing platforms for solid dispersion formulations

    Science.gov (United States)

    Karry-Rivera, Krizia Marie

    In 2013 16,000 people died in the US due to overdose from prescription drugs and synthetic narcotics. As of that same year, 90% of new molecular entities in the pharmaceutical drug pipeline are classified as poor water-soluble. The work in this dissertation aims to design, develop and validate platforms that solubilize weak acids and can potentially deter drug abuse. These platforms are based on processing solid dispersions via solvent-casting and hot-melt extrusion methods to produce oral transmucosal films and melt tablets. To develop these platforms, nanocrystalline suspensions and glassy solutions were solvent-casted in the form of films after physicochemical characterizations of drug-excipient interactions and design of experiment approaches. A second order model was fitted to the emulsion diffusion process to predict average nanoparticle size and for process optimization. To further validate the manufacturing flexibility of the formulations, glassy solutions were also extruded and molded into tablets. This process included a systematic quality-by-design (QbD) approach that served to identify the factors affecting the critical quality attributes (CQAs) of the melt tablets. These products, due to their novelty, lack discriminatory performance tests that serve as predictors to their compliance and stability. Consequently, Process Analytical Technology (PAT) tools were integrated into the continuous manufacturing platform for films. Near-infrared (NIR) spectroscopy, including chemical imaging, combined with deconvolution algorithms were utilized for a holistic assessment of the effect of formulation and process variables on the product's CQAs. Biorelevant dissolution protocols were then established to improve the in-vivo in-vitro correlation of the oral transmucosal films. In conclusion, the work in this dissertation supports the delivery of poor-water soluble drugs in products that may deter abuse. Drug nanocrystals ensured high bioavailability, while glassy

  5. 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.

  6. Determination of clenbuterol in bovine liver by combining matrix solid phase dispersion and molecularly imprinted solid phase extraction followed by liquid chromatography/electrospray ion trap multiple stage mass spectrometry

    NARCIS (Netherlands)

    Crescenzi, C; Bayoudh, S; Cormack, P.A G; Klein, T; Ensing, K

    2001-01-01

    Matrix solid-phase dispersion(MSPD) is a new sample pretreatment for solid samples. This technique greatly simplifies sample pretreatment but, nonetheless, the extracts often still require an extra cleanup step that is both laborious and time-consuming. The potential;of combining MSPD with

  7. 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...

  8. 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.

  9. Humid storage conditions increase the dissolution rate of diazepam from solid dispersions prepared by melt agglomeration

    DEFF Research Database (Denmark)

    Jørgensen, Anna Cecilia; Torstenson, Anette Seo

    2008-01-01

    The purpose of this study is to investigate the effect of cooling mode and storage conditions on the dissolution rate of a solid dispersion prepared by melt agglomeration. The aim has been to relate this effect to the solid state properties of the agglomerates. The cooling mode had an effect on t...

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. Comparative study of curcumin and curcumin formulated in a solid dispersion: Evaluation of their antigenotoxic effects

    Directory of Open Access Journals (Sweden)

    Leonardo Meneghin Mendonça

    2015-01-01

    Full Text Available AbstractCurcumin (CMN is the principal active component derived from the rhizome of Curcuma longa (Curcuma longa L.. It is a liposoluble polyphenolic compound that possesses great therapeutic potential. Its clinical application is, however, limited by the low concentrations detected following oral administration. One key strategy for improving the solubility and bioavailability of poorly water-soluble drugs is solid dispersion, though it is not known whether this technique might influence the pharmacological effects of CMN. Thus, in this study, we aimed to evaluate the antioxidant and antigenotoxic effects of CMN formulated in a solid dispersion (CMN SD compared to unmodified CMN delivered to Wistar rats. Cisplatin (cDDP was used as the damage-inducing agent in these evaluations. The comet assay results showed that CMN SD was not able to reduce the formation of cDDP-DNA crosslinks, but it decreased the formation of micronuclei induced by cDDP and attenuated cDDP-induced oxidative stress. Furthermore, at a dose of 50 mg/kg b.w. both CMN SD and unmodified CMN increased the expression of Tp53 mRNA. Our results showed that CMN SD did not alter the antigenotoxic effects observed for unmodified CMN and showed effects similar to those of unmodified CMN for all of the parameters evaluated. In conclusion, CMN SD maintained the protective effects of unmodified CMN with the advantage of being chemically water soluble, with maximization of absorption in the gastrointestinal tract. Thus, the optimization of the physical and chemical properties of CMN SD may increase the potential for the therapeutic use of curcumin.

  15. 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

  16. Development and characterization of clay facial mask containing turmeric extract solid dispersion.

    Science.gov (United States)

    Pan-On, Suchiwa; Rujivipat, Soravoot; Ounaroon, Anan; Tiyaboonchai, Waree

    2018-04-01

    To develop clay facial mask containing turmeric extract solid dispersion (TESD) for enhancing curcumin water solubility and permeability and to determine suitable clay based facial mask. The TESD were prepared by solvent and melting solvent method with various TE to polyvinylpyrrolidone (PVP) K30 mass ratios. The physicochemical properties, water solubility, and permeability were examined. The effects of clay types on physical stability of TESD, water adsorption, and curcumin adsorption capacity were evaluated. The TESD prepared by solvent method with a TE to PVP K30 mass ratio of 1:2 showed physically stable, dry powders, when mixed with clay. When TESD was dissolved in water, the obtained TESD micelles showed spherical shape with mean size of ∼100 nm resulting in a substantial enhancement of curcumin water solubility, ∼5 mg/ml. Bentonite (Bent) and mica (M) showed the highest water adsorption capacity. The TESD's color was altered when mixed with Bent, titanium dioxide (TiO 2 ) and zinc oxide (ZnO) indicating curcumin instability. Talcum (Talc) showed the greatest curcumin adsorption followed by M and kaolin (K), respectively. Consequently, in vitro permeation studies of the TESD mixed with Talc showed lowest curcumin permeation, while TESD mixed with M or K showed similar permeation profile as free TESD solutions. The developed TESD-based clay facial mask showed lower curcumin permeation as compared to those formulations with Tween 80. The water solubility and permeability of curcumin in clay based facial mask could be improved using solid dispersion technique and suitable clay base composed of K, M, and Talc.

  17. 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.

  18. 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.

  19. Structures of the particles of the condensed dispersed phase in solid fuel combustion products plasma

    International Nuclear Information System (INIS)

    Samaryan, A.A.; Chernyshev, A.V.; Nefedov, A.P.; Petrov, O.F.; Fortov, V.E.; Mikhailov, Yu.M.; Mintsev, V.B.

    2000-01-01

    The results of experimental investigations of a type of dusty plasma which has been least studied--the plasma of solid fuel combustion products--were presented. Experiments to determine the parameters of the plasma of the combustion products of synthetic solid fuels with various compositions together with simultaneous diagnostics of the degree of ordering of the structures of the particles of the dispersed condensed phase were performed. The measurements showed that the charge composition of the plasma of the solid fuels combustion products depends strongly on the easily ionized alkali-metal impurities which are always present in synthetic fuel in one or another amount. An ordered arrangement of the particles of a condensed dispersed phase in structures that form in a boundary region between the high-temperature and condensation zones was observed for samples of aluminum-coated solid fuels with a low content of alkali-metal impurities

  20. Disintegration mediated controlled release supersaturating solid dispersion formulation of an insoluble drug: design, development, optimization, and in vitro evaluation.

    Science.gov (United States)

    Verma, Sanjay; Rudraraju, Varma S

    2015-02-01

    The objective of this study was to develop a solid dispersion based controlled release system for drug substances that are poorly soluble in water. A wax-based disintegration mediated controlled release system was designed based on the fact that an amorphous drug can crystallize out from hydrophilic matrices. For this study, cilostazol (CIL) was selected as the model drug, as it exhibits poor aqueous solubility. An amorphous solid dispersion was prepared to assist the drug to attain a supersaturated state. Povidone was used as carrier for solid dispersion (spray drying technique), hydrogenated vegetable oil (HVO) as wax matrix former, and sodium carboxymethyl cellulose (NaCMC) as a disintegrant. The extreme vertices mixture design (EVMD) was applied to optimize the designed and developed composition. The optimized formulation provided a dissolution pattern which was equivalent to the predicted curve, ascertaining that the optimal formulation could be accomplished with EVMD. The release profile of CIL was described by the Higuchi's model better than zero-order, first-order, and Hixson-Crowell's model, which indicated that the supersaturation state of CIL dominated to allow drug release by diffusion rather than disintegration regulated release as is generally observed by Hixson-Crowell's model. The optimized composition was evaluated for disintegration, dissolution, XRD, and stability studies. It was found that the amorphous state as well as the dissolution profile of CIL was maintained under the accelerated conditions of 40°C/75% RH for 6 months.

  1. Solid dispersions: a strategy for poorly aqueous soluble drugs and technology updates.

    Science.gov (United States)

    Alam, Mohd Aftab; Ali, Raisuddin; Al-Jenoobi, Fahad Ibrahim; Al-Mohizea, Abdullah M

    2012-11-01

    Present article reviews solid dispersion (SD) technologies and other patented inventions in the area of pharmaceutical SDs, which provide stable amorphous SDs. The review briefly compiles different techniques for preparing SDs, their applications, characterization of SDs, types of SDs and also elaborates the carriers used to prepare SDs. The advantages of recently introduced SD technologies such as RightSize(™), closed-cycle spray drying (CSD), Lidose® are summarized. Stability-related issues like phase separation, re-crystallization and methods to curb these problems are also discussed. A patented carrier-screening tool for predicting physical stability of SDs on the basis of drug-carrier interaction is explained. Applications of SD technique in controlled drug delivery systems and cosmetics are explored. Review also summarizes the carriers such as Soluplus®, Neusilin®, Solumer(TM) used to prepare stable amorphous SD. Binary and ternary SDs are found to be more stable and provide better enhancement of solubility or dissolution of poorly water-soluble drugs. The use of surfactants in the carrier system of SD is a recent trend. Surfactants and polymers provide stability against re-crystallization of SDs, surfactants also improve solubility and dissolution of drug.

  2. 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

  3. 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.

  4. CLSM as quantitative method to determine the size of drug crystals in a solid dispersion

    NARCIS (Netherlands)

    de Waard, Hans; Hessels, Martin J T; Boon, Maarten; Sjollema, Klaas A; Hinrichs, Wouter L J; Eissens, Anko C; Frijlink, Henderik W

    2011-01-01

    PURPOSE: To test whether confocal laser scanning microscopy (CLSM) can be used as an analytical tool to determine the drug crystal size in a powder mixture or a crystalline solid dispersion. METHODS: Crystals of the autofluorescent drug dipyridamole were incorporated in a matrix of crystalline

  5. Effect of drug-carrier interaction on the dissolution behavior of solid dispersion tablets

    NARCIS (Netherlands)

    Srinarong, Parinda; Kouwen, Sander; Visser, Marinella R; Hinrichs, Wouter L J; Frijlink, Henderik W

    2010-01-01

    The objective of this study was to compare the dissolution behavior of tablets prepared from solid dispersions with and without drug-carrier interactions. Diazepam and nifedipine were used as model drugs. Two types of carriers were used; polyvinylpyrrolidone (PVP K12, K30 and K60) and saccharides

  6. 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

  7. Characterization and physical stability of spray dried solid dispersions of probucol and PVP-K30

    DEFF Research Database (Denmark)

    Thybo, Pia; Pedersen, Betty L; Hovgaard, Lars

    2008-01-01

    The main purpose of this study was to obtain stable, well-characterized solid dispersions (SDs) of amorphous probucol and polyvinylpyrrolidone K-30 (PVP-K30) with improved dissolution rates. A secondary aim was to investigate the flow-through dissolution method for in-vitro dissolution measuremen...

  8. 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

  9. Both solubility and chemical stability of curcumin are enhanced by solid dispersion in cellulose derivative matrices.

    Science.gov (United States)

    Li, Bin; Konecke, Stephanie; Wegiel, Lindsay A; Taylor, Lynne S; Edgar, Kevin J

    2013-10-15

    Amorphous solid dispersions (ASD) of curcumin (Cur) in cellulose derivative matrices, hydroxypropylmethylcellulose acetate succinate (HPMCAS), carboxymethylcellulose acetate butyrate (CMCAB), and cellulose acetate adipate propionate (CAAdP) were prepared in order to investigate the structure-property relationship and identify polymer properties necessary to effectively increase Cur aqueous solution concentration. XRD results indicated that all investigated solid dispersions were amorphous, even at a 9:1 Cur:polymer ratio. Both stability against crystallization and Cur solution concentration from these ASDs were significantly higher than those from physical mixtures and crystalline Cur. Remarkably, curcumin was also stabilized against chemical degradation in solution. Chemical stabilization was polymer-dependent, with stabilization in CAAdP>CMCAB>HPMCAS>PVP, while matrices enhanced solution concentration as PVP>HPMCAS>CMCAB≈CAAdP. HPMCAS/Cur dispersions have useful combinations of pH-triggered release profile, chemical stabilization, and strong enhancement of Cur solution concentration. Copyright © 2013 Elsevier Ltd. All rights reserved.

  10. 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.

  11. 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.

  12. The effect of dispersion technique of montmorillonite on polyisocyanurate nanocomposites

    Science.gov (United States)

    Cabulis, U.; Fridrihsone, A.; Andersons, J.; Vlcek, T.

    2014-05-01

    The biomass represents an abundant, renewable, competitive and low cost resource that can play an alternative role to petrochemical resources. The central topic of the research activity reported is the use of rape seed oil (RO) as a raw material for the production of rigid polyisocyanurate foams (PIR). The content of the renewable resource-derived polymers achieved in ready foams is up to 20%. By using biopolymers as a matrix, a prospective way is to reinforce them with nanoparticles, organically modified clays, for improvement of mechanical properties while, at the same time, replacing petrochemical raw materials. Organoclay Cloisite® 15A was tested as a filler of PIR foams. Three different techniques - ultrasonification, mixing by three-roll mills, and high-pressure homogenization were used for dispergation of nanoclays in polyols. Composite polyisocyanurate foams and solid polymer samples were produced and tested for stiffness and strength. This paper discusses the studies into the use of RO as a renewable source in rigid PIR foams filled with organomodified montmorillonite clay with loadings from 1 to 5% by weight.

  13. 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.

  14. Norfloxacin mixed solvency based solid dispersions: An in-vitro and in-vivo investigation

    Directory of Open Access Journals (Sweden)

    Ravindra Kamble

    2017-05-01

    Full Text Available Norfloxacin (NF is a synthetic fluoro-quinolone molecule that is used for the treatment of urinary tract infections. However, due to its poor aqueous solubility, it has low oral bioavailability. The aim of the present study was to improve the aqueous solubility and dissolution profile of NF by formulating its mixed-solvency based solid dispersions (SDs. The NF-loaded SDs were prepared by a solvent evaporation technique using urea, sodium benzoate and a niacinamide hydrotropic mixture. The prepared SDs were evaluated regarding their solubility, mean particle size, in-vitro drug release and oral bioavailability. The optimized batch showed a high percentage yield of 99.04% , with a mean particle size of 132.91 μm. Optimized SDs Exhibit 96.48% drug release. The oral bioavailabilities of NF from the optimized SDs, drug alone and marketed formulation were evaluated in Wistar rats at a dose of 20.0 mg/kg. In comparison to the drug alone, approximately 6.90- and 5.0-fold increases in AUC and Cmax, respectively, were observed for NF from mixed-solvency based SDs. The superior dissolution rate due to its reduced particle size may have contributed to the increased oral bioavailability. This study demonstrated that mixed-solvency may be an alternative approach for poorly soluble drugs to improve their solubility and oral bioavailability.

  15. Combined application of mixture experimental design and artificial neural networks in the solid dispersion development.

    Science.gov (United States)

    Medarević, Djordje P; Kleinebudde, Peter; Djuriš, Jelena; Djurić, Zorica; Ibrić, Svetlana

    2016-01-01

    This study for the first time demonstrates combined application of mixture experimental design and artificial neural networks (ANNs) in the solid dispersions (SDs) development. Ternary carbamazepine-Soluplus®-poloxamer 188 SDs were prepared by solvent casting method to improve carbamazepine dissolution rate. The influence of the composition of prepared SDs on carbamazepine dissolution rate was evaluated using d-optimal mixture experimental design and multilayer perceptron ANNs. Physicochemical characterization proved the presence of the most stable carbamazepine polymorph III within the SD matrix. Ternary carbamazepine-Soluplus®-poloxamer 188 SDs significantly improved carbamazepine dissolution rate compared to pure drug. Models developed by ANNs and mixture experimental design well described the relationship between proportions of SD components and percentage of carbamazepine released after 10 (Q10) and 20 (Q20) min, wherein ANN model exhibit better predictability on test data set. Proportions of carbamazepine and poloxamer 188 exhibited the highest influence on carbamazepine release rate. The highest carbamazepine release rate was observed for SDs with the lowest proportions of carbamazepine and the highest proportions of poloxamer 188. ANNs and mixture experimental design can be used as powerful data modeling tools in the systematic development of SDs. Taking into account advantages and disadvantages of both techniques, their combined application should be encouraged.

  16. Preparation and evaluation of azithromycin binary solid dispersions using various polyethylene glycols for the improvement of the drug solubility and dissolution rate

    Directory of Open Access Journals (Sweden)

    Ehsan Adeli

    Full Text Available ABSTRACT Azithromycin is a water-insoluble drug, with a very low bioavailability. In order to increase the solubility and dissolution rate, and consequently increase the bioavailability of poorly-soluble drugs (such as azithromycin, various techniques can be applied. One of such techniques is "solid dispersion". This technique is frequently used to improve the dissolution rate of poorly water-soluble compounds. Owing to its low solubility and dissolution rate, azithromycin does not have a suitable bioavailability. Therefore, the main purpose of this investigation was to increase the solubility and dissolution rate of azithromycin by preparing its solid dispersion, using different Polyethylene glycols (PEG. Preparations of solid dispersions and physical mixtures of azithromycin were made using PEG 4000, 6000, 8000, 12000 and 20000 in various ratios, based on the solvent evaporation method. From the studied drug release profile, it was discovered that the dissolution rate of the physical mixture, as the well as the solid dispersions, were higher than those of the drug alone. There was no chemical incompatibility between the drug and polymer from the observed Infrared (IR spectra. Drug-polymer interactions were also investigated using Differential Scanning Calorimetry (DSC, Powder X-Ray Diffraction (PXRD and Scanning Election Microscopy (SEM. In conclusion, the dissolution rate and solubility of azithromycin were found to improve significantly, using hydrophilic carriers, especially PEG 6000.

  17. 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.

  18. In-Vitro Characterization and Oral Bioavailability of Organic Solvent-free Solid Dispersions Containing Telmisartan

    DEFF Research Database (Denmark)

    Cao, Yue; Shi, Li-Li; Cao, Qing-Ri

    2016-01-01

    Poorly water-soluble drugs often suffer from limited or irreproducible clinical response due to their low solubility and dissolution rate. In this study, organic solvent-free solid dispersions (OSF-SDs) containing telmisartan (TEL) were prepared using polyvinylpyrrolidone K30 (PVP K30....... The results from DSC, XRD showed that TEL was molecularly dispersed in the OSF-SDs as an amorphous form. The FT-IR results suggested that intermolecular hydrogen bonding had formed between TEL and its carriers. The OSF-SDs exhibited significantly higher AUC0-24 h and Cmax, but similar Tmax as compared...

  19. 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)

  20. Patterning titania with the conventional and modified micromolding in capillaries technique from sol–gel and dispersion solutions

    Directory of Open Access Journals (Sweden)

    Sajid Ullah Khan and Johan E ten Elshof

    2012-01-01

    Full Text Available We report TiO2 patterns obtained by a soft-lithographic technique called 'micromolding in capillaries' using sol–gel and dispersion solutions. A comparison between patterning with a sol–gel and dispersion solutions has been performed. The patterns obtained from sol–gel solutions showed good adhesion to the substrate and uniform shapes, but large shrinkage, whereas those obtained from dispersion solution had high solid content, but exhibited poor adhesion and non-uniform shapes. A fabrication method of a layer-by-layer structured pattern is also demonstrated. This type of pattern may find application in sensors, waveguides and other photonics elements. The occurrence of an undesirable residue layer, which hinders the fabrication of isolated patterns, is highlighted and a method of prevention is suggested.

  1. 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.

  2. 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.

  3. Solid dispersions, part II: new strategies in manufacturing methods for dissolution rate enhancement of poorly water-soluble drugs.

    Science.gov (United States)

    Bikiaris, Dimitrios N

    2011-12-01

    The absorption of poorly water-soluble drugs, when presented in the crystalline state to the gastrointestinal tract, is typically dissolution rate-limited, and according to BCS these drugs belong mainly to class II. Both dissolution kinetics and solubility are particle size dependent. Nowadays, various techniques are available to the pharmaceutical industry for dissolution rate enhancement of such drugs. Among such techniques, nanosuspensions and drug formulation in solid dispersions are those with the highest interest. This review discusses strategies undertaken over the last 10 years, which have been applied for the dissolution enhancement of poorly water-soluble drugs; such processes include melt mixing, electrospinning, microwave irradiation and the use of inorganic nanoparticles. Many problems in this field still need to be solved, mainly the use of toxic solvents, and for this reason the use of innovative new procedures and materials will increase over the coming years. Melt mixing remains extremely promising for the preparation of SDs and will probably become the most used method in the future for the preparation of solid drug dispersions.

  4. Fast-track to a solid dispersion formulation using multi-way analysis of complex interactions

    DEFF Research Database (Denmark)

    Wu, Jian-Xiong; Den Berg, Frans Van; Søgaard, Søren Vinter

    2013-01-01

    Several factors with complex interactions influence the physical stability of solid dispersions, thus highlighting the need for efficient experimental design together with robust and simple multivariate model. Design of Experiments together with ANalysis Of VAriance (ANOVA) model is one of the ce.......g., an entire spectral data set), model uniqueness, and curve resolution abilities. © 2012 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 102:904-914, 2013....

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

    Science.gov (United States)

    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.

  6. Hypercrosslinked particles for the extraction of sweeteners using dispersive solid-phase extraction from environmental samples.

    Science.gov (United States)

    Lakade, Sameer S; Zhou, Qing; Li, Aimin; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa M

    2018-04-01

    This work presents a new extraction material, namely, Q-100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid-phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q-100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior toward sweeteners. Different dispersive solid-phase extraction parameters such as amount of magnetic particles or extraction time were optimized. Under optimum conditions, Q-100 showed suitable apparent recovery, ranging in the case of river water sample from 21 to 88% for all the sweeteners, except for alitame (12%). The validated method based on dispersive solid-phase extraction using Q-100 followed by liquid chromatography with tandem mass spectrometry provided good linearity and limits of quantification between 0.01 and 0.1 μg/L. The method was applied to analyze samples from river water and effluent wastewater, and four sweeteners (acesulfame, saccharin, cyclamate, and sucralose) were found in both types of sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  9. Influence of solvent evaporation rate and formulation factors on solid dispersion physical stability.

    Science.gov (United States)

    Wu, Jian X; Yang, Mingshi; Berg, Frans van den; Pajander, Jari; Rades, Thomas; Rantanen, Jukka

    2011-12-18

    New chemical entities (NCEs) often show poor water solubility necessitating solid dispersion formulation. The aim of the current study is to employ design of experiments in investigating the influence of one critical process factor (solvent evaporation rate) and two formulation factors (PVP:piroxicam ratio (PVP:PRX) and PVP molecular weight (P(MW))) on the physical stability of PRX solid dispersion prepared by the solvent evaporation method. The results showed the rank order of an increase in factors contributing to a decrease in the extent of PRX nucleation being evaporation rate>PVP:PRX>P(MW). The same rank order was found for the decrease in the extent of PRX crystal growth in PVP matrices from day 0 up to day 12. However, after 12days the rank became PVP:PRX>evaporation rate>P(MW). The effects of an increase in evaporation rate and PVP:PRX ratio in stabilizing PRX were of the same order of magnitude, while the effect from P(MW) was much smaller. The findings were confirmed by XRPD. FT-IR showed that PRX recrystallization in the PVP matrix followed Ostwald's step rule, and an increase in the three factors all led to increased hydrogen bonding interaction between PRX and PVP. The present study showed the applicability of the Quality by Design approach in solid dispersion research, and highlights the need for multifactorial analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

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

    Directory of Open Access Journals (Sweden)

    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

  11. Influence of the microwave technology on solid dispersions of mefenamic acid and flufenamic acid.

    Directory of Open Access Journals (Sweden)

    Sultan Alshehri

    Full Text Available The present studies were undertaken to develop solvent-free solid dispersions (SDs for poorly soluble anti-inflammatory drugs mefenamic acid (MA and flufenamic acid (FFA in order to enhance their in vitro dissolution rate and in vivo anti-inflammatory effects. The SDs of MA and FFA were prepared using microwaves irradiation (MW technique. Different carriers such as Pluronic F127® (PL, Eudragit EPO® (EPO, polyethylene glycol 4000 (PEG 4000 and Gelucire 50/13 (GLU were used for the preparation of SDs. Prepared MW irradiated SDs were characterized physicochemically using differential scanning calorimetry (DSC, thermogravimetric analysis (TGA, Fourier transform infra-red (FT-IR spectroscopy, powder X-ray diffraction (PXRD and scanning electron microscopy (SEM. The physicochemical characteristics and drug release profile of SDs were compared with pure drugs. The results of DSC, TGA, FT-IR, PXRD and SEM showed that SDs were successfully prepared. In vitro dissolution rate of MA and FFA was remarkably enhanced by SDs in comparison with pure MA and FFA. The SDs of MA and FFA prepared using PEG 400 showed higher drug release profile in comparison with those prepared using PL, EPO or GLU. The dissolution efficiency for MA-PEG SD and FFA-PEG SD was obtained as 61.40 and 59.18%, respectively. Optimized SDs were also evaluated for in vivo anti-inflammatory effects in male Wistar rats. The results showed significant % inhibition by MA-PEG (87.74% after 4 h and FFA-PEG SDs (81.76% after 4 h in comparison with pure MA (68.09% after 4 h and pure FFA (55.27% after 4 h (P<0.05. These results suggested that MW irradiated SDs of MA and FFA could be successfully used for the enhancement of in vitro dissolution rate and in vivo therapeutic efficacy of both drugs.

  12. 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.

  13. Studies of electron transitions using solid He pressure techniques

    International Nuclear Information System (INIS)

    Schirber, J.E.

    1977-01-01

    Changes in the topology of the Fermi surfaces of metals occur with variation of temperature or stoichiometry in a number of metallic systems of current interest. Pressure generated by a variety of techniques has proven to be the most useful experimental variable in the study of these transitions, but in most cases only solid He techniques yield sufficiently hydrostatic conditions to permit direct measurements of the Fermi surface as a function of pressure

  14. Stabilizing ability of surfactant on physicochemical properties of drug nanoparticles generated from solid dispersions.

    Science.gov (United States)

    Thongnopkoon, Thanu; Puttipipatkhachorn, Satit

    2017-07-01

    This study was aimed to examine the nanoparticle formation from redispersion of binary and ternary solid dispersions. Binary systems are composed of various ratios of glibenclamide (GBM) and polyvinylpyrrolidone K30 (PVP-K30), whereas a constant amount at 2.5%w/w of a surfactant, sodium lauryl sulfate (SLS) or Gelucire44/14 (GLC), was added to create ternary systems. GBM nanoparticles were collected after the systems were dispersed in water for 15 min. The obtained nanoparticles were characterized for size distribution, crystallinity, thermal behavior, molecular structure, and dissolution properties. The results indicated that GBM nanoparticles could be formed when the drug content of the systems was lower than 30%w/w in binary systems and ternary systems containing SLS. The particle size ranged from 200 to 500 nm in diameter with narrow size distribution. The particle size was increased with increasing drug content in the systems. The obtained nanoparticles were spherical and showed the amorphous state. Furthermore, because of being amorphous form and reduced particle size, the dissolution of the generated nanoparticles was markedly improved compared with the GBM powder. In contrast, all the ternary solid dispersions prepared with GLC anomalously provided the crystalline particles with the size ranging over 5 µm and irregular shape. Interestingly, this was irrelevant to the drug content in the systems. These results indicated the ability of GLC to destabilize the polymer network surrounding the particles during particle precipitation. Therefore, this study suggested that drug content, quantity, and type of surfactant incorporated in solid dispersions drastically affected the physicochemical properties of the precipitated particles.

  15. 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.

  16. Solid phase separation technique for use in radioimmunoassays

    International Nuclear Information System (INIS)

    Tu, J.I.

    1979-01-01

    A radioimmunoassay procedure, and article of manufacture for carrying out that procedure, are disclosed herein. The solid phase separation technique utilized in the radioimmunoassay of this invention utilizes a test tube, the internal surface of which has been coated with two antibody layers

  17. Evaluation of single-walled carbon nanohorns as sorbent in dispersive micro solid-phase extraction

    Energy Technology Data Exchange (ETDEWEB)

    Jimenez-Soto, Juan Manuel; Cardenas, Soledad [Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus de Rabanales, University of Cordoba, 14071 Cordoba (Spain); Valcarcel, Miguel, E-mail: qa1meobj@uco.es [Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus de Rabanales, University of Cordoba, 14071 Cordoba (Spain)

    2012-02-10

    Highlights: Black-Right-Pointing-Pointer The potential of single walled carbon nanohorns in dispersive solid phase microextraction has been evaluated. Black-Right-Pointing-Pointer The method was characterized for the extraction of PAHs from waters. Black-Right-Pointing-Pointer Single walled carbon nanohorns were better extractant than carbon nanotubes and carbon nanocones. Black-Right-Pointing-Pointer The limits of detection were adequate for the target analytes in environmental waters. - Abstract: A new dispersive micro solid-phase extraction method which uses single-walled carbon nanohorns (SWNHs) as sorbent is proposed. The procedure combines the excellent sorbent properties of the nanoparticles with the efficiency of the dispersion of the material in the sample matrix. Under these conditions, the interaction with the analytes is maximized. The determination of polycyclic aromatic hydrocarbons was selected as model analytical problem. Two dispersion strategies were evaluated, being the functionalization via microwave irradiation better than the use of a surfactant. The extraction was accomplished by adding 1 mL of oxidized SWHNs (o-SWNHs) dispersion to 10 mL of water sample. After extraction, the mixture was passed through a disposable Nylon filter were the nanoparticles enriched with the PAHs were retained. The elution was carried out with 100 {mu}L of hexane. The limits of detection achieved were between 30 and 60 ng L{sup -1} with a precision (as repeatability) better than 12.5%. The recoveries obtained for the analytes in three different water samples were acceptable in all instances. The performance of o-SWNHs was favourably compared with that provided by carboxylated single-walled carbon nanotubes and thermally treated carbon nanocones.

  18. A correction technique for the dispersive effects of mass lumping for transport problems

    KAUST Repository

    Guermond, Jean-Luc; Pasquetti, Richard

    2013-01-01

    This paper addresses the well-known dispersion effect that mass lumping induces when solving transport-like equations. A simple anti-dispersion technique based on the lumped mass matrix is proposed. The method does not require any non-trivial matrix

  19. Hot Melt Extruded Amorphous Solid Dispersion of Posaconazole with Improved Bioavailability: Investigating Drug-Polymer Miscibility with Advanced Characterisation

    Directory of Open Access Journals (Sweden)

    Ritesh Fule

    2014-01-01

    Full Text Available Invasive antifungal infections are reasons for morbidity and mortality in immunogenic patients worldwide. Posaconazole is a most promising antifungal agent against all types of invasive infections with high % of cure rate. The marketed suspension formulation has low bioavailability and is needed to be taken with food. In this paper, PCZ hot melt extruded amorphous solid dispersion (SD with immediate release and improved bioavailability was prepared using Soluplus (Sol as primary carrier for solubilization. Surfactants such as PEG 400, Lutrol F27, Lutrol F68, and TPGS are also used in combination with Soluplus to improve the physicochemical performance of the formulation when it comes in contact with GI (gastrointestinal fluid. Drug-polymer miscibility of SD was investigated using advanced techniques. In the in vivo study, the AUC(0–72 and Cmax of PCZ/Soluplus were 11.5 and 11.74 time higher than those of pure PCZ. The formulation of the extrudate SD had an AUC(0–72 and Cmax higher than those with the commercial capsule (Noxafil. Molecular dynamic (MD simulation studies were carried out using in silico molecular modelling to understand the drug-polymer intermolecular behaviour. The results of this research ensure enhanced dissolution and bioavailability of the solid dispersion of PCZ prepared by HME compared with the PCZ suspension.

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

    Directory of Open Access Journals (Sweden)

    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

  1. Solubility and dissolution enhancement of flurbiprofen by solid dispersion using hydrophilic carriers

    Directory of Open Access Journals (Sweden)

    Bhaskar Daravath

    2018-05-01

    Full Text Available ABSTRACT The intent of the current work is to study the effect of polyethylene glycol 8000 and polyethylene glycol 10000 as hydrophilic carriers on dissolution behaviour of flurbiprofen. In the present study, solvent evaporation method was used to prepare flurbiprofen solid dispersions and evaluated for physico-chemical properties, drug-carrier compatibility studies and dissolution behaviour of drug. Solubility studies showed more solubility in higher pH values and formulations SD4 and SD8 were selected to prepare the fast dissolving tablets. FTIR and DSC study showed no interaction and drug was dispersed molecularly in hydrophilic carrier. XRD studies revealed that there was change in the crystallinity of the drug. The results of In vitro studies showed SD8 formulation confer significant improvement (p<0.05 in drug release, Q20 was 99.08±1.35% compared to conventional and marketed tablets (47.31±0.74% and 56.86±1.91%. The mean dissolution time (MDT was reduced to 8.79 min compared to conventional and marketed tablets (25.76 and 22.22 min. indicating faster drug release. The DE (% dissolution efficiency was increased by 2.5 folds (61.63% compared to conventional tablets (23.71%. From the results, it is evident that polyethylene glycol solid dispersions in less carrier ratio may enhance the solubility and there by improve the dissolution rate of flurbiprofen.

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

    International Nuclear Information System (INIS)

    Li, Jianjun; Liu, Yun; Liu, Qianping; Hui, Junfeng; Liu, Yangzi

    2017-01-01

    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 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 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.

  3. 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.

  4. Crosslinked hydrogels?a promising class of insoluble solid molecular dispersion carriers for enhancing the delivery of poorly soluble drugs

    OpenAIRE

    Sun, Dajun D.; Lee, Ping I.

    2014-01-01

    Water-insoluble materials containing amorphous solid dispersions (ASD) are an emerging category of drug carriers which can effectively improve dissolution kinetics and kinetic solubility of poorly soluble drugs. ASDs based on water-insoluble crosslinked hydrogels have unique features in contrast to those based on conventional water-soluble and water-insoluble carriers. For example, solid molecular dispersions of poorly soluble drugs in poly(2-hydroxyethyl methacrylate) (PHEMA) can maintain a ...

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. Amorphous Solid Dispersion of Epigallocatechin Gallate for Enhanced Physical Stability and Controlled Release.

    Science.gov (United States)

    Cao, Yizheng; Teng, Jing; Selbo, Jon

    2017-11-09

    Epigallocatechin gallate (EGCG) has been recognized as the most prominent green tea extract due to its healthy influences. The high instability and low bioavailability, however, strongly limit its utilization in food and drug industries. This work, for the first time, develops amorphous solid dispersion of EGCG to enhance its bioavailability and physical stability. Four commonly used polymeric excipients are found to be compatible with EGCG in water-dioxane mixtures via a stepwise mixing method aided by vigorous mechanical interference. The dispersions are successfully generated by lyophilization. The physical stability of the dispersions is significantly improved compared to pure amorphous EGCG in stress condition (elevated temperature and relative humidity) and simulated gastrointestinal tract environment. From the drug release tests, one of the dispersions, EGCG-Soluplus ® 50:50 ( w / w ) shows a dissolution profile that only 50% EGCG is released in the first 20 min, and the remains are slowly released in 24 h. This sustained release profile may open up new possibilities to increase EGCG bioavailability via extending its elimination time in plasma.

  10. Amorphous Solid Dispersion of Epigallocatechin Gallate for Enhanced Physical Stability and Controlled Release

    Directory of Open Access Journals (Sweden)

    Yizheng Cao

    2017-11-01

    Full Text Available Epigallocatechin gallate (EGCG has been recognized as the most prominent green tea extract due to its healthy influences. The high instability and low bioavailability, however, strongly limit its utilization in food and drug industries. This work, for the first time, develops amorphous solid dispersion of EGCG to enhance its bioavailability and physical stability. Four commonly used polymeric excipients are found to be compatible with EGCG in water-dioxane mixtures via a stepwise mixing method aided by vigorous mechanical interference. The dispersions are successfully generated by lyophilization. The physical stability of the dispersions is significantly improved compared to pure amorphous EGCG in stress condition (elevated temperature and relative humidity and simulated gastrointestinal tract environment. From the drug release tests, one of the dispersions, EGCG-Soluplus® 50:50 (w/w shows a dissolution profile that only 50% EGCG is released in the first 20 min, and the remains are slowly released in 24 h. This sustained release profile may open up new possibilities to increase EGCG bioavailability via extending its elimination time in plasma.

  11. A novel technique to determine concentration-dependent solvent dispersion in Vapex

    Energy Technology Data Exchange (ETDEWEB)

    Abukhalifeh, H.; Lohi, A.; Upreti, S. R. [Department of Chemical Engineering, Ryerson University, 350 Victoria Street, Toronto, Ontario, M5B 2K3 (Canada)

    2009-07-01

    Vapex (vapor extraction of heavy oil and bitumen) is a promising recovery technology because it consumes low energy, and is very environmentally-friendly. The dispersion of solvents into heavy oil and bitumen is a crucial transport property governing Vapex. The accurate determination of solvent dispersion in Vapex is essential to effectively predict the amount and time scale of oil recovery as well to optimize the field operations. In this work, a novel technique is developed to experimentally determine the concentration-dependent dispersion coefficient of a solvent in Vapex process. The principles of variational calculus are utilized in conjunction with a mass transfer model of the experimental Vapex process. A computational algorithm is developed to optimally compute solvent dispersion as a function of its concentration in heavy oil. The developed technique is applied to Vapex utilizing propane as a solvent. The results show that dispersion of propane is a unimodal function of its concentration in bitumen. (author)

  12. A Novel Technique to Determine Concentration-Dependent Solvent Dispersion in Vapex

    Directory of Open Access Journals (Sweden)

    Hadil Abukhalifeh

    2009-10-01

    Full Text Available Vapex (vapor extraction of heavy oil and bitumen is a promising recovery technology because it consumes low energy, and is very environmentally-friendly. The dispersion of solvents into heavy oil and bitumen is a crucial transport property governing Vapex. The accurate determination of solvent dispersion in Vapex is essential to effectively predict the amount and time scale of oil recovery as well to optimize the field operations. In this work, a novel technique is developed to experimentally determine the concentration-dependent dispersion coefficient of a solvent in Vapex process. The principles of variational calculus are utilized in conjunction with a mass transfer model of the experimental Vapex process. A computational algorithm is developed to optimally compute solvent dispersion as a function of its concentration in heavy oil. The developed technique is applied to Vapex utilizing propane as a solvent. The results show that dispersion of propane is a unimodal function of its concentration in bitumen.

  13. Preparation, characterization, and dissolution studies of naproxen solid dispersions using polyethylene glycol 6000 and labrafil M2130

    Directory of Open Access Journals (Sweden)

    Jafar Akbari

    2015-06-01

    Full Text Available Naproxen is a poor water soluble, non-steroidal analgesic and anti-inflammatory drug. The enhancement of oral bioavailability of poor water soluble drugs remains one of the most challenging aspects of drug development. Although salt formation, solubilization and particle size reduction have commonly been used to increase dissolution rate and thereby oral absorption and bioavailability of low water soluble drugs, there are practical limitation of these techniques. However, the most attractive option for increasing the release rate is improvement of solubility through formulation approaches. In this study, solid dispersions (SD of naproxen were prepared by hot melt method using various ratios of drug to polymers (PEG6000 separately and characterized for physical appearance, FTIR, DSC, X-Ray crystallography, and in-vitro dissolution studies. The influence of several amounts of Labrafil M2130 was also studied. FTIR study revealed that drug was stable in SDs, and great state of amorphous formed particles was proofed by DSC analysis. The in vitro dissolution studies were carried using USP type II (paddle dissolution apparatus at medium (pH 1.5. Solubility of naproxen from SDs was increased in dissolution media. The prepared dispersion showed increase in the dissolution rate of naproxen comparing to that of physical mixtures of drug and polymers and pure drug. Percent of drug released in 60 minutes was 23.92% for pure naproxen witch is increased in SDs and reached to100% for best formulations of PEG6000 and labrafil based SDs respectively, considering ratio of drug to polymers.It is concluded that dissolution of the naproxen could be improved by the solid dispersion. Although physical mixtures have increased the rate of dissolution, dissolution shows faster release from SDs which would therefore be due to formation of amorphous particles through the hot melt process which was also revealed by DSC analysis and XRD.

  14. A correction technique for the dispersive effects of mass lumping for transport problems

    KAUST Repository

    Guermond, Jean-Luc

    2013-01-01

    This paper addresses the well-known dispersion effect that mass lumping induces when solving transport-like equations. A simple anti-dispersion technique based on the lumped mass matrix is proposed. The method does not require any non-trivial matrix inversion and has the same anti-dispersive effects as the consistent mass matrix. A novel quasi-lumping technique for P2 finite elements is introduced. Higher-order extensions of the method are also discussed. © 2012 Elsevier B.V.

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

    Science.gov (United States)

    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.

  16. 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.

  17. Aplicação da técnica de dispersão da matriz em fase sólida (DMFS na análise de pesticidas em quiabo por CG-EM Application of the matrix solid phase dispersion (MSPD technique in the analysis of pesticides in okra by GC-MS

    Directory of Open Access Journals (Sweden)

    Haroldo Silveira Dórea

    2004-12-01

    Full Text Available A matrix solid phase dispersion and gas chromatography-mass selective detection method for the simultaneous determination of monocrotophos, methyl parathion, cypermethrin and deltamethrin in okra is described. Analyses of 2 g of fortified okra (0.05-0.75 mg kg-1 showed an average recovery of 96.2% (71.4-128.4% and average relative standard deviation of 11.7% (1.4-37.1%. The cypermethrin recovery at the lower level was above 130%. The limit of detection ranged from 0.02 to 0.15 mg kg-1. The procedure was applied to the okra samples and has found 0.56 mg kg-1 of cypermethrin-cis, 0.75 mg kg-1 of cypermethrin-trans and 2.71 mg kg-1 of deltamethrin.

  18. 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.

  19. Measurements of Turbulence Attenuation by a Dilute Dispersion of Solid Particles in Homogeneous Isotropic Turbulence

    Science.gov (United States)

    Eaton, John; Hwang, Wontae; Cabral, Patrick

    2002-11-01

    This research addresses turbulent gas flows laden with fine solid particles at sufficiently large mass loading that strong two-way coupling occurs. By two-way coupling we mean that the particle motion is governed largely by the flow, while the particles affect the gas-phase mean flow and the turbulence properties. Our main interest is in understanding how the particles affect the turbulence. Computational techniques have been developed which can accurately predict flows carrying particles that are much smaller than the smallest scales of turbulence. Also, advanced computational techniques and burgeoning computer resources make it feasible to fully resolve very large particles moving through turbulent flows. However, flows with particle diameters of the same order as the Kolmogorov scale of the turbulence are notoriously difficult to predict. Some simple flows show strong turbulence attenuation with reductions in the turbulent kinetic energy by up to a factor of five. On the other hand, some seemingly similar flows show almost no modification. No model has been proposed that allows prediction of when the strong attenuation will occur. Unfortunately, many technological and natural two-phase flows fall into this regime, so there is a strong need for new physical understanding and modeling capability. Our objective is to study the simplest possible turbulent particle-laden flow, namely homogeneous, isotropic turbulence with a uniform dispersion of monodisperse particles. We chose such a simple flow for two reasons. First, the simplicity allows us to probe the interaction in more detail and offers analytical simplicity in interpreting the results. Secondly, this flow can be addressed by numerical simulation, and many research groups are already working on calculating the flow. Our detailed data can help guide some of these efforts. By using microgravity, we can further simplify the flow to the case of no mean velocity for either the turbulence or the particles. In fact

  20. Radioactive ion beams and techniques for solid state research

    International Nuclear Information System (INIS)

    Correia, J.G.

    1998-01-01

    In this paper we review the most recent and new applications of solid state characterization techniques using radioactive ion beams. For such type ofresearch, high yields of chemically clean ion beams of radioactive isotopesare needed which are provided by the on-line coupling of high resolution isotope separators to particle accelerators, such as the isotope separator on-line (ISOLDE) facility at CERN. These new experiments are performed by an increasing number of solid state groups. They combine nuclear spectroscopic techniques such as Moessbauer, perturbed angular correlations (PAC) and emission channeling with the traditional non-radioactive techniques liked deep level transient spectroscopy (DLTS) and Hall effect measurements. Recently isotopes of elements, not available before, were successfully used in new PAC experiments, and the first photoluminescence (PL) measurements, where the element transmutation plays the essential role on the PL peak identification, have been performed. The scope of applications of radioactive ion beams for research in solid state physics will be enlarged in the near future, with the installation at ISOLDE of a post-accelerator device providing radioactive beams with energies ranging from a few keV up to a few MeV. (orig.)

  1. Introduction to electronic relaxation in solids: mechanisms and measuring techniques

    International Nuclear Information System (INIS)

    Bonville, P.

    1983-01-01

    The fluctuations of electronic magnetic moments in solids may be investigated by several techniques, either electronic or nuclear. This paper is an introduction of the most frequently encountered paramagnetic relaxation mechanisms (phonons, conduction electrons, exchange or dipolar interactions) in condensed matter, and to the different techniques used for measuring relaxation frequencies: electronic paramagnetic resonance, nuclear magnetic resonance, Moessbauer spectroscopy, inelastic neutron scattering, measurement of longitudinal ac susceptibility and γ-γ perturbed angular correlations. We mainly focus our attention on individual ionic fluctuation spectra, the majority of the experimental work refered to concerning rare earth systems [fr

  2. Solid-state characterization and dissolution properties of meloxicam-moringa coagulant-PVP ternary solid dispersions.

    Science.gov (United States)

    Noolkar, Suhail B; Jadhav, Namdeo R; Bhende, Santosh A; Killedar, Suresh G

    2013-06-01

    The effect of ternary solid dispersions of poor water-soluble NSAID meloxicam with moringa coagulant (obtained by salt extraction of moringa seeds) and polyvinylpyrrolidone on the in vitro dissolution properties has been investigated. Binary (meloxicam-moringa and meloxicam-polyvinylpyrrolidone (PVP)) and ternary (meloxicam-moringa-PVP) systems were prepared by physical kneading and ball milling and characterized by Fourier transform infrared spectroscopy, differential scanning calorimetry, and X-ray diffractometry. The in vitro dissolution behavior of meloxicam from the different products was evaluated by means of United States Pharmacopeia type II dissolution apparatus. The results of solid-state studies indicated the presence of strong interactions between meloxicam, moringa, and PVP which were of totally amorphous nature. All ternary combinations were significantly more effective than the corresponding binary systems in improving the dissolution rate of meloxicam. The best performance in this respect was given by the ternary combination employing meloxicam-moringa-PVP ratio of [1:(3:1)] prepared by ball milling, with about six times increase in percent dissolution rate, whereas meloxicam-moringa (1:3) and meloxicam-PVP (1:4) prepared by ball milling improved dissolution of meloxicam by almost 3- and 2.5-folds, respectively. The achieved excellent dissolution enhancement of meloxicam in the ternary systems was attributed to the combined effects of impartation of hydrophilic characteristic by PVP, as well as to the synergistic interaction between moringa and PVP.

  3. 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.

  4. 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

  5. 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

    Ketoconazole is one of the most widely prescribed oral antifungal drugs for the systemic treatment of various fungal infections. However, due its hydrophobic nature and poor solubility profiles in the gastro-intestinal fluids, variations in its bioavailability have been documented. Therefore, to enhance its dissolution in the biological fluids, this study was initiated to develop and evaluate Nanoparticles and Solid Dispersion forms of the drug. Nanoparticles of ketoconazole were developed by Wet Bead Milling technique using PVP-10k as the stabilizing material at a weight ratio of (2:1). Solid dispersion powder was prepared by Hot Melt method using PEG-8000 at a weight ratio of (1:2). A commercial product containing 200mg of ketoconazole tablet and pure drug powder were used as the control for comparison purposes. The dissolution studies were carried out in SGF, SIF, USP; and SIF with 0.2% sodium lauryl sulfate using the USP-II method for a 2 hours period. Physical characterizations were carried out using SEM, DSC, XRD and FTIR studies. Wet Bead Milling method yielded nanoparticles in the particles size range of (100-300nm.). First all samples were evaluated for their in-vitro dissolution in SGF at pH=1.2. After 15 minutes, the amounts of drug dissolved were observed to be 27% from both the pure powder and commercial tablet (control), 29% from solid dispersion and 100% from the Nanoparticles dosage form. This supports the fact that Nanoparticles had a strong influence on the dissolution rate of the drug and exhibited much faster dissolution of ketoconazole. When the same formulations were studied in the SIF, USP medium, the control formulation gave 3%, solid dispersion 8% and Nanoparticles 8% drug dissolution after 2 hours period. This could be because the weakly basic ketoconazole drug remained un-dissociated in the alkaline medium. Since this medium was unable to clearly distinguish the dissolution profiles from different formulation of the drug, the SIF solution

  6. 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.

  7. Evaluation and modeling of the eutectic composition of various drug-polyethylene glycol solid dispersions.

    Science.gov (United States)

    Baird, Jared A; Taylor, Lynne S

    2011-06-01

    The purpose of this study was to gain a better understanding of which factors contribute to the eutectic composition of drug-polyethylene glycol (PEG) blends and to compare experimental values with predictions from the semi-empirical model developed by Lacoulonche et al. Eutectic compositions of various drug-PEG 3350 solid dispersions were predicted, assuming athermal mixing, and compared to experimentally determined eutectic points. The presence or absence of specific interactions between the drug and PEG 3350 were investigated using Fourier transform infrared (FT-IR) spectroscopy. The eutectic composition for haloperidol-PEG and loratadine-PEG solid dispersions was accurately predicted using the model, while predictions for aceclofenac-PEG and chlorpropamide-PEG were very different from those experimentally observed. Deviations in the model prediction from ideal behavior for the systems evaluated were confirmed to be due to the presence of specific interactions between the drug and polymer, as demonstrated by IR spectroscopy. Detailed analysis showed that the eutectic composition prediction from the model is interdependent on the crystal lattice energy of the drug compound (evaluated from the melting temperature and the heat of fusion) as well as the nature of the drug-polymer interactions. In conclusion, for compounds with melting points less than 200°C, the model is ideally suited for predicting the eutectic composition of systems where there is an absence of drug-polymer interactions.

  8. Improved oral absorption of tacrolimus by a solid dispersion with hypromellose and sodium lauryl sulfate.

    Science.gov (United States)

    Jung, Hyuck Jun; Ahn, Hye In; Park, Ji Yeon; Ho, Myoung Jin; Lee, Dae Ro; Cho, Ha Ra; Park, Jun Seo; Choi, Yong Seok; Kang, Myung Joo

    2016-02-01

    A novel surfactant-incorporated hydroxypropyl methylcellulose (HPMC) solid dispersion (SD) system was constructed in order to facilitate the release rate and oral absorption of tacrolimus (FK506), a poorly water-soluble immunosuppressant. Several emulsifiers including sodium lauryl sulfate (SLS), as drug release promotors, were employed with HPMC to fabricate SD using the solvent wetting method. The solid state characteristics using differential scanning calorimetry and X-ray powder diffraction, revealed that FK506 was molecularly distributed within all dispersions in amorphous form. The dissolution rates of FK506 in SLS-incorporated SDs were much higher than those in SDs prepared with HPMC alone, and even with stearoyl polyoxyl-32 glycerides or tocopheryl polyethylene glycol 1000 succinate. In particular, the greatest dissolution enhancement was obtained from the SD consisting of the drug, HPMC, and SLS in a weight ratio of 1:1:3, providing a 50-fold higher drug concentration within 15 min, compared with HPMC SD. In vivo absorption study in rats demonstrates that the optimized formula remarkably increased the oral absorption of FK506, providing about 4.0-fold greater bioavailability (p<0.05) compared with the marketed product (Prograf®, Astellas Pharma). These data suggest that a novel SLS/HPMC SD may be an advantageous dosage form of FK506, boosting the dissolution and absorption in gastrointestinal tract. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. 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.

  10. 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.

  11. Revealing facts behind spray dried solid dispersion technology used for solubility enhancement

    Science.gov (United States)

    Patel, Bhavesh B.; Patel, Jayvadan K.; Chakraborty, Subhashis; Shukla, Dali

    2013-01-01

    Poor solubility and bioavailability of an existing or newly synthesized drug always pose challenge in the development of efficient pharmaceutical formulation. Numerous technologies can be used to improve the solubility and among them amorphous solid dispersion based spray drying technology can be successfully useful for development of product from lab scale to commercial scale with a wide range of powder characteristics. Current review deals with the importance of spray drying technology in drug delivery, basically for solubility and bioavailability enhancement. Role of additives, selection of polymer, effect of process and formulation parameters, scale up optimization, and IVIVC have been covered to gain the interest of readers about the technology. Design of experiment (DoE) to optimize the spray drying process has been covered in the review. A lot more research work is required to evaluate spray drying as a technology for screening the right polymer for solid dispersion, especially to overcome the issue related to drug re-crystallization and to achieve a stable product both in vitro and in vivo. Based on the recent FDA recommendation, the need of the hour is also to adopt Quality by Design approach in the manufacturing process to carefully optimize the spray drying technology for its smooth transfer from lab scale to commercial scale. PMID:27134535

  12. Enhanced chemoprophylactic and clinical efficacy of albendazole formulated as solid dispersions in experimental cystic echinococcosis.

    Science.gov (United States)

    Pensel, Patricia E; Castro, Silvina; Allemandi, Daniel; Bruni, Sergio Sánchez; Palma, Santiago D; Elissondo, María Celina

    2014-06-16

    Cystic echinococcosis is a chronic, complex, and still neglected disease. Although albendazole has demonstrated efficacy, only about one-third of patients experience complete remission or cure and 30-50% of treated patients develop some evidence of a therapeutic response. Different strategies have been developed in order to improve the albendazole water solubility and dissolution rate. The aim of the current work was to investigate the chemoprophylactic and clinical efficacy of an albendazole:poloxamer 188 solid dispersion formulation on mice infected with Echinococcus granulosus metacestodes. Albendazole formulated as solid dispersion had greater chemoprophylactic and clinical efficacy than albendazole alone. The improved in therapeutic efficacy could be a consequence of the increase in the systemic availability of albendazole sulfoxide. The work reported here demonstrates that in vivo treatment with albendazole:poloxamer 188 impairs the development of the hydatid cysts. This new pharmacotechnically based strategy could be a suitable alternative for treating cystic echinococcosis in humans. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Modified emission-transmission method for determining trace elements in solid samples using the XRF techniques

    International Nuclear Information System (INIS)

    Poblete, V.; Alvarez, M.; Hermosilla, M.

    2000-01-01

    This is a study of an analysis of trace elements in medium thick solid samples, by the modified transmission emission method, using the energy dispersion X-ray fluorescence technique (EDXRF). The effects of absorption and reinforcement are the main disadvantages of the EDXRF technique for the quantitative analysis of bigger elements and trace elements in solid samples. The implementation of this method and its application to a variety of samples was carried out using an infinitely thick multi-element white sample that calculates the correction factors by absorbing all the analytes in the sample. The discontinuities in the masic absorption coefficients versus energies association for each element, with medium thick and homogenous samples, are analyzed and corrected. A thorough analysis of the different theoretical and test variables are proven by using real samples, including certified material with known concentration. The simplicity of the calculation method and the results obtained show the method's major precision, with possibilities for the non-destructive routine analysis of different solid samples, using the EDXRF technique (author)

  14. 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.

  15. A Miniaturized Extruder to Prototype Amorphous Solid Dispersions: Selection of Plasticizers for Hot Melt Extrusion.

    Science.gov (United States)

    Lauer, Matthias E; Maurer, Reto; Paepe, Anne T De; Stillhart, Cordula; Jacob, Laurence; James, Rajesh; Kojima, Yuki; Rietmann, Rene; Kissling, Tom; van den Ende, Joost A; Schwarz, Sabine; Grassmann, Olaf; Page, Susanne

    2018-05-19

    Hot-melt extrusion is an option to fabricate amorphous solid dispersions and to enhance oral bioavailability of poorly soluble compounds. The selection of suitable polymer carriers and processing aids determines the dissolution, homogeneity and stability performance of this solid dosage form. A miniaturized extrusion device (MinEx) was developed and Hypromellose acetate succinate type L (HPMCAS-L) based extrudates containing the model drugs neurokinin-1 (NK1) and cholesterylester transfer protein (CETP) were manufactured, plasticizers were added and their impact on dissolution and solid-state properties were assessed. Similar mixtures were manufactured with a lab-scale extruder, for face to face comparison. The properties of MinEx extrudates widely translated to those manufactured with a lab-scale extruder. Plasticizers, Polyethyleneglycol 4000 (PEG4000) and Poloxamer 188, were homogenously distributed but decreased the storage stability of the extrudates. Stearic acid was found condensed in ultrathin nanoplatelets which did not impact the storage stability of the system. Depending on their distribution and physicochemical properties, plasticizers can modulate storage stability and dissolution performance of extrudates. MinEx is a valuable prototyping-screening method and enables rational selection of plasticizers in a time and material sparing manner. In eight out of eight cases the properties of the extrudates translated to products manufactured in lab-scale extrusion trials.

  16. Comparative study of sustained-release lipid microparticles and solid dispersions containing ibuprofen

    Directory of Open Access Journals (Sweden)

    Hugo Almeida

    2012-09-01

    Full Text Available Ibuprofen is one of the most important non-steroidal anti-inflammatory drugs used in the treatment of inflammatory diseases. In its pure state, ibuprofen presents poor physical and mechanical characteristics and its use in solid dosage forms needs the addition of excipients that improve these properties. The selection of the best excipients and the most suitable pharmaceutical dosage form to carry ibuprofen is very important for the industrial success of this drug. Given these factors, lipid microparticles and solid dispersions of ibuprofen with cetyl alcohol, stearic acid, and hydrogenated castor oil were prepared. These formulations were intended to improve the physical and mechanical characteristics and to sustain the release of this drug. Physical mixtures were also prepared with the same ingredients in similar proportions. The solid dispersions of ibuprofen/stearic acid and ibuprofen/hydrogenated castor oil showed the best flow characteristics compared with pure ibuprofen. Further, gelatin capsules filled with lipid microparticles and solid dispersions were submitted to dissolution tests in order to study the influence of the prepared systems in the release profiles of ibuprofen. Prolonged release of ibuprofen was achieved with the lipid microparticles and solid dispersions prepared with the different types of excipients.O ibuprofeno é um dos antiinflamatórios não esteróides mais utilizados no tratamento de patologias associadas a processos inflamatórios. Este fármaco, quando no seu estado puro, apresenta características físicas e mecânicas pouco satisfatórias e a sua utilização em formas sólidas só é possível se forem adicionados excipientes que permitam melhorar estas propriedades. A seleção dos excipientes ideais e da forma farmacêutica mais adequada para veicular o ibuprofeno é fundamental para o sucesso industrial deste fármaco. Tendo em conta estes fatores, prepararam-se micropartículas lipídicas e dispersões s

  17. 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:

  18. 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:

  19. 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.

  20. Peptide-Loaded Solid Lipid Nanoparticles Prepared through Coacervation Technique

    Directory of Open Access Journals (Sweden)

    Marina Gallarate

    2011-01-01

    Full Text Available Stearic acid solid lipid nanoparticles were prepared according to a new technique, called coacervation. The main goal of this experimental work was the entrapment of peptide drugs into SLN, which is a difficult task, since their chemical characteristics (molecular weight, hydrophilicity, and stability hamper peptide-containing formulations. Insulin and leuprolide, chosen as model peptide drugs, were encapsulated within nanoparticles after hydrophobic ion pairing with anionic surfactants. Peptide integrity was maintained after encapsulation, and nanoparticles can act in vitro as a sustained release system for peptide.

  1. Treatment and disposal techniques of dangerous municipal solid wastes

    International Nuclear Information System (INIS)

    Beone, G.; Carbone, A.I.; Zagaroli, M.

    1989-01-01

    This paper describes the qualitative and quantitative features of the different types of dangerous municipal solid wastes, according to Italian law. In the second part the impact on environment and man health is presented. This impact should be minimized by suitable controlled disposal techniques, which differ from other municipal waste treatments. Finally, the paper deals with the most appropriate systems for treatment and disposal of such kind of waste. Particularly, some research activities in the field of metal recovery from used batteries, sponsored by ENEA, and carrying out by private companies, are described. (author)

  2. 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

  3. A new percolation model for composite solid electrolytes and dispersed ionic conductors

    Science.gov (United States)

    Risyad Hasyim, Muhammad; Lanagan, Michael T.

    2018-02-01

    Composite solid electrolytes (CSEs) including conductor/insulator composites known as dispersed ionic conductors (DICs) have motivated the development of novel percolation models that describe their conductivity. Despite the long history, existing models lack in one or more key areas: (1) rigorous foundation for their physical theory, (2) explanation for non-universal conductor-insulator transition, (3) classification of DICs, and (4) extension to frequency-domain. This work describes a frequency-domain effective medium approximation (EMA) of a bond percolation model for CSEs. The EMA is derived entirely from Maxwell’s equations and contains basic microstructure parameters. The model was applied successfully to several composite systems from literature. Simulations and fitting of literature data address these key areas and illustrate the interplay between space charge layer properties and bulk microstructure.

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

    Directory of Open Access Journals (Sweden)

    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.

  5. Preparation and investigation of mefenamic acid - polyethylene glycol - sucrose ester solid dispersions.

    Science.gov (United States)

    Fülöp, Ibolya; Gyéresi, Árpád; Kiss, Lóránd; Deli, Mária A; Croitoru, Mircea Dumitru; Szabó-Révész, Piroska; Aigner, Zoltán

    2015-12-01

    Mefenamic acid (MA) is a widely used non-steroidal antiinflammatory (NSAID) drug. The adverse effects typical of NSAIDs are also present in the case of MA, partly due to its low water solubility. The aim of this study was to increase the water solubility of MA in order to influence its absorption and bioavailability. Solid dispersions of MA were prepared by the melting method using polyethylene glycol 6000 and different types (laurate, D-1216; palmitate, P-1670; stearate, S-1670) and amounts of sucrose esters as carriers. The X-ray diffraction results show that MA crystals were not present in the products. Dissolution tests carried out in artificial intestinal juice showed that the product containing 10 % D-1216 increased water solubility about 3 times. The apparent permeability coefficient of MA across human Caco-2 intestinal epithelial cell layers was high and, despite the difference in solubility, there was no further increase in drug penetration in the presence of the applied additives.

  6. Polymer⁻Surfactant System Based Amorphous Solid Dispersion: Precipitation Inhibition and Bioavailability Enhancement of Itraconazole.

    Science.gov (United States)

    Feng, Disang; Peng, Tingting; Huang, Zhengwei; Singh, Vikramjeet; Shi, Yin; Wen, Ting; Lu, Ming; Quan, Guilan; Pan, Xin; Wu, Chuanbin

    2018-04-24

    The rapid release of poorly water-soluble drugs from amorphous solid dispersion (ASD) is often associated with the generation of supersaturated solution, which provides a strong driving force for precipitation and results in reduced absorption. Precipitation inhibitors, such as polymers and surfactants, are usually used to stabilize the supersaturated solution by blocking the way of kinetic or thermodynamic crystal growth. To evaluate the combined effect of polymers and surfactants on maintaining the supersaturated state of itraconazole (ITZ), various surfactants were integrated with enteric polymer hydroxypropyl methylcellulose acetate succinate (HPMC AS) to develop polymer⁻surfactant based solid dispersion. The supersaturation stability was investigated by in vitro supersaturation dissolution test and nucleation induction time measurement. Compared to the ASD prepared with HPMC AS alone, the addition of d-alpha-tocopheryl polyethylene glycol 1000 succinate (TPGS) exhibited a synergistic effect on precipitation inhibition. The results indicated that the TPGS not only significantly reduced the degree of supersaturation which is the driving force for precipitation, but also provided steric hindrance to delay crystal growth by absorbing onto the surface of small particles. Subsequently, the formulations were evaluated in vivo in beagle dogs. Compared with commercial product Sporanox ® , the formulation prepared with HPMC AS/TPGS exhibited a 1.8-fold increase in the AUC (0⁻24 h) of ITZ and a 1.43-fold increase of hydroxyitraconazole (OH-ITZ) in the plasma. Similarly, the extent of absorption was increased by more than 40% when compared to the formulation prepared with HPMC AS alone. The results of this study demonstrated that the ASD based on polymer⁻surfactant system could obviously inhibit drug precipitation in vitro and in vivo, which provides a new access for the development of ASD for poorly water-soluble drug.

  7. Characterization, in Vivo and in Vitro Evaluation of Solid Dispersion of Curcumin Containing d-α-Tocopheryl Polyethylene Glycol 1000 Succinate and Mannitol

    OpenAIRE

    Im-Sook Song; Jin-Sun Cha; Min-Koo Choi

    2016-01-01

    The aim of this study was to prepare a solid dispersion formulation of curcumin to enhance its solubility, dissolution rate, and oral bioavailability. The formulation was prepared with d-α-tocopheryl polyethylene glycol 1000 succinate (TPGS) and mannitol using solvent evaporation and freeze-drying methods, which yielded a solid dispersion composed of curcumin, TPGS, and mannitol at a ratio of 1:10:15 (w/w/w). The solubility and dissolution rate of the curcumin solid dispersion markedly improv...

  8. Solid-State NMR Investigation of Drug-Excipient Interactions and Phase Behavior in Indomethacin-Eudragit E Amorphous Solid Dispersions.

    Science.gov (United States)

    Lubach, Joseph W; Hau, Jonathan

    2018-02-20

    To investigate the nature of drug-excipient interactions between indomethacin (IMC) and methacrylate copolymer Eudragit® E (EE) in the amorphous state, and evaluate the effects on formulation and stability of these amorphous systems. Amorphous solid dispersions containing IMC and EE were spray dried with drug loadings from 20% to 90%. PXRD was used to confirm the amorphous nature of the dispersions, and DSC was used to measure glass transition temperatures (T g ). 13 C and 15 N solid-state NMR was utilized to investigate changes in local structure and protonation state, while 1 H T 1 and T 1ρ relaxation measurements were used to probe miscibility and phase behavior of the dispersions. T g values for IMC-EE solid dispersions showed significant positive deviations from predicted values in the drug loading range of 40-90%, indicating a relatively strong drug-excipient interaction. 15 N solid-state NMR exhibited a change in protonation state of the EE basic amine, with two distinct populations for the EE amine at -360.7 ppm (unprotonated) and -344.4 ppm (protonated). Additionally, 1 H relaxation measurements showed phase separation at high drug load, indicating an amorphous ionic complex and free IMC-rich phase. PXRD data showed all ASDs up to 90% drug load remained physically stable after 2 years. 15 N solid-state NMR experiments show a change in protonation state of EE, indicating that an ionic complex indeed forms between IMC and EE in amorphous solid dispersions. Phase behavior was determined to exhibit nanoscale phase separation at high drug load between the amorphous ionic complex and excess free IMC.

  9. Effect of composition in the development of carbamazepine hot-melt extruded solid dispersions by application of mixture experimental design.

    Science.gov (United States)

    Djuris, Jelena; Ioannis, Nikolakakis; Ibric, Svetlana; Djuric, Zorica; Kachrimanis, Kyriakos

    2014-02-01

    This study investigates the application of hot-melt extrusion for the formulation of carbamazepine (CBZ) solid dispersions, using polyethyleneglycol-polyvinyl caprolactam-polyvinyl acetate grafted copolymer (Soluplus, BASF, Germany) and polyoxyethylene-polyoxypropylene block copolymer (Poloxamer 407). In agreement with the current Quality by Design principle, formulations of solid dispersions were prepared according to a D-optimal mixture experimental design, and the influence of formulation composition on the properties of the dispersions (CBZ heat of fusion and release rate) was estimated. Prepared solid dispersions were characterized using differential scanning calorimetry, attenuated total reflectance infrared spectroscopy and hot stage microscopy, as well as by determination of the dissolution rate of CBZ from the hot-melt extrudates. Solid dispersions of CBZ can be successfully prepared using the novel copolymer Soluplus. Inclusion of Poloxamer 407 as a plasticizer facilitated the processing and decreased the hardness of hot-melt extrudates. Regardless of their composition, all hot-melt extrudates displayed an improvement in the release rate compared to the pure CBZ, with formulations having the ratio of CBZ : Poloxamer 407 = 1 : 1 showing the highest increase in CBZ release rate. Interactions between the mixture components (CBZ and polymers), or quadratic effects of the components, play a significant role in overall influence on the CBZ release rate. © 2013 Royal Pharmaceutical Society.

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

    Directory of Open Access Journals (Sweden)

    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.

  11. 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.

  12. 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....

  13. Physicochemical characterization of atorvastatin calcium/ezetimibe amorphous nano-solid dispersions prepared by electrospraying method.

    Science.gov (United States)

    Jahangiri, Azin; Barzegar-Jalali, Mohammad; Javadzadeh, Yousef; Hamishehkar, Hamed; Adibkia, Khosro

    2017-09-01

    In the present study, electrospraying was applied as a novel method for the fabrication of amorphous nano-solid dispersions (N-SDs) of atorvastatin calcium (ATV), ezetimibe (EZT), and ATV/EZT combination as poorly water-soluble drugs. N-SDs were prepared using polyvinylpyrrolidone K30 as an amorphous carrier in 1:1 and 1:5 drug to polymer ratios and the total solid (including drug and polymer) concentrations of 10 and 20% (w/v). The prepared formulations were further investigated for their morphological, physicochemical, and dissolution properties. Scanning electron microscopy studies indicated that the morphology and diameter of the electrosprayed samples (ESs) were influenced by the solution concentration and drug:polymer ratio, so that an increase in the solution concentration resulted in fiber formation while an increase in the polymer ratio led to enhancement of the particle diameter. Differential scanning calorimetry and X-ray powder diffraction studies together with in vitro dissolution test revealed that the ESs were present in an amorphous form with improved dissolution properties. Infrared spectroscopic studies showed hydrogen-bonding interaction between the drug and polymer in ESs. Since the electrospraying method benefits from the both amorphization and nanosizing effect, this novel approach seems to be an efficient method for the fabrication of N-SDs of poorly water-soluble drugs.

  14. New technique for levitating solid particles using a proton beam

    International Nuclear Information System (INIS)

    Misconi, N.Y.

    1996-01-01

    A new technique for levitating solid particles inside a vacuum chamber is developed using a proton beam. This new technique differs from the classical laser-levitation technique invented by Ashkin in that it does not heat up light-absorbing levitated particles to vaporization. This unique property of the method will make it possible to levitate real interplanetary dust particles in a vacuum chamber and study their spin-up dynamics in a ground-based laboratory. It is found that a flux of protons from a proton gun of ∼ 10 15 cm -2 sec -1 is needed to levitate a 10-mm particle. Confinement of the levitated particle can be achieved by a Z or θ pinch to create a gravity well, or by making the beam profile doughnut in shape. In levitating real interplanetary particles, two spin-up mechanisms can be investigated using this technique: one is the Paddack Effect and the other is a spin-up mechanism by the interaction of F-coronal dust with CMEs (Coronal Mass Ejections). The real interplanetary particles were collected by Brownie and associates (also known as the Brownie Particles) from the earth's upper atmosphere. (author)

  15. Initial Drug Dissolution from Amorphous Solid Dispersions Controlled by Polymer Dissolution and Drug-Polymer Interaction.

    Science.gov (United States)

    Chen, Yuejie; Wang, Shujing; Wang, Shan; Liu, Chengyu; Su, Ching; Hageman, Michael; Hussain, Munir; Haskell, Roy; Stefanski, Kevin; Qian, Feng

    2016-10-01

    To identify the key formulation factors controlling the initial drug and polymer dissolution rates from an amorphous solid dispersion (ASD). Ketoconazole (KTZ) ASDs using PVP, PVP-VA, HMPC, or HPMC-AS as polymeric matrix were prepared. For each drug-polymer system, two types of formulations with the same composition were prepared: 1. Spray dried dispersion (SDD) that is homogenous at molecular level, 2. Physical blend of SDD (80% drug loading) and pure polymer (SDD-PB) that is homogenous only at powder level. Flory-Huggins interaction parameters (χ) between KTZ and the four polymers were obtained by Flory-Huggins model fitting. Solution (13)C NMR and FT-IR were conducted to investigate the specific drug-polymer interaction in the solution and solid state, respectively. Intrinsic dissolution of both the drug and the polymer from ASDs were studied using a Higuchi style intrinsic dissolution apparatus. PXRD and confocal Raman microscopy were used to confirm the absence of drug crystallinity on the tablet surface before and after dissolution study. In solid state, KTZ is completely miscible with PVP, PVP-VA, or HPMC-AS, demonstrated by the negative χ values of -0.36, -0.46, -1.68, respectively; while is poorly miscible with HPMC shown by a positive χ value of 0.23. According to solution (13)C NMR and FT-IR studies, KTZ interacts with HPMC-AS strongly through H-bonding and dipole induced interaction; with PVPs and PVP-VA moderately through dipole-induced interactions; and with HPMC weakly without detectable attractive interaction. Furthermore, the "apparent" strength of drug-polymer interaction, measured by the extent of peak shift on NMR or FT-IR spectra, increases with the increasing number of interacting drug-polymer pairs. For ASDs with the presence of considerable drug-polymer interactions, such as KTZ/PVPs, KTZ/PVP-VA, or KTZ /HPMC-AS systems, drug released at the same rate as the polymer when intimate drug-polymer mixing was ensured (i.e., the SDD systems

  16. Analysis of a nanocrystalline polymer dispersion of ebselen using solid-state NMR, Raman microscopy, and powder X-ray diffraction.

    Science.gov (United States)

    Vogt, Frederick G; Williams, Glenn R

    2012-07-01

    Nanocrystalline drug-polymer dispersions are of significant interest in pharmaceutical delivery. The purpose of this work is to demonstrate the applicability of methods based on two-dimensional (2D) and multinuclear solid-state NMR (SSNMR) to a novel nanocrystalline pharmaceutical dispersion of ebselen with polyvinylpyrrolidone-vinyl acetate (PVP-VA), after initial characterization with other techniques. A nanocrystalline dispersion of ebselen with PVP-VA was prepared and characterized by powder X-ray diffraction (PXRD), confocal Raman microscopy and mapping, and differential scanning calorimetry (DSC), and then subjected to detailed 1D and 2D SSNMR analysis involving ¹H, ¹³C, and ⁷⁷Se isotopes and ¹H spin diffusion. PXRD was used to show that dispersion contains nanocrystalline ebselen in the 35-60 nm size range. Confocal Raman microscopy and spectral mapping were able to detect regions where short-range interactions may occur between ebselen and PVP-VA. Spin diffusion effects were analyzed using 2D SSNMR experiments and are able to directly detect interactions between ebselen and the surrounding PVP-VA. The methods used here, particularly the 2D SSNMR methods based on spin diffusion, provided detailed structural information about a nanocrystalline polymer dispersion of ebselen, and should be useful in other studies of these types of materials.

  17. Spray freeze drying to produce a stable Delta(9)-tetrahydrocannabinol containing inulin-based solid dispersion powder suitable for inhalation

    NARCIS (Netherlands)

    van Drooge, Dirk-Jan; Hinrichs, Wouter L J; Dickhoff, Bastiaan H J; Elli, Marco N A; Visser, Marinella R; Zijlstra, Gerrit S; Frijlink, Henderik W

    2005-01-01

    The purpose of this study is to investigate whether spray freeze drying produces an inhalable solid dispersion powder in which Delta(9)-tetrahydrocannabinol (THC) is stabilised. Solutions of THC and inulin in a mixture of tertiary butanol (TBA) and water were spray freeze dried. Drug loads varied

  18. 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

  19. 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.

  20. Pharmaceutical development of an amorphous solid dispersion formulation of elacridar hydrochloride for proof-of-concept clinical studies

    NARCIS (Netherlands)

    Sawicki, E.; Schellens, J. H M; Beijnen, J. H.; Nuijen, B.

    2017-01-01

    Objective: A novel tablet formulation containing an amorphous solid dispersion (ASD) of elacridar hydrochloride was developed with the purpose to resolve the drug’s low solubility in water and to conduct proof-of-concept clinical studies. Significance: Elacridar is highly demanded for

  1. Pigment dispersion syndrome associated with intraocular lens implantation: a new surgical technique.

    Science.gov (United States)

    Canut Jordana, M Isabel; Pérez Formigó, Daniel; Abreu González, Rodrigo; Nadal Reus, Jeroni

    2010-11-11

    We report the case of a myopic patient who, after intraocular lens transplant in the posterior chamber, suffered elevated intraocular pressure due to pigment dispersion, with recurrent episodes of blurred vision. The patient was treated with a new surgical technique that can avoid potential iridolenticular contact. Complete ophthalmologic examination and optical coherence tomography (OCT) of the anterior segment were performed. Contact between the pigmentary epithelium and the iris with an intraocular lens was revealed by utrasound biomicroscopy and OCT. In this case, Nd:YAG laser iridotomy and laser iridoplasty were not effective for iridolenticular separation and control of the pigment dispersion. We propose a new technique: stitches on the surface of the iris to obtain good iridolenticular separation and good intraocular pressure control. Stitches on the iris surface should be considered as optional therapy in pigmentary glaucoma secondary to intraocular lens implantation. This surgical technique can avoid potential iridolenticular contacts more definitively.

  2. Physiochemical Characterization and Release Rate Studies of SolidDispersions of Ketoconazole with Pluronic F127 and PVP K-30

    Science.gov (United States)

    Kumar, Pankaj; Mohan, Chander; KanamSrinivasan Uma Shankar, Mara; Gulati, Monica

    2011-01-01

    In the present study solid dispersions of the antifungal drug Ketoconazole were prepared with Pluronic F-127 and PVP K-30 with an intention to improve its dissolution properties. Investigations of the properties of the dispersions were performed using release studies, Differential scanning calorimetery (DSC), X-ray powder diffraction (XRD) and Fourier transform infrared (FTIR). The results obtained showed that the rate of dissolution of Ketoconazole was considerably improved when formulated in solid dispersions with PVP K-30 and Pluronic F-127 as compared with pure drug and physical mixtures. The results from DSC and XRD studies showed the transition of crystalline nature of drug to amorphous form, while FTIR studies demonstrated the absence of drug-carriers interaction. PMID:24250403

  3. Bioenhanced advanced third generation solid dispersion of tadalafil: Repurposing with improved therapy in pyelonephritis

    Directory of Open Access Journals (Sweden)

    Prashant P. Mande

    2017-11-01

    Full Text Available Tadalafil (TDL a BCS-II drug is recently reported for repurposing nephroprotective effect in Pyelonephritis (PN. However, poor water solubility and dissolution rate limited oral bioavailability pose serious challenges in its therapeutic applications. We present an advanced third generation Solid Dispersion (SD of TDL comprising a polymer in combination with a Self Micro-emulsifying Composition (SMEC to achieve high drug loading, improved stability and rapid dissolution of TDL for enhancing bioavailability and efficacy in PN. TDL-SMEC-SD was coated onto rapidly disintegrating inert tablet cores which disintegrated rapidly in water to release SD as a film. TDL-SMEC-SD was evaluated for in-vivo oral bioavailability and in-vivo efficacy in lipopolysaccharide-induced PN in rats. TDL exhibited high solubility (45.6 mg/ml in the SMEC. TDL-SMEC-SD exhibited remarkably high TDL loading (45%w/w, exceptionally low contact angle (9°, rapid in-vitro release (t50 7.3 min, microemulsion formation (globule size ~100 nm in aqueous dispersion, and stability as per ICH guidelines. SEM, DSC, and XRD confirmed high physical stability. A relative bioavailability of 350% and 150% compared to TDL and TDL-SD without SMEC respectively, established the superiority of TDL-SMEC-SD. A significant reduction in serum creatinine, blood urea nitrogen and nitric oxide levels in the lipopolysaccharide-induced PN confirmed the benefit of the TDL-SMEC-SD. The advanced third generation SMEC SDs presents the possibility of platform technology for bioenhancement of poorly water soluble drugs.

  4. Rheology Guided Rational Selection of Processing Temperature To Prepare Copovidone-Nifedipine Amorphous Solid Dispersions via Hot Melt Extrusion (HME).

    Science.gov (United States)

    Yang, Fengyuan; Su, Yongchao; Zhang, Jingtao; DiNunzio, James; Leone, Anthony; Huang, Chengbin; Brown, Chad D

    2016-10-03

    The production of amorphous solid dispersions via hot melt extrusion (HME) relies on elevated temperature and prolonged residence time, which can result in potential degradation and decomposition of thermally sensitive components. Herein, the rheological properties of a physical mixture of polymer and an active pharmaceutical ingredient (API) were utilized to guide the selection of appropriate HME processing temperature. In the currently studied copovidone-nifedipine system, a critical temperature, which is substantially lower (∼13 °C) than the melting point of crystalline API, was captured during a temperature ramp examination and regarded as the critical point at which the API could molecularly dissolve into the polymer. Based on the identification of this critical point, various solid dispersions were prepared by HME processing below, at, and above the critical temperature (both below and above the melting temperature (T m ) of crystalline API). In addition, the resultant extrudates along with two control solid dispersions prepared by physical mixing and cryogenic milling were assessed by X-ray diffraction, differential scanning calorimetry, hot stage microscopy, rheology, and solid-state NMR. Physicochemical properties of resultant solid dispersions indicated that the identified critical temperature is sufficient for the polymer-API system to reach a molecular-level mixing, manifested by the transparent and smooth appearance of extrudates, the absence of API crystalline diffraction and melting peaks, dramatically decreased rheological properties, and significantly improved polymer-API miscibility. Once the critical temperature has been achieved, further raising the processing temperature only results in limited improvement of API dispersion, reflected by slightly reduced storage modulus and complex viscosity and limited improvement in miscibility.

  5. Manufacturing Amorphous Solid Dispersions with a Tailored Amount of Crystallized API for Biopharmaceutical Testing.

    Science.gov (United States)

    Theil, Frank; Milsmann, Johanna; Anantharaman, Sankaran; van Lishaut, Holger

    2018-05-07

    The preparation of an amorphous solid dispersion (ASD) by dissolving a poorly water-soluble active pharmaceutical ingredient (API) in a polymer matrix can improve the bioavailability by orders of magnitude. Crystallization of the API in the ASD, though, is an inherent threat for bioavailability. Commonly, the impact of crystalline API on the drug release of the dosage form is studied with samples containing spiked crystallinity. These spiked samples possess implicit differences compared to native crystalline samples, regarding size and spatial distribution of the crystals as well as their molecular environment. In this study, we demonstrate that it is possible to grow defined amounts of crystalline API in solid dosage forms, which enables us to study the biopharmaceutical impact of actual crystallization. For this purpose, we studied the crystal growth in fenofibrate tablets over time under an elevated moisture using transmission Raman spectroscopy (TRS). As a nondestructive method to assess API crystallinity in ASD formulations, TRS enables the monitoring of crystal growth in individual dosage forms. Once the kinetic trace of the crystal growth for a certain environmental condition is determined, this method can be used to produce samples with defined amounts of crystallized API. To investigate the biopharmaceutical impact of crystallized API, non-QC dissolution methods were used, designed to identify differences between the various amounts of crystalline materials present. The drug release in the samples manufactured in this fashion was compared to that of samples with spiked crystallinity. In this study, we present for the first time a method for targeted crystallization of amorphous tablets to simulate crystallized ASDs. This methodology is a valuable tool to generate model systems for biopharmaceutical studies on the impact of crystallinity on the bioavailability.

  6. Nuclear techniques and the disposal of non-radioactive solid wastes

    International Nuclear Information System (INIS)

    Landsberger, S.; Buchholz, B.

    1993-01-01

    One of the most vital and persistent public health challenges facing local, state, and national governments is the disposal of solid waste produced from industrial, utility, and municipal sources. There is a growing interest in the monitoring, control, and safe disposal of the chemical constituents arising from these sources. For instance, it is now well known that the release of by products from coal-fired power plants - namely airborne particulates, bottom ash, and fly ash - can have adverse effects on air and water quality. It is therefore important that reliable chemical analytical techniques are readily available to assess the impact of widespread disposal practices of organic and inorganic chemicals. The use of nuclear and nuclear-related analytical techniques - such as neutron activation analysis, energy dispersive x-ray fluorescence and particle induced X-ray emission - have become widespread in major areas of science and technology. These methods and techniques have important applications in such work since they can be used for both the determination of specific individual pollutants (e.g. toxic heavy metals) and multi-elemental analyses for source identification and apportionment purposes. Other nuclear techniques, such as isotope tracers, have also had wide acceptance in characterizing diffusion patterns for metals in soil and aqueous environments and water pollution flows. 1 graph., 1 tab

  7. Effects of tablet formulation and subsequent film coating on the supersaturated dissolution behavior of amorphous solid dispersions.

    Science.gov (United States)

    Sakai, Toshiro; Hirai, Daiki; Kimura, Shin-Ichiro; Iwao, Yasunori; Itai, Shigeru

    2018-04-05

    The effects of tablet preparation and subsequent film coating with amorphous solid dispersion (ASD) particles that were composed of a drug with poor water solubility and hydrophilic polymers were investigated. ASD particles were prepared with a drug and vinylpyrrolidone-vinyl acetate copolymer (PVPVA) or polyvinylpyrrolidone (PVP) at a weight ratio of 1:1 or 1:2 using a melt extrusion technique. Tablets were prepared by conventional direct compression followed by pan coating. A mathematical model based on the Noyes-Whitney equation assuming that stable crystals precipitated at the changeable surface area of the solid-liquid interface used to estimate drug dissolution kinetics in a non-sink dissolution condition. All the ASD particles showed a maximum dissolution concentration approximately ten times higher than that of the crystalline drug. The ASD particles with PVPVA showed higher precipitation rate with lower polymer ratio, while PVP did not precipitate within 960 min regardless of the polymer ratio, suggesting the ASD particles of 1:1 drug:PVPVA (ASD-1) were the most unstable among the ASD particles considered. The dissolution of a core tablet with ASD-1 showed less supersaturation and a much higher precipitation rate than those of ASD-1 particles. However, a film-coated tablet or core tablet with a trace amount of hydroxypropylmethylcellulose (HPMC) showed a similar dissolution profile to that of the ASD-1 particles, indicating HPMC had a remarkable precipitation inhibition effect. Overall, these results suggest that tablet preparation with ASD may adversely affect the maintenance of supersaturation; however, this effect can be mitigated by adding an appropriate precipitation inhibitor to the formulation. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. Solid polymer electrolyte composite membrane comprising a porous support and a solid polymer electrolyte including a dispersed reduced noble metal or noble metal oxide

    Science.gov (United States)

    Liu, Han; Mittelsteadt, Cortney K; Norman, Timothy J; Griffith, Arthur E; LaConti, Anthony B

    2015-02-24

    A solid polymer electrolyte composite membrane and method of manufacturing the same. According to one embodiment, the composite membrane comprises a thin, rigid, dimensionally-stable, non-electrically-conducting support, the support having a plurality of cylindrical, straight-through pores extending perpendicularly between opposing top and bottom surfaces of the support. The pores are unevenly distributed, with some or no pores located along the periphery and more pores located centrally. The pores are completely filled with a solid polymer electrolyte, the solid polymer electrolyte including a dispersed reduced noble metal or noble metal oxide. The solid polymer electrolyte may also be deposited over the top and/or bottom surfaces of the support.

  9. Impact of noise barriers on the dispersal of solid pollutants from car emissions and their deposition in soil

    Directory of Open Access Journals (Sweden)

    Wawer Małgorzata

    2017-03-01

    Full Text Available Despite the existence of various methods aimed at protecting the environment from the negative influence of roads, there is a lack of adequate techniques for monitoring and reducing the spread of roadside pollution into the air and soils. The aim of this study was to assess the impact of noise barriers (sound walls on the dispersal and soil deposition of solid pollutants from car emissions, based on both quantitative and qualitative analysis. Magnetic susceptibility measurements, trace elements analyses, and platinum (Pt and rhodium (Rh content determinations were performed on soil samples collected in the vicinity of various types of noise barrier. Previous investigations have shown that most traffic emissions are deposited in the close vicinity of roads (up to 10 m, with pollution levels decreasing with increasing distance from the road edge. However, the results of the present study indicate that this distribution is disturbed in areas in which noise barriers are located. Moreover, additional soil enrichment with trace elements was observed at approx. 10-15 m behind the barriers. The spatial distribution of trace elements contents in the tested soil samples corresponded to the magnetic susceptibility values. High Fe, Zn, Mn and Pb levels were observed adjacent to noise barriers composed of sawdust concrete and steel panels.

  10. Dispersion of dielectric permittivity and magnetic properties of solid solution PZT–PFT

    Directory of Open Access Journals (Sweden)

    Skulski Ryszard

    2015-09-01

    Full Text Available In this paper we present the results of investigations into ceramic samples of solid solution (1-x(PbZr0.53Ti0.47O3- x(PbFe0.5Ta0.503 (i.e. (1-xPZT-xPFT with x = 0.25, 0.35 and 0.45. We try to find the relation between the character of dielectric dispersion at various temperatures and the composition of this solution. We also describe the magnetic properties of investigated samples. With increasing the content of PFT also mass magnetization and mass susceptibility increase (i.e. magnetic properties are more pronounced at every temperature. The temperature dependences of mass magnetization and re­ciprocal of mass susceptibility have similar runs for all the compositions. However, our magnetic investigations exhibit weak antiferromagnetic ordering instead of the ferromagnetic one at room temperature. We can also say that up to room tempera­ture any magnetic phase transition has not occurred. It may be a result of the conditions of the technological process during producing our PZT-PFT ceramics.

  11. Use of solid dispersions to increase stability of dithranol in topical formulations

    Directory of Open Access Journals (Sweden)

    Marilene Estanqueiro

    2014-09-01

    Full Text Available The present study was planned to improve the stability of dithranol using solid dispersions (SD. Two different SD at a 1:9 ratio of dithranol/excipient were prepared: one of them using glyceryl behenate as excipient and the other using a mixture of argan oil with stearic acid (1:8 ratio as excipient. Pure dithranol and SD of dithranol were incorporated in an oil-in-water cream and in a hydrophobic ointment in a drug/dermatological base ratio of 1:10. The physical and mechanical properties of semisolid formulations incorporating the pure drug and the developed SD were evaluated through rheological and textural analysis. To evaluate the stability, L*a*b* color space parameters of SD and semisolid formulations, and pH of hydrophilic formulations were determined at defined times, during one month. Each sample was stored at different conditions namely, light exposure (room temperature, high temperature exposition (37 °C (protected from light and protected from light (room temperature. Despite higher values of firmness and adhesiveness, hydrophobic ointment exhibited the best rheological features compared to the oil-in-water cream, namely a shear-thinning behavior and high thixotropy. These formulations have also presented more stability, with minor changes in L*a*b* color space parameters. The results of this study indicate that is possible to conclude that the developed SD contributed to the increased stability of dithranol.

  12. Investigation of itraconazole ternary amorphous solid dispersions based on povidone and Carbopol.

    Science.gov (United States)

    Meng, Fan; Meckel, Jordan; Zhang, Feng

    2017-08-30

    We investigate a ternary system that consists of itraconazole (ITZ) and two polymers: povidone K12 and Carbopol 907. The interactions between these two polymers and their effects on the properties of ternary ITZ amorphous solid dispersions (ASDs) are studied. These two polymers can form a water-insoluble complex in acidic aqueous media. The critical pH is determined to be 4.17. The weight percentage of Carbopol 907 in the interpolymer complex range from 59 to 70%, depending on the initial ratios between these two polymers in the starting solutions. This complexation is driven by a negative enthalpy change from the H-bonding between the two polymers and a positive entropy change from the freed water molecules. Due to the slow precipitation of the interpolymer complex in aqueous media, the attempt to prepare ternary ASD using solvent-controlled coprecipitation is not successful. Melt extrusion is identified to be the only viable method to prepare this ternary ASD. We find that interpolymer complex-based ASDs are physically less stable and demonstrate the poorest drug-release properties when compared to individual polymer-based binary ASDs. This study illustrates that the too strong interaction between polymers in ternary ASDs is detrimental to their performance. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Evaluation of Intestinal Absorption and Bioavailability of a Bergenin-Phospholipid Complex Solid Dispersion in Rats.

    Science.gov (United States)

    Gao, Haoshi; Wei, Yue; Xi, Long; Sun, Yuanyuan; Zhang, Tianhong

    2018-05-01

    Bergenin (BN) is a Biopharmaceutics Classification System class IV (BCS IV) drug with poor hydrophilicity and lipophilicity and is potentially eliminated by the efflux function of P-glycoprotein (P-gp). These factors may explain its low oral bioavailability. In the present study, a BN-phospholipid complex solid dispersion (BNPC-SD) was prepared by solvent evaporation and characterized based on differential scanning calorimetry, powder X-ray diffraction, scanning electron microscopy, infrared diffraction, solubility, octanol-water partition coefficient, and in vitro dissolution. To investigate how P-gp can inhibit BN absorption in vivo, the P-gp inhibitor verapamil was co-administered with BNPC-SD to Sprague Dawley rats. By in situ single-pass intestinal perfusion, the membrane permeability of BN from BNPC-SD was higher than that of BN given alone and was improved further by co-administered verapamil. A pharmacokinetics study was done in Sprague Dawley rats, with plasma BN levels estimated by high-performance liquid chromatography. C max and AUC 0 → t values for BN were significantly higher for BNPC-SD than for BN given alone and were increased further by verapamil. Thus, the relative oral bioavailability of BNPC-SD as well as BNPC-SD co-administered with verapamil was 156.33 and 202.46%, respectively, compared with the value for BN given alone. These results showed that BNPC-SD can increase the oral bioavailability of BCS IV drugs.

  14. Development and characterization of controlled release polar lipid microparticles of candesartan cilexetil by solid dispersion

    Science.gov (United States)

    Kamalakkannan, V; Puratchikody, A; Ramanathan, L

    2013-01-01

    Candesartan cilexetil (CC) is a newer class of angiotensin II receptor antagonist used for the treatment of hypertension. The solubility of the CC is very poor and its oral bioavailability is only 15%. The controlledrelease polar lipid microparticles of CC (formulations F1, F2, F3 and F4) were prepared using variable erodible lipophilic excipients like hydrogenated castor oil, stearic acid, cetostearyl alcohol and carnauba wax by fusion method. The particle sizes of polar lipid microparticles were less than 50 microns and they were irregular in shape. Drug content ranged between 98.96 ± 2.1 and 101.9 ± 1.6% were present in all the formulations. The formulation F3 showed better drug release throughout the study period in a controlled release manner. Moreover, the in vitro release showed that all the formulations were best fitted to Higuchi model. Accelerated stability studies indicated that there was no significant changes in the chemical and physical characteristics of the formulated drug product during initial and at the end of the study period. The FTIR and DSC studies showed that there was no interaction between the drug and lipophilic excipients and no polymorphic transitions in all formulations. The X-ray diffraction peak of solid dispersion indicated that the crystalline nature of CC disappeared and no new peaks could be observed, suggesting the absence of interaction between drug and excipients. PMID:24019822

  15. Dissolution and bioavailability enhancement of alpha-asarone by solid dispersions via oral administration.

    Science.gov (United States)

    Deng, Li; Wang, Yu; Gong, Tao; Sun, Xun; Zhang, Zhi-Rong

    2017-11-01

    Alpha (α)-asarone (1-propenyl-2,4,5-methoxybenzol) (ARE) has been extensively used to treat chronic obstructive pulmonary diseases (COPD), bronchial asthma, pneumonia, and epilepsy. Due to its poor solubility and bioavailability, ARE was clinically administered via intravenous injection. However, severe allergies were often reported due to the presence of solublizers in the injection formulation. In our study, we sought to explore the biopharmaceutical classification of ARE, elucidate the mechanisms behind ARE absorption, and to develop a viable formulation to improve the oral bioavailability of ARE. ARE was not a P-glycoprotein substrate, which was absorbed in the passive mode without site specificity in the gastrointestinal tract. Solid dispersions prepared using hydrophilic matrix materials such as Pluronic F68, and polyethylene glycol (PEG) of varying molecular weights (PEG4K, PEG10K, and PEG20K) were proven to significantly improve the dissolution of ARE in vitro and the oral bioavailability of ARE in rats, which represent a promising strategy for the oral administration of ARE and other BCS II compounds.

  16. 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.

  17. Solid Dispersion of Curcumin as Polymeric Films for Bioenhancement and Improved Therapy of Rheumatoid Arthritis.

    Science.gov (United States)

    Mande, Prashant P; Bachhav, Sagar S; Devarajan, Padma V

    2016-08-01

    The aim of our study was development of advanced third generation Curcumin self microemulsifying composition solid dispersion (Cur SMEC-SD) with high drug loading, improved stability, rapid in-vitro dissolution and enhanced bioavailability for improved therapy of rheumatoid arthritis. The Cur SMEC-SD comprising polymers (KollidonVA64[KVA], Eudragits, HPMC and Soluplus) and self microemulsifying composition of surfactant:co-surfactant:oil were coated onto rapidly disintegrating inert tablet core. SDs evaluated for stability, in-vitro release and bioenhancement. Cur SMEC-SDs exhibited high Cur loading of 45% w/w and microemulsion formation with globule size (~100 nm) irrespective of polymers. Among the polymers, SD with KVA revealed exceptionally low contact angle (7°C) and rapid in-vitro release (t50%-6.45 min). No crystallization was evident as confirmed by SEM, DSC and XRD and is attributed to SMEC aided solubilization/amorphisation, and interaction of KVA with Cur seen in the FTIR spectra. Stability was confirmed as per ICH guidelines. Remarkable bioenhancement with Cur SMEC-SD was confirmed by the > four fold and a two fold compared to Cur and Cur-SD without SMEC respectively. High efficacy ~ 80% compared to Indomethacin, seen with rheumatoid arthritis (RA) induced rats coupled with no adverse toxicity. The advanced third generation Cur SMEC-SD presents a practical technological advancement and suggests Cur SMEC-SD as promising alternative for RA therapy.

  18. Preparation and investigation of mefenamic acid – polyethylene glycol – sucrose ester solid dispersions

    Directory of Open Access Journals (Sweden)

    Fülöp Ibolya

    2015-12-01

    Full Text Available Mefenamic acid (MA is a widely used non-steroidal antiinflammatory (NSAID drug. The adverse effects typical of NSAIDs are also present in the case of MA, partly due to its low water solubility. The aim of this study was to increase the water solubility of MA in order to influence its absorption and bioavailability. Solid dispersions of MA were prepared by the melting method using polyethylene glycol 6000 and different types (laurate, D-1216; palmitate, P-1670; stearate, S-1670 and amounts of sucrose esters as carriers. The X-ray diffraction results show that MA crystals were not present in the products. Dissolution tests carried out in artificial intestinal juice showed that the product containing 10 % D-1216 increased water solubility about 3 times. The apparent permeability coefficient of MA across human Caco-2 intestinal epithelial cell layers was high and, despite the difference in solubility, there was no further increase in drug penetration in the presence of the applied additives.

  19. Refractive index dispersion of swift heavy ion irradiated BFO thin films using Surface Plasmon Resonance technique

    International Nuclear Information System (INIS)

    Paliwal, Ayushi; Sharma, Savita; Tomar, Monika; Singh, Fouran; Gupta, Vinay

    2016-01-01

    Highlights: • Investigated the optical properties of BiFeO_3 (BFO) thin films after irradiation using SPR. • Otto configuration has been used to excite the surface plasmons using gold metal thin film. • BFO thin films were prepared by sol–gel spin coating technique. • Examined the refractive index dispersion of pristine and irradiated BFO thin film. - Abstract: Swift heavy ion irradiation (SHI) is an effective technique to induce defects for possible modifications in the material properties. There is growing interest in studying the optical properties of multiferroic BiFeO_3 (BFO) thin films for optoelectronic applications. In the present work, BFO thin films were prepared by sol–gel spin coating technique and were irradiated using the 15 UD Pelletron accelerator with 100 MeV Au"9"+ ions at a fluence of 1 × 10"1"2 ions cm"−"2. The as-grown films became rough and porous on ion irradiation. Surface Plasmon Resonance (SPR) technique has been identified as a highly sensitive and powerful technique for studying the optical properties of a dielectric material. Optical properties of BFO thin films, before and after irradiation were studied using SPR technique in Otto configuration. Refractive index is found to be decreasing from 2.27 to 2.14 on ion irradiation at a wavelength of 633 nm. Refractive index dispersion of BFO thin film (from 405 nm to 633 nm) before and after ion radiation was examined.

  20. Refractive index dispersion of swift heavy ion irradiated BFO thin films using Surface Plasmon Resonance technique

    Energy Technology Data Exchange (ETDEWEB)

    Paliwal, Ayushi [Department of Physics and Astrophysics, University of Delhi, Delhi 110007 (India); Sharma, Savita [Department of Applied Physics, Delhi Technological University, Delhi (India); Tomar, Monika [Physics Department, Miranda House, University of Delhi, Delhi 110007 (India); Singh, Fouran [Inter University Accelerator Centre, Aruna Asaf Ali Marg, New Delhi 110075 (India); Gupta, Vinay, E-mail: drguptavinay@gmail.com [Department of Physics and Astrophysics, University of Delhi, Delhi 110007 (India)

    2016-07-15

    Highlights: • Investigated the optical properties of BiFeO{sub 3} (BFO) thin films after irradiation using SPR. • Otto configuration has been used to excite the surface plasmons using gold metal thin film. • BFO thin films were prepared by sol–gel spin coating technique. • Examined the refractive index dispersion of pristine and irradiated BFO thin film. - Abstract: Swift heavy ion irradiation (SHI) is an effective technique to induce defects for possible modifications in the material properties. There is growing interest in studying the optical properties of multiferroic BiFeO{sub 3} (BFO) thin films for optoelectronic applications. In the present work, BFO thin films were prepared by sol–gel spin coating technique and were irradiated using the 15 UD Pelletron accelerator with 100 MeV Au{sup 9+} ions at a fluence of 1 × 10{sup 12} ions cm{sup −2}. The as-grown films became rough and porous on ion irradiation. Surface Plasmon Resonance (SPR) technique has been identified as a highly sensitive and powerful technique for studying the optical properties of a dielectric material. Optical properties of BFO thin films, before and after irradiation were studied using SPR technique in Otto configuration. Refractive index is found to be decreasing from 2.27 to 2.14 on ion irradiation at a wavelength of 633 nm. Refractive index dispersion of BFO thin film (from 405 nm to 633 nm) before and after ion radiation was examined.

  1. Energy dispersion X-ray fluorescence techniques in water pollution analysis

    International Nuclear Information System (INIS)

    Holynska, B.

    1980-01-01

    Advantages and limitations of energy dispersion X-ray fluorescence methods for analysis of pollutants in water are discussed. The necessary equipment for X-ray measurement of insoluble and dissolved trace metals in water is described. Different techniques of enrichment of trace metals are presented: ion exchange on selective Chelex-100 exchanger, precipitation with chelating agents DDTC and APDC, and adsorption on activated carbon. Some results obtained using different preconcentration methods for trace metals determination in different waters are presented. (author)

  2. 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.

  3. [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.

  4. Crystalline Ethylene Oxide and Propylene Oxide Triblock Copolymer Solid Dispersion Enhance Solubility, Stability and Promoting Time- Controllable Release of Curcumin.

    Science.gov (United States)

    Alves, Thais F R; das Neves Lopes, Franciely C C; Rebelo, Marcia A; Souza, Juliana F; da Silva Pontes, Katiusca; Santos, Carolina; Severino, Patricia; Junior, Jose M O; Komatsu, Daniel; Chaud, Marco V

    2018-01-01

    The design and development of an effective medicine are, however, often faced with a number of challenges. One of them is the close relationship of drug's bioavailability with solubility, dissolution rate and permeability. The use of curcumin's (CUR) therapeutic potential is limited by its poor water solubility and low chemical stability. The purpose was to evaluate the effect of polymer and solid dispersion (SD) preparation techniques to enhance the aqueous solubility, dissolution rate and stability of the CUR. The recent patents on curcumin SD were reported as (i) curcumin with polyvinylpyrrolidone (CN20071 32500 20071214, WO2006022012 and CN20151414227 20150715), (ii) curcumin-zinc/polyvinylpyrrolidone (CN20151414227 20150715), (iii) curcumin-poloxamer 188 (CN2008171177 20080605), (iv) curcumin SD prepared by melting method (CN20161626746-20160801). SD obtained by co-preciptation or microwave fusion and the physical mixture of CUR with Poloxamer-407 (P-407), Hydroxypropylmetylcellulose-K4M (HPMC K4M) and Polyvinylpyrrolidone-K30 (PVP-K30) were prepared at the ratios of 1:2; 1:1 and 2:1. The samples were evaluated by solubility, stability, dissolution rate and characterized by SEM, PXRD, DSC and FTIR. The solubility, stability (pH 7.0) and dissolution rate were significantly greater for SD (CUR:P-407 1:2). The PXRD,SEM and DSC indicated a change in the crystalline state of CUR. The enhancement of solubility was dependent on a combination of factors including the weight ratio, preparation techniques and carrier properties. The drug release data fitted well with the Weibull equation, indicating that the drug release was controlled by diffusion, polymer relaxation and erosion occurring simultaneously. Thus, these SDs, specifically CUR:P-407 1:2 w/w, can overcome the barriers of poor bioavailability to reap many beneficial properties. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  5. Solid state welding processes for an oxide dispersion strengthened nickel-chromium-aluminum alloy

    Science.gov (United States)

    Moore, T. J.

    1975-01-01

    Solid-state welding processes were evaluated for joining TD-NiCrAl (Ni-16Cr-4Al-2ThO2) alloy sheet. Both hot-press and resistance spot welding techniques were successfully applied in terms of achieving grain growth across the bond line. Less success was achieved with a resistance seam welding process. In stress-rupture shear and tensile shear tests of lap joints at 1100 C, most failures occurred in the parent material, which indicates that the weld quality was good and that the welds were not a plane of weakness. The overall weld quality was not as good as previously attained with TD-NiCr, probably because the presence of alumina at the faying surfaces and the developmental TD-NiCrAl sheet, which was not of the quality of the TD-NiCr sheet in terms of surface flatness and dimensional control.

  6. 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

  7. Dispersion of Silicate in Tricalcium Phosphate Elucidated by Solid-State NMR

    Energy Technology Data Exchange (ETDEWEB)

    Rewal, A.; Wei, X.; Akinc, M.; Schmidt-Rohr, K.

    2008-03-12

    The dispersion of silicate in tricalcium phosphate, a resorbable bioceramics for bone replacement, has been investigated by various solid-state nuclear magnetic resonance (NMR) methods. In samples prepared with 5 and 10 mol% of both {sup 29}SiO{sub 2} and ZnO, three types of silicate have been detected: (i) SiO{sub 4}{sup 4-} (Q{sub 0} sites) with long longitudinal (T{sub 1,Si}) relaxation times ({approx} 10,000 s), which substitute for {approx}1% of PO{sub 4}{sup 3-}; (ii) silicate nanoinclusions containing Q{sub 2}, Q{sub 1}, and Q{sub 0} sites with T{sub 1,Si} 100 s, which account for most of the silicon; and (iii) crystalline Q{sub 4} (SiO{sub 2}) with long T{sub 1,Si}. Sensitivity was enhanced >100-fold by {sup 29}Si enrichment and refocused detection. The inclusions in both samples have a diameter of {approx}8 nm, as proved by {sup 29}Si{l_brace}{sup 31}P{r_brace} REDOR dephasing on a 30-ms time scale, which was simulated using a multispin approach specifically suited for nanoparticles. {sup 29}Si CODEX NMR with 30-s {sup 29}Si spin diffusion confirms that an inclusion contains >10 Si (consistent with the REDOR result of >100 Si per inclusion). Overlapping signals of silicate Q{sub 2}, Q{sub 1}, and Q{sub 0} sites were spectrally edited based on their J-couplings, using double-quantum filtering. The large inhomogeneous broadening of the Q{sub 2}, Q{sub 1}, and Q{sub 0} {sup 29}Si subspectra indicates that the nanoinclusions are amorphous.

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

    Science.gov (United States)

    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.

  9. Characterization of ultrashort laser pulses employing self-phase modulation dispersion-scan technique

    Science.gov (United States)

    Sharba, A. B.; Chekhlov, O.; Wyatt, A. S.; Pattathil, R.; Borghesi, M.; Sarri, G.

    2018-03-01

    We present a new phase characterization technique for ultrashort laser pulses that employs self-phase modulation (SPM) in the dispersion scan approach. The method can be implemented by recording a set of nonlinearly modulated spectra generated with a set of known chirp values. The unknown phase of the pulse is retrieved by linking the recorded spectra to the initial spectrum of the pulse via a phase function guessed by a function minimization iterative algorithm. This technique has many advantages over the dispersion scan techniques that use frequency conversion processes. Mainly, the use of SPM cancels out the phase and group velocity mismatch errors and dramatically widens the spectral acceptance of the nonlinear medium and the range of working wavelength. The robustness of the technique is demonstrated with smooth and complex phase retrievals using numerical examples. The method is shown to be not affected by the spatial distribution of the beam or the presence of nonlinear absorption process. In addition, we present an efficient method for phase representation based on a summation of a set of Gaussian functions. The independence of the functions from each other prevents phase coupling of any kind and facilitates a flexible phase representation.

  10. 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.

  11. Development and evaluation of gastroretentive raft forming systems incorporating curcumin-Eudragit® EPO solid dispersions for gastric ulcer treatment.

    Science.gov (United States)

    Kerdsakundee, Nattha; Mahattanadul, Sirima; Wiwattanapatapee, Ruedeekorn

    2015-08-01

    Novel raft forming systems incorporating curcumin-Eudragit® EPO solid dispersions were developed to prolong the gastric residence time and provide for a controlled release therapy of curcumin to treat gastric ulcers. The solid dispersions of curcumin with Eudragit® EPO were prepared by the solvent evaporation method at various ratios to improve the solubility and the dissolution of curcumin. The optimum weight ratio of 1:5 for curcumin to Eudragit® EPO was used to incorporate into the raft forming systems. The raft forming formulations were composed of curcumin-Eudragit® EPO solid dispersions, sodium alginate as a gelling polymer and calcium carbonate for generating divalent Ca(2+) ions and carbon dioxide to form a floating raft. All formulations formed a gelled raft in 1min and sustained buoyancy on the 0.1N hydrochloric acid (pH 1.2) surface with a 60-85% release of curcumin within 8h. The curative effect on the acetic acid-induced chronic gastric ulcer in rats was determined. The curcumin raft forming formulations at 40mg/kg once daily showed a superior curative effect on the gastric ulcer in terms of the ulcer index and healing index than the standard antisecretory agent: lansoprazole (1mg/kg, twice daily) and a curcumin suspension (40mg/kg, twice daily). These studies demonstrated that the new raft forming systems containing curcumin solid dispersions are promising carriers for a stomach-specific delivery of poorly soluble lipophilic compounds. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Physicochemical properties of direct compression tablets with spray dried and ball milled solid dispersions of tadalafil in PVP-VA.

    Science.gov (United States)

    Wlodarski, K; Tajber, L; Sawicki, W

    2016-12-01

    The aim of this research was to develop immediate release tablets comprising solid dispersion (IRSDTs) of tadalafil (Td) in a vinylpyrrolidone and vinyl acetate block copolymer (PVP-VA), characterized by improved dissolution profiles. The solid dispersion of Td in PVP-VA (Td/PVP-VA) in a weight ratio of 1:1 (w/w) was prepared using two different processes i.e. spray drying and ball milling. While the former process has been well established in the formulation of IRSDTs the latter has not been exploited in these systems yet. Regardless of the preparation method, both Td/PVP-VA solid dispersions were amorphous as confirmed by PXRD, DSC and FTIR. However, different morphology of particles (SEM) resulted in differences in water apparent solubility and disk intrinsic dissolution rate (DIDR). Both solid dispersions and crystalline Td were successfully made into directly compressible tablets at three doses of Td, i.e. 2.5mg, 10mgand20mg, yielding nine different formulations (D 1 -D 9 ). Each of the lots met the requirements set by Ph.Eur. and was evaluated with respect to appearance, diameter, thickness, mass, hardness, friability, disintegration time and content of Td. IRSDTs performed as supersaturable formulations and had significantly improved water dissolution profiles in comparison with equivalent tablets containing crystalline Td and the marketed formulations. Tablets with both spray dried and ball milled Td/PVP-VA revealed the greatest improvement in dissolution depending on the investigated doses, i.e. 2.5mgand20mg, respectively. Also, dissolution of Td from Td/PVP-VA delivered in different forms occurred in the following order: powders>tablets>capsules. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction of herbicides in peanuts.

    Science.gov (United States)

    Li, Na; Wang, Zhibing; Zhang, Liyuan; Nian, Li; Lei, Lei; Yang, Xiao; Zhang, Hanqi; Yu, Aimin

    2014-10-01

    Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction was developed and applied to the extraction of pesticides in high fatty matrices. The herbicides were ultrasonically extracted from peanut using ethyl acetate as extraction solvent. The separation of the analytes from a large amount of co-extractive fat was achieved by dispersive solid-phase extraction using MIL-101(Cr) as sorbent. In this step, the analytes were adsorbed on MIL-101(Cr) and the fat remained in bulk. The herbicides were separated and determined by high-performance liquid chromatography. The experimental parameters, including type and volume of extraction solvent, ultrasonication time, volume of hexane and eluting solvent, amount of MIL-101(Cr) and dispersive solid phase extraction time, were optimized. The limits of detection for herbicides range from 0.98 to 1.9 μg/kg. The recoveries of the herbicides are in the range of 89.5-102.7% and relative standard deviations are equal or lower than 7.0%. The proposed method is simple, effective and suitable for treatment of the samples containing high content of fat. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. 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.

  15. Pigment dispersion syndrome associated with intraocular lens implantation: a new surgical technique

    Directory of Open Access Journals (Sweden)

    M Isabel Canut Jordana

    2010-11-01

    Full Text Available M Isabel Canut Jordana1, Daniel Pérez Formigó1, Rodrigo Abreu González2, Jeroni Nadal Reus11Barraquer Ophthalmology Centre, Barcelona, Spain; 2University Hospital of La Candelaria, Tenerife, SpainAims: We report the case of a myopic patient who, after intraocular lens transplant in the posterior chamber, suffered elevated intraocular pressure due to pigment dispersion, with recurrent episodes of blurred vision. The patient was treated with a new surgical technique that can avoid potential iridolenticular contact.Methods: Complete ophthalmologic examination and optical coherence tomography (OCT of the anterior segment were performed.Results: Contact between the pigmentary epithelium and the iris with an intraocular lens was revealed by utrasound biomicroscopy and OCT. In this case, Nd:YAG laser iridotomy and laser iridoplasty were not effective for iridolenticular separation and control of the pigment dispersion. We propose a new technique: stitches on the surface of the iris to obtain good iridolenticular separation and good intraocular pressure control.Conclusion: Stitches on the iris surface should be considered as optional therapy in pigmentary glaucoma secondary to intraocular lens implantation. This surgical technique can avoid potential iridolenticular contacts more definitively.Keywords: pigmentary glaucoma, intraocular lens, optical coherence tomography, laser

  16. Application of energy-dispersive XRF technique in the hydrometallurgy study of local zircon

    International Nuclear Information System (INIS)

    Meor Yusoff Sulaiman; Kamaruddin Hussin; Azizan Aziz

    1996-01-01

    In this study, energy-dispersive X-ray Fluorescence (EDXR-F) was used to analyse the elemental composition of the starting zircon mineral associated elements in the leaching solution. Besides analysing the major elements i.e. of zirconium, silicon and hafnium, trace elemental analysis for iron, titanium and the naturally occurring radioactive element thorium and uranium are important in establishing the grades of Malaysian zircon. The technique was also used in determine the optimum conditions for zirconium and hafnium recovery during the leaching process

  17. 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.

  18. 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.

  19. Time-resolved shock compression of porous rutile: Wave dispersion in porous solids

    Energy Technology Data Exchange (ETDEWEB)

    Anderson, M.U.; Graham, R.A.; Holman, G.T.

    1993-08-01

    Rutile (TiO{sub 2}) samples at 60% of solid density have been shock-loaded from 0.21 to 6.1 GPa with sample thickness of 4 mm and studied with the PVDF piezoelectric polymer stress-rate gauge. The technique uses a copper capsule to contain the sample which has PVDF gauge packages in direct contact with front and rear surfaces. A precise measure is made of the compressive stress wave velocity through the sample, as well as the input and propagated shock stress. Initial density is known from sample preparation, and the amount of shock-compression is calculated from the measurement of shock velocity and input stress. Shock states and re-shock states are measured. Observed data are consistent with previously published high pressure data. It is observed that rutile has a ``crush strength`` near 6 GPa. Propagated stress-pulse rise times vary from 234 to 916 nsec. Propagated stress-pulse rise times of shock-compressed HMX, 2Al + Fe{sub 2}O{sub 3}, 3Ni + Al, and 5Ti + 3Si are presented.

  20. Chemical reaction on solid surface observed through isotope tracer technique

    International Nuclear Information System (INIS)

    Tanaka, Ken-ichi

    1983-01-01

    In order to know the role of atoms and ions on solid surfaces as the partners participating in elementary processes, the literatures related to the isomerization and hydrogen exchanging reaction of olefines, the hydrogenation of olefines, the metathesis reaction and homologation of olefines based on solid catalysts were reviewed. Various olefines, of which the hydrogen atoms were substituted with deuterium at desired positions, were reacted using various solid catalysts such as ZnO, K 2 CO 3 on C, MoS 2 (single crystal and powder) and molybdenum oxide (with various carriers), and the infra-red spectra of adsorbed olefines on catalysts, the isotope composition of reaction products and the production rate of the reaction products were measured. From the results, the bonding mode of reactant with the atoms and ions on solid surfaces, and the mechanism of the elementary process were considered. The author emphasized that the mechanism of the chemical reaction on solid surfaces and the role of active points or catalysts can be made clear to the considerable extent by combining isotopes suitably. (Yoshitake, I.)

  1. 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.

  2. Refractive index dispersion of swift heavy ion irradiated BFO thin films using Surface Plasmon Resonance technique

    Science.gov (United States)

    Paliwal, Ayushi; Sharma, Savita; Tomar, Monika; Singh, Fouran; Gupta, Vinay

    2016-07-01

    Swift heavy ion irradiation (SHI) is an effective technique to induce defects for possible modifications in the material properties. There is growing interest in studying the optical properties of multiferroic BiFeO3 (BFO) thin films for optoelectronic applications. In the present work, BFO thin films were prepared by sol-gel spin coating technique and were irradiated using the 15 UD Pelletron accelerator with 100 MeV Au9+ ions at a fluence of 1 × 1012 ions cm-2. The as-grown films became rough and porous on ion irradiation. Surface Plasmon Resonance (SPR) technique has been identified as a highly sensitive and powerful technique for studying the optical properties of a dielectric material. Optical properties of BFO thin films, before and after irradiation were studied using SPR technique in Otto configuration. Refractive index is found to be decreasing from 2.27 to 2.14 on ion irradiation at a wavelength of 633 nm. Refractive index dispersion of BFO thin film (from 405 nm to 633 nm) before and after ion radiation was examined.

  3. Preparation and pharmacokinetic evaluation of curcumin solid dispersion using Solutol® HS15 as a carrier.

    Science.gov (United States)

    Seo, Sang-Wan; Han, Hyo-Kyung; Chun, Myung-Kwan; Choi, Hoo-Kyun

    2012-03-15

    Solubility of curcumin at physiological pH was significantly increased by forming solid dispersion (SD) with Solutol® HS15. Since curcumin undergoes hydrolytic degradation, chemical stability study was conducted in pH 1.2, 6.8 and 7.4 buffer media. Solutol® HS15 exhibited superior stabilizing effect to Cremophor® RH40 and Kollidon® 30. The physical state of the dispersed curcumin in the polymer matrix was characterized by differential scanning calorimetry and X-ray diffraction studies. SD preparation transformed curcumin into amorphous form and facilitated micellar incorporation, thereby preventing hydrolysis in aqueous medium. In vitro drug release in pH 6.8 buffer revealed that SD (1:10) improved the dissolution of curcumin with approximately 90% release of the drug within 1h. Pharmacokinetic study of the solid dispersion formulation in rat showed that bioavailability of the drug was significantly improved as compared to pure curcumin. SD containing 1:10 ratio of drug and Solutol® HS15 resulted in approximately 5 fold higher AUC(0-12h). SD formulation was physically stable over the study period of 3 months. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. Magnetic matrix solid phase dispersion assisted dispersive liquid liquid microextraction of ultra trace polychlorinated biphenyls in water prior to GC-ECD determination

    International Nuclear Information System (INIS)

    Diao, Chunpeng; Li, Cong; Yang, Xiao; Sun, Ailing; Liu, Renmin

    2016-01-01

    Magnetic matrix solid phase dispersion (MMSPD) assisted dispersive liquid liquid microextraction (DLLME) was applied to extract ultra traces of polychlorinated biphenyls (PCBs) from water samples prior to gas chromatography with electron capture detection. PCBs in water were adsorbed by micro particles of magnetic bamboo charcoal and then transferred into the elution solvent. PCBs in the elution solvent of the MMSPD were further concentrated into trace volume extraction solvent of the DLLME procedure. Under optimized conditions, good linearity in the range of 0.2–100 ng L"−"1 was obtained with regression coefficients (r) higher than 0.9987. Based on a signal-noise ratio of 3, the limits of detection (LODs) range from 0.05–0.1 ng L"−"1. These LODs are much lower than those of MMSPD or DLLME alone. Relative standard deviations are between 4.9–8.2 %. The method was successfully applied to the determination of PCBs in lake and river water. Relative recoveries were 85.5–117.4 % for the spiked environmental water samples. (author)

  5. Crosslinked hydrogels—a promising class of insoluble solid molecular dispersion carriers for enhancing the delivery of poorly soluble drugs

    Directory of Open Access Journals (Sweden)

    Dajun D. Sun

    2014-02-01

    Full Text Available Water-insoluble materials containing amorphous solid dispersions (ASD are an emerging category of drug carriers which can effectively improve dissolution kinetics and kinetic solubility of poorly soluble drugs. ASDs based on water-insoluble crosslinked hydrogels have unique features in contrast to those based on conventional water-soluble and water-insoluble carriers. For example, solid molecular dispersions of poorly soluble drugs in poly(2-hydroxyethyl methacrylate (PHEMA can maintain a high level of supersaturation over a prolonged period of time via a feedback-controlled diffusion mechanism thus avoiding the initial surge of supersaturation followed by a sharp decline in drug concentration typically encountered with ASDs based on water-soluble polymers. The creation of both immediate- and controlled-release ASD dosage forms is also achievable with the PHEMA based hydrogels. So far, ASD systems based on glassy PHEMA have been shown to be very effective in retarding precipitation of amorphous drugs in the solid state to achieve a robust physical stability. This review summarizes recent research efforts in investigating the potential of developing crosslinked PHEMA hydrogels as a promising alternative to conventional water-soluble ASD carriers, and a related finding that the rate of supersaturation generation does affect the kinetic solubility profiles implications to hydrogel based ASDs.

  6. Crosslinked hydrogels-a promising class of insoluble solid molecular dispersion carriers for enhancing the delivery of poorly soluble drugs.

    Science.gov (United States)

    Sun, Dajun D; Lee, Ping I

    2014-02-01

    Water-insoluble materials containing amorphous solid dispersions (ASD) are an emerging category of drug carriers which can effectively improve dissolution kinetics and kinetic solubility of poorly soluble drugs. ASDs based on water-insoluble crosslinked hydrogels have unique features in contrast to those based on conventional water-soluble and water-insoluble carriers. For example, solid molecular dispersions of poorly soluble drugs in poly(2-hydroxyethyl methacrylate) (PHEMA) can maintain a high level of supersaturation over a prolonged period of time via a feedback-controlled diffusion mechanism thus avoiding the initial surge of supersaturation followed by a sharp decline in drug concentration typically encountered with ASDs based on water-soluble polymers. The creation of both immediate- and controlled-release ASD dosage forms is also achievable with the PHEMA based hydrogels. So far, ASD systems based on glassy PHEMA have been shown to be very effective in retarding precipitation of amorphous drugs in the solid state to achieve a robust physical stability. This review summarizes recent research efforts in investigating the potential of developing crosslinked PHEMA hydrogels as a promising alternative to conventional water-soluble ASD carriers, and a related finding that the rate of supersaturation generation does affect the kinetic solubility profiles implications to hydrogel based ASDs.

  7. Optical techniques for solid-state materials characterization

    CERN Document Server

    Prasankumar, Rohit P

    2016-01-01

    This book has comprehensively covered the essential optical approaches needed for solid-state materials characterization. Written by experts in the field, this will be a great reference for students, engineers, and scientists.-Professor Yoke Khin Yap, Michigan Technical University.

  8. All-solid-state flexible supercapacitors based on highly dispersed polypyrrole nanowire and reduced graphene oxide composites.

    Science.gov (United States)

    Yu, Chenfei; Ma, Peipei; Zhou, Xi; Wang, Anqi; Qian, Tao; Wu, Shishan; Chen, Qiang

    2014-10-22

    Highly dispersed polypyrrole nanowires are decorated on reduced graphene oxide sheets using a facile in situ synthesis route. The prepared composites exhibit high dispersibility, large effective surface area, and high electric conductivity. All-solid-state flexible supercapacitors are assembled based on the prepared composites, which show excellent electrochemical performances with a specific capacitance of 434.7 F g(-1) at a current density of 1 A g(-1). The as-fabricated supercapacitor also exhibits excellent cycling stability (88.1% capacitance retention after 5000 cycles) and exceptional mechanical flexibility. In addition, outstanding power and energy densities were obtained, demonstrating the significant potential of prepared material for flexible and portable energy storage devices.

  9. Measurement of liquid holdup and axial dispersion in trickle bed reactors using radiotracer technique

    International Nuclear Information System (INIS)

    Pant, H.J.; Saroha, A.K.; Nikam, K.D.P.

    2000-01-01

    The holdup and axial dispersion of aqueous phase has been measured in trickle bed reactors as a function of liquid and gas flow rates using radioisotope tracer technique. Experiments were carried out in the glass column of inner diameter of 15.2x10 -2 m column for air-water system using three different types of packings i.e. non-porous glass beads, porous catalyst of tablet and extrudate shape. The range of liquid and gas flow rates used were 8.3x10 -5 - 3.3x1- -4 m 3 /s and 0 - 6.67x10 -4 m 3 /s, respectively. Residence time distributions of liquid phase and gas phase were measured and mean residence times were determined. The values of liquid holdup were calculated from the measured mean residence times. It was observed that the liquid holdup increases with increase in liquid flow rates and was independent of increase in gas flow rates used in the study. Two-parameter axial dispersion model was used to simulate measured residence time distribution data and values of mean residence time and Peclet number were obtained. It was observed that the values of Peclet number increases with increase in liquid flow rate for glass beads and tablets and remains almost constant for extrudates. The values of mean residence time obtained from model simulation were found to be in good agreement with the values measured experimentally. (author)

  10. A new analysis technique to measure fusion excitation functions with large beam energy dispersions

    Science.gov (United States)

    Figuera, P.; Di Pietro, A.; Fisichella, M.; Lattuada, M.; Shotter, A. C.; Ruiz, C.; Zadro, M.

    2018-01-01

    Peculiar nuclear structures of two colliding nuclei such has clustering, neutron halo/skin or very low breakup thresholds can affect the reaction dynamics below the Coulomb barrier and this may also have astrophysical consequences. In order to have a better understanding of this topic, in the last decade, several experiments were performed. A typical experimental challenge of such studies is the need to measure excitation functions below the Coulomb barrier, having a strong energy dependence, with rather large beam energy dispersions inside the target. This may easily lead to ambiguities in associating the measured cross section with a proper beam energy. In this paper a discussion on this topic is reported and a new technique to deal with the above problem will be proposed.

  11. Laser--Doppler anemometry technique applied to two-phase dispersed flows in a rectangular channel

    International Nuclear Information System (INIS)

    Lee, S.L.; Srinivasan, J.

    1979-01-01

    A new optical technique using Laser--Doppler anemometry has been applied to the local measurement of turbulent upward flow of a dilute water droplet--air two-phase dispersion in a vertical rectangular channel. Individually examined were over 20,000 droplet signals coming from each of a total of ten transversely placed measuring points, the closest of which to the channel wall was 250 μ away from the wall. Two flows of different patterns due to different imposed flow conditions were investigated, one with and the other without a liquid film formed on the channel wall. Reported are the size and number density distribution and the axial and lateral velocity distributions for the droplets as well as the axial and lateral velocity distributions for the air

  12. Accuracy and Uncertainty Analysis of Intelligent Techniques for Predicting the Longitudinal Dispersion Coefficient in Rivers

    Directory of Open Access Journals (Sweden)

    Abbas Akbarzadeh

    2010-09-01

    Full Text Available Accurate prediction of longitudinal dispersion coefficient (LDC can be useful for the determination of pollutants concentration distribution in natural rivers. However, the uncertainty associated with the results obtained from forecasting models has a negative effect on pollutant management in water resources. In this research, appropriate models are first developed using ANN and ANFIS techniques to predict the LDC in natural streams. Then, an uncertainty analysis is performed for ANN and ANFIS models based on Monte-Carlo simulation. The input parameters of the models are related to hydraulic variables and stream geometry. Results indicate that ANN is a suitable model for predicting the LDC, but it is also associated with a high level of uncertainty. However, results of uncertainty analysis show that ANFIS model has less uncertainty; i.e. it is the best model for forecasting satisfactorily the LDC in natural streams.

  13. Novel all-optical dispersion monitoring technique for ultra-high-speed WDM networks

    Energy Technology Data Exchange (ETDEWEB)

    Cui Sheng; Li Li; Liu Deming, E-mail: cuisheng@mail.hust.edu.cn [Wuhan National Laboratory for Optoelectronics, No.1037, Luoyu Road, Wuhan, Hubei, 430074 (China)

    2011-02-01

    This paper represents a novel all-optical dispersion monitoring technique based on fiber parametric amplifiers (FOPAs). The monitoring method is truly bit-rate transparent because it is enabled by the exponential power transfer function (PTF) provided by the FOPA gain. The slope of the PTF is increased from 2 to 3 by choosing appropriate phase-matching conditions. Due to the steeper PTF the monitoring sensitivity is greatly improved compared to the other PTF-based methods proposed before. The PTF obtained by numerical simulations agrees very well with the experimental results. Numerical simulations are then used to demonstrate that our method can be used to monitor signals in various modulation formats.

  14. Application of energy dispersive x-ray techniques for water analysis

    International Nuclear Information System (INIS)

    Funtua, I. I.

    2000-07-01

    Energy dispersive x-ray fluorescence (EDXRF) is a class of emission spectroscopic techniques that depends upon the emission of characteristic x-rays following excitation of the atomic electron energy levels by tube or isotopic source x-rays. The technique has found wide range of applications that include determination of chemical elements of water and water pollutants. Three EDXRF systems, the isotopic source, secondary target and total reflection (TXRF) are available at the Centre for Energy research and Training. These systems have been applied for the analysis of sediments, suspensions, ground water, river and rainwater. The isotopic source is based on 55 Fe, 109 Cd and 241 Am excitations while the secondary target and the total reflection are utilizing a Mo x-ray tube. Sample preparation requirements for water analysis range from physical and chemical pre-concentration steps to direct analysis and elements from Al to U can be determined with these systems. The EDXRF techniques, TXRF in particular with its multielement capability, low detection limit and possibility of direct analysis for water have competitive edge over the traditional methods of atomic absorption and flame photometry

  15. Degree of dispersion monitoring by ultrasonic transmission technique and excitation of the transducer's harmonics

    Science.gov (United States)

    Schober, G.; Heidemeyer, P.; Kretschmer, K.; Bastian, M.; Hochrein, T.

    2014-05-01

    The degree of dispersion of filled polymer compounds is an important quality parameter for various applications. For instance, there is an influence on the chroma in pigment colored plastics or on the mechanical properties of filled or reinforced compounds. Most of the commonly used offline methods are work-intensive and time-consuming. Moreover, they do not allow an all-over process monitoring. In contrast, the ultrasonic technique represents a suitable robust and process-capable inline method. Here, we present inline ultrasonic measurements on polymer melts with a fundamental frequency of 1 MHz during compounding. In order to extend the frequency range we additionally excite the fundamental and the odd harmonics vibrations at 3 and 5 MHz. The measurements were carried out on a compound consisting of polypropylene and calcium carbonate. For the simulation of agglomerates calcium carbonate with a larger particle size was added with various rates. The total filler content was kept constant. The frequency selective analysis shows a linear correlation between the normalized extinction and the rate of agglomerates simulated by the coarser filler. Further experiments with different types of glass beads with a well-defined particle size verify these results. A clear correlation between the normalized extinction and the glass bead size as well as a higher damping with increasing frequency corresponds to the theoretical assumption. In summary the dispersion quality can be monitored inline by the ultrasonic technique. The excitation of the ultrasonic transducer's harmonics generates more information about the material as the usage of the pure harmonic vibration.

  16. 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%.

  17. Anomalous dissolution behaviour of tablets prepared from sugar glass-based solid dispersions

    NARCIS (Netherlands)

    Van Drooge, D.J.; Hinrichs, W.L.J.; Frijlink, H.W.

    2004-01-01

    In this study, anomalous dissolution behaviour of tablets consisting of sugar glass dispersions was investigated. The poorly aqueous soluble diazepam was used as a lipophilic model drug. The release of diazepam and sugar carrier was determined to study the mechanisms governing dissolution behaviour.

  18. A Comparative Study of Dispersion Characteristics Determination of a Trapezoidally Corrugated Slow Wave Structure Using Different Techniques

    International Nuclear Information System (INIS)

    Saber, Md. Ghulam; Sagor, Rakibul Hasan; Amin, Md. Ruhul

    2016-01-01

    The linear dispersion relation of a trapezoidally corrugated slow wave structure (TCSWS) is analyzed and presented. The size parameters of the TCSWS are chosen in such a way that they operate in the x-band frequency range. The dispersion relation is solved by utilizing the Rayleigh–Fourier method by expressing the radial function in terms of the Fourier series. A highly accurate synthetic technique is also applied to determine the complete dispersion characteristics from experimentally measured resonances (cold test). Periodic structures resonate at specific frequencies when the terminals are shorted appropriately. The dispersion characteristics obtained from numerical calculation, synthetic technique and cold test are compared, and an excellent agreement is achieved. (paper)

  19. New Solid Phases for Estimation of Hormones by Radioimmunoassay Technique

    International Nuclear Information System (INIS)

    Sheha, R.R.; Ayoub, H.S.M.; Shafik, M.

    2013-01-01

    The efforts in this study were initiated to develop and validate new solid phases for estimation of hormones by radioimmunoassay (RIA). The study argued the successful application of different hydroxy apatites (HAP) as new solid phases for estimation of Alpha fetoprotein (AFP), Thyroid Stimulating hormone (TSH) and Luteinizing hormone (LH) in human serum. Hydroxy apatites have different alkali earth elements were successfully prepared by a well-controlled co-precipitation method with stoichiometric ratio value 1.67. The synthesized barium and calcium hydroxy apatites were characterized using XRD and Ftir and data clarified the preparation of pure structures of both BaHAP and CaHAP with no evidence on presence of other additional phases. The prepared solid phases were applied in various radioimmunoassay systems for separation of bound and free antigens of AFP, TSH and LH hormones. The preparation of radiolabeled tracer for these antigens was carried out using chloramine-T as oxidizing agent. The influence of different parameters on the activation and coupling of the used apatite particles with the polyclonal antibodies was systematically investigated and the optimum conditions were determined. The assay was reproducible, specific and sensitive enough for regular estimation of the studied hormones. The intra-and inter-assay variation were satisfactory and also the recovery and dilution tests indicated an accurate calibration. The reliability of these apatite particles had been validated by comparing the results that obtained by using commercial kits. The results finally authenticates that hydroxyapatite particles would have a great potential to address the emerging challenge of accurate quantitation in laboratory medical application

  20. Fast dissolving cyclodextrin complex of piroxicam in solid dispersion part I: influence of β-CD and HPβ-CD on the dissolution rate of piroxicam.

    Science.gov (United States)

    Bouchal, F; Skiba, M; Chaffai, N; Hallouard, F; Fatmi, S; Lahiani-Skiba, M

    2015-01-30

    Sublingual drug delivery is an interesting route for drug having significant hepatic first-pass metabolism or requiring rapid pharmacological effect as for patients suffering from swallowing difficulties, nausea or vomiting. Sublingual absorption could however be limited by the kinetic of drug dissolution. This study evaluated influences of cyclodextrins (β-CD or HP-β-CD) and their different inclusion process (spray-drying or freeze-drying) on the drug dissolution kinetic of solid dispersions in poly(ethylene glycol) (PEG, Mw 6000Da) of piroxicam, used as poor hydrosoluble drug model. A secondary objective was to determine influences of drug dispersion process in PEG (evaporation or melting methods) on the drug dissolution kinetic of piroxicam. Piroxicam solid dispersions containing or not cyclodextrins were characterized by different scanning calorimetry (DSC), Thermogravometry analyser (TGA) and Fourier transform-infrared spectroscopy (FT-IR) spectroscopy. In vitro drug dissolution study of these solid dispersions was then performed. The results demonstrated the high potential and interest of solid dispersions of drug previously included in cyclodextrins for sublingual delivery of hydrophobic drugs. This study also showed the advantages of evaporation method on the melting ones during drug dispersion in PEG. Indeed, drug complexation with cyclodextrins as dispersion by melting prevented the presence in solid dispersions of drug in crystalline form which can represent up to 63%. Moreover, dispersion in PEG by evaporation method gave more porous drug delivery system than with melting methods. This allowed complete (limited at most at 80-90% with melting methods) and quick drug dissolution without rebound effect like with melting ones. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Solid lubricants and surfaces

    CERN Document Server

    Braithwaite, E R

    1964-01-01

    Solid Lubricants and Surfaces deals with the theory and use of solid lubricants, particularly in colloidal form. Portions of this book are devoted to graphite and molybdenum disulfides, which are widely used solid lubricants in colloidal form. An extensive literature on the laboratory examination of hundreds of solids as potential lubricants is also provided in this text. Other topics discussed include the metals and solid lubricants; techniques for examining surfaces; other solid lubricants; metal shaping; and industrial uses of solid-lubricant dispersions. This publication is beneficial to e

  2. Characterization, in Vivo and in Vitro Evaluation of Solid Dispersion of Curcumin Containing d-α-Tocopheryl Polyethylene Glycol 1000 Succinate and Mannitol

    Directory of Open Access Journals (Sweden)

    Im-Sook Song

    2016-10-01

    Full Text Available The aim of this study was to prepare a solid dispersion formulation of curcumin to enhance its solubility, dissolution rate, and oral bioavailability. The formulation was prepared with d-α-tocopheryl polyethylene glycol 1000 succinate (TPGS and mannitol using solvent evaporation and freeze-drying methods, which yielded a solid dispersion composed of curcumin, TPGS, and mannitol at a ratio of 1:10:15 (w/w/w. The solubility and dissolution rate of the curcumin solid dispersion markedly improved compared with those of curcumin powder and a physical mixture of curcumin, TPGS, and mannitol. About 90% of the curcumin was released from the solid dispersion formulation within 10 min. After administering the formulation orally to rats, higher plasma concentrations of curcumin were observed, with increases in the maximum plasma concentration (Cmax and area under the plasma concentration-time curve (AUC of 86- and 65-fold, respectively, compared with those of curcumin powder. The solid dispersion formulation effectively increased intestinal permeability and inhibited P-gp function. These effects increased the anti-proliferative effect of curcumin in MDA-MB-231 breast cancer cells. Moreover, 2 h incubation with curcumin powder, solid dispersion formulation, and its physical mixture resulted in differential cytotoxic effect of paclitaxel in P-gp overexpressed LLC-PK1-P-gp and MDA-MB-231 cells through the inhibition of P-gp-mediated paclitaxel efflux. In conclusion, compared with curcumin, a solid dispersion formulation of curcumin with TPGS and mannitol could be a promising option for enhancing the oral bioavailability and efficacy of curcumin through increased solubility, dissolution rate, cell permeability, and P-gp modulation.

  3. Characterization, in Vivo and in Vitro Evaluation of Solid Dispersion of Curcumin Containing d-α-Tocopheryl Polyethylene Glycol 1000 Succinate and Mannitol.

    Science.gov (United States)

    Song, Im-Sook; Cha, Jin-Sun; Choi, Min-Koo

    2016-10-17

    The aim of this study was to prepare a solid dispersion formulation of curcumin to enhance its solubility, dissolution rate, and oral bioavailability. The formulation was prepared with d-α-tocopheryl polyethylene glycol 1000 succinate (TPGS) and mannitol using solvent evaporation and freeze-drying methods, which yielded a solid dispersion composed of curcumin, TPGS, and mannitol at a ratio of 1:10:15 ( w / w / w ). The solubility and dissolution rate of the curcumin solid dispersion markedly improved compared with those of curcumin powder and a physical mixture of curcumin, TPGS, and mannitol. About 90% of the curcumin was released from the solid dispersion formulation within 10 min. After administering the formulation orally to rats, higher plasma concentrations of curcumin were observed, with increases in the maximum plasma concentration (C max ) and area under the plasma concentration-time curve (AUC) of 86- and 65-fold, respectively, compared with those of curcumin powder. The solid dispersion formulation effectively increased intestinal permeability and inhibited P-gp function. These effects increased the anti-proliferative effect of curcumin in MDA-MB-231 breast cancer cells. Moreover, 2 h incubation with curcumin powder, solid dispersion formulation, and its physical mixture resulted in differential cytotoxic effect of paclitaxel in P-gp overexpressed LLC-PK1-P-gp and MDA-MB-231 cells through the inhibition of P-gp-mediated paclitaxel efflux. In conclusion, compared with curcumin, a solid dispersion formulation of curcumin with TPGS and mannitol could be a promising option for enhancing the oral bioavailability and efficacy of curcumin through increased solubility, dissolution rate, cell permeability, and P-gp modulation.

  4. Enhanced dissolution and bioavailability of biochanin A via the preparation of solid dispersion: in vitro and in vivo evaluation.

    Science.gov (United States)

    Han, Hyo-Kyung; Lee, Beom-Jin; Lee, Hyoung-Kyu

    2011-08-30

    The present study aimed to improve the bioavailability of biochanin A, a poorly soluble bioflavonoid, via the preparation of solid dispersion (SD) using Solutol HS15 and HPMC 2910. Solubility of biochanin A was enhanced by 8-60 folds as the drug-carrier ratio was increased in SDs. Furthermore, compared to pure biochanin A or physical mixture (PM), SDs significantly improved the dissolution rate and the extent of drug release. Particularly, SDs (Drug:Solutol HS15:HPMC 2910=1:5:5 or 1:10:10) achieved the rapid and complete drug release (approximately 100% within 1h) at pH 6.8. The XRD patterns indicated that SDs might enhance the solubility of biochanin A by changing the drug crystallinity to amorphous state in addition to the solubilizing effect of hydrophilic carriers. The improved dissolution of biochanin A via SD formulation appeared to be well correlated with the enhanced oral exposure of biochanin A in rats. After an oral administration of SD (Drug:Solutol HS15:HPMC 2910=1:10:10), C(max) and AUC of biochanin A were increased by approximately 13 and 5 folds, respectively, implying that SDs could be effective to improve the bioavailability of biochanin A. In conclusion, solid dispersion with Solutol HS15 and HPMC 2910 appeared to be promising to improve the dissolution and oral exposure of biochanin A. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. Transport of temperature-velocity covariance in gas-solid flow and its relation to the axial dispersion coefficient

    Science.gov (United States)

    Subramaniam, Shankar; Sun, Bo

    2015-11-01

    The presence of solid particles in a steady laminar flow generates velocity fluctuations with respect to the mean fluid velocity that are termed pseudo-turbulence. The level of these pseudo-turbulent velocity fluctuations has been characterized in statistically homogeneous fixed particle assemblies and freely evolving suspensions using particle-resolved direct numerical simulation (PR-DNS) by Mehrabadi et al. (JFM, 2015), and it is found to be a significant contribution to the total kinetic energy associated with the flow. The correlation of these velocity fluctuations with temperature (or a passive scalar) generates a flux term that appears in the transport equation for the average fluid temperature (or average scalar concentration). The magnitude of this transport of temperature-velocity covariance is quantified using PR-DNS of thermally fully developed flow past a statistically homogeneous fixed assembly of particles, and the budget of the average fluid temperature equation is presented. The relation of this transport term to the axial dispersion coefficient (Brenner, Phil. Trans. Roy. Soc. A, 1980) is established. The simulation results are then interpreted in the context of our understanding of axial dispersion in gas-solid flow. NSF CBET 1336941.

  6. Enhancement of Solubility of Lamotrigine by Solid Dispersion and Development of Orally Disintegrating Tablets Using 32 Full Factorial Design

    Directory of Open Access Journals (Sweden)

    Jatinderpal Singh

    2015-01-01

    Full Text Available Present investigation deals with the preparation and evaluation of orally disintegrating tablets (ODTs of lamotrigine using β-cyclodextrin and PVP-K30 as polymers for the preparation of solid dispersion which help in enhancement of aqueous solubility of this BCS CLASS-II drug and sodium starch glycolate (SSG and crospovidone as a superdisintegrating agent, to reduce disintegration time. The ODTs were prepared by direct compression method. Nine formulations were developed with different ratios of superdisintegrating agents. All the formulations were evaluated for disintegration time, weight variation, hardness, friability, drug content uniformity, wetting time, and in vitro drug release study. In vitro drug release study was performed using United States Pharmacopoeia (USP type 2 dissolution test apparatus employing paddle stirrer at 50 rpm using 900 mL of 0.1 N HCl maintained at 37°C ± 0.5°C as the dissolution medium. On the basis of evaluation parameters formulations were prepared using β-CD 1 : 1 solid dispersion. Then 32 full factorial design was applied using SSG and crospovidone in different ratios suggested by using design expert 8.0.7.1 and optimized formulation was prepared using amount of SSG and crospovidone as suggested by the software. The optimized formulation prepared had disintegrating time of 15 s, wetting time of 24 s, and % friability of 0.55.

  7. Application of dispersion and dose assessment models to the solid and liquid wastes facilities of Ezeiza radioactive waste management area

    International Nuclear Information System (INIS)

    Amado, Valeria A.; Lopez, Fabio O.

    2007-01-01

    This paper provides a dose assessment of the critic group from the near surface facility for solid and liquid waste, located at Ezeiza Atomic Center in Argentina (Ezeiza Radioactive Waste Management Area-AGE). The calculations were made using several approaches about source term. The activities for each radionuclide and facility were taken from the National Atomic Energy Commission's Inventory that corresponds to the first trimester of 2005. The radioactive decay of each radionuclide was considered. The work was performed in two steps. In the first step, using the Nuclide Dispersion in Phreatic Aquifer Model (DRAF), the dispersion of the contaminants into the phreatic aquifer until the discharge point at a superficial water course was considered. In the second step, the Consequences of Releases to the Environment Assessment Methodology Program (PC CREAM) was used for the study of radionuclides dispersion in superficial water course and dose calculations. The results from this paper show that, for every studied radionuclide, the doses involved are significantly lower than the values established by current regulations. On the other hand, those results put in evidence the utility of simple models in estimating the order of magnitude of expected concentrations and doses. It is important to highlight that the obtained results can be used only in the context of the suppositions that were made. (author) [es

  8. 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...

  9. N-isopropylacrylamide-based fine-dispersed thermosensitive ferrogels obtained via in-situ technique.

    Science.gov (United States)

    Korotych, O; Samchenko, Yu; Boldeskul, I; Ulberg, Z; Zholobak, N; Sukhodub, L

    2013-03-01

    Thermosensitive hydrogels with magnetic properties (ferrogels) are very promising for medical application, first of all, for the design of targeted delivery systems with controlled release of drugs and for magnetic hyperthermia and chemotherapy treatment of cancer. These magnetic hydrogels could be obtained using diverse techniques: ex- and in-situ syntheses. The present work is devoted to the study of magnetite (Fe(3)O(4)) formation inside the nanoreactors of (co)polymeric hydrogels. Polymeric templates (hydrogel films and fine-dispersed hydrogels) used for obtaining ferrogels were based on acrylic monomers: thermosensitive N-isopropylacrylamide, and hydrophilic acrylamide. Covalent cross-linking was accomplished using bifunctional monomer N,N'-methylenebisacrylamide. Influence of hydrophilic-lipophilic balance of polymeric templates and concentration of iron cations on the magnetite formation were investigated along with the development of ferrogel preparation technique. Cytotoxicity, physical and chemical properties of obtained magnetic hydrogels have been studied in this work. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. 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

  11. Solid dispersions, part I: recent evolutions and future opportunities in manufacturing methods for dissolution rate enhancement of poorly water-soluble drugs.

    Science.gov (United States)

    Bikiaris, Dimitrios N

    2011-11-01

    In recent years, the number of active pharmaceutical ingredients with high therapeutic impact, but very low water solubility, has increased significantly. Thus, a great challenge for pharmaceutical technology is to create new formulations and efficient drug-delivery systems to overcome these dissolution problems. Drug formulation in solid dispersions (SDs) is one of the most commonly used techniques for the dissolution rate enhancement of poorly water-soluble drugs. Generally, SDs can be defined as a dispersion of active ingredients in molecular, amorphous and/or microcrystalline forms into an inert carrier. This review covers literature which states that the dissolution enhancement of SDs is based on the fact that drugs in the nanoscale range, or in amorphous phase, dissolve faster and to a greater extent than micronized drug particles. This is in accordance to the Noyes-Whitney equation, while the wetting properties of the used polymer may also play an important role. The main factors why SD-based pharmaceutical products on the market are steadily increasing over the last few years are: the recent progress in various methods used for the preparation of SDs, the effect of evolved interactions in physical state of the drug and formulation stability during storage, the characterization of the physical state of the drug and the mechanism of dissolution rate enhancement.

  12. 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.

  13. Amorphous solid dispersions of piroxicam and Soluplus(®): Qualitative and quantitative analysis of piroxicam recrystallization during storage.

    Science.gov (United States)

    Lust, Andres; Strachan, Clare J; Veski, Peep; Aaltonen, Jaakko; Heinämäki, Jyrki; Yliruusi, Jouko; Kogermann, Karin

    2015-01-01

    The conversion of active pharmaceutical ingredient (API) from amorphous to crystalline form is the primary stability issue in formulating amorphous solid dispersions (SDs). The aim of the present study was to carry out qualitative and quantitative analysis of the physical solid-state stability of the SDs of poorly water-soluble piroxicam (PRX) and polyvinyl caprolactam-polyvinyl acetate-polyethylene-glycol graft copolymer (Soluplus(®)). The SDs were prepared by a solvent evaporation method and stored for six months at 0% RH/6 °C, 0% RH/25 °C, 40% RH/25 °C and 75% RH/25 °C. Fourier transform infrared spectroscopy equipped with attenuated total reflection accessory (ATR-FTIR) and Raman spectroscopy were used for characterizing the physical solid-state changes and drug-polymer interactions. The principal component analysis (PCA) and multivariate curve resolution alternating least squares (MCR-ALS) were used for the qualitative and quantitative analysis of Raman spectra collected during storage. When stored at 0% RH/6 °C and at 0% RH/25 °C, PRX in SDs remained in an amorphous form since no recrystallization was observed by ATR-FTIR and Raman spectroscopy. Raman spectroscopy coupled with PCA and MCR-ALS and ATR-FTIR spectroscopy enabled to detect the recrystallization of amorphous PRX in the samples stored at higher humidity. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. A Novel Melt-Dispersion Technique for Simplistic Preparation of Chlorpromazine-Loaded Polycaprolactone Nanocapsules

    Directory of Open Access Journals (Sweden)

    Thiresen Govender

    2015-06-01

    Full Text Available The aim of this study was to design, synthesize and optimize chlorpromazine hydrochloride (CPZ-loaded, poly-ε-caprolactone (PCL based nanocapsules, intended for site specific delivery to the frontal lobe, using a novel melt-dispersion technique that is non-arduous, inexpensive and devoid of any hazardous organic solvents. Experimental trials using a central composite design were performed on 13 statistically derived formulations of various combinations of PCL (1000–3000 mg and Polysorbate 80 (2%–5% v/v on the physicochemical and physicomechanical properties and interactive effects on PCL nanocapsule formulation. Differential scanning calorimetry (DSC, Temperature modulated differential scanning calorimetry (TMDSC and Fourier transform infrared spectroscopy (FTIR revealed that there was no thermodegardation of the constituents utilized in the melt dispersion technique. Nanocapsule yields achieved were very high however entrapment of CPZ proved to be relatively low due to the highly hydrophilic nature of CPZ and the processing of the nanocapsules post synthesis. Nanocapsule sizes were in the nanotherapeutic range and varied from 132.7 ± 6.8 nm to 566.6 ± 5.5 nm. Zeta potential ranged from 15.1 ± 0.65 mV to 28.8 ± 0.84 mV revealing capsules that were of incipient to moderate stability. Transmission electron microscopy revealed nanocapsules that were spherical shape, well individualized with a moderate degree of flocculation. In vitro CPZ release was biphasic for all formulations with an initial burst release followed by pseudo-steady controlled release over 30 days. The cytotoxicity of the optimized nanocapsule system on a PC12 neuronal cell line proved to be minimal. Following incorporation of the optimized nanocapsules within a polymeric membrane, in vivo implantation of the device in a New Zealand Albino rabbit model proved the efficacy of the system in achieving prolonged more targeted CPZ levels to the brain. Extensive in vitro

  15. 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.

  16. Characterization and enhanced nonlinear optical limiting response in carbon nanodots dispersed in solid-state hybrid organically modified silica gel glasses

    Science.gov (United States)

    Huang, Li; Zheng, Chan; Guo, Qiaohang; Huang, Dongdong; Wu, Xiukai; Chen, Ling

    2018-02-01

    Freely dispersed carbon nanodots (CNDs) were introduced into a 3-glycidoxy-propyltrimethoxysilane modified silicate gel glass (i.e. an organically modified silica or ORMOSIL) by a highly efficient and simple sol-gel process, which could be easily extended to prepare functional molecules/nanoparticles solid state optoelectronic devices. Scanning electron microscope imaging, Fourier transform infrared spectroscopy, pore structure measurements, ultraviolet-visible spectroscopy, and fluorescence spectroscopy were used to investigate the surface characteristics, structure, texture, and linear optical properties of the CND/SiO2 ORMOSIL gel glasses. Images and UV/Vis spectra confirmed the successful dispersion of CNDs in the ORMOSIL gel glass. The surface characteristics and pore structure of the host SiO2 matrix were markedly changed through the introduction of the CNDs. The linear optical properties of the guest CNDs were also affected by the sol-gel procedure. The nonlinear optical (NLO) properties of the CNDs were investigated by a nanosecond open-aperture Z-scan technique at 532 nm both in liquid and solid matrices. We found that the NLO response of the CNDs was considerably improved after their incorporation into the ORMOSIL gel glasses. Possible enhancement mechanisms were also explored. The nonlinear extinction coefficient gradually increased while the optical limiting (OL) threshold decreased as the CND doping level was increased. This result suggests that the NLO and OL properties of the composite gel glasses can be optimized by tuning the concentration of CNDs in the gel glass matrix. Our findings show that CND/SiO2 ORMOSIL gel glasses are promising candidates for optical limiters to protect sensitive instruments and human eyes from damage caused by high power lasers.

  17. Effective dispersion and crosslinking in PVA/cellulose fiber biocomposites via solid-state mechanochemistry.

    Science.gov (United States)

    Niu, Yan; Zhang, Xiaofang; He, Xu; Zhao, Jiangqi; Zhang, Wei; Lu, Canhui

    2015-01-01

    A mechanochemical approach to improve the dispersion and the degree of crosslinking between cellulose fiber and polymer matrix is presented herein to create high performance poly(vinyl alcohol) (PVA)/cellulose biocomposites in a solvent-free and catalyst-free system. During a pan-milling process, the hydrogen bonds in both cellulose and PVA were effectively broken up, and the released hydroxyl groups could react with succinic anhydride (SA) to form covalent bonds between the two components. This stress-induced chemical reaction was verified by fourier transform infrared spectroscopy. The reaction kinetics was discussed according to the conversion rate of SA during the pan-milling process. Soxhlet extraction with hot water showed that the crosslinked PVA/cellulose retained more PVA in the composites due to the homogeneous and heterogeneous crosslinking. Scanning electron microscope images indicated the dispersion and interfacial interactions between PVA and cellulose were largely improved. The resulting composites exhibited remarkably enhanced mechanical properties. The tensile strength increased from 8.8 MPa (without mechanochemical treatment) to 18.2 MPa, and elongation at break increased from 76.8 to 361.7% after the treatment. Their thermal stability was also significantly improved. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. A survey on multiproperty measurement techniques of solid materials

    International Nuclear Information System (INIS)

    Matsumoto, Tsuyoshi

    1989-01-01

    The term 'multiproperty measurement' has not as yet been widely used. It is defined as the simultaneous (or continuous) measurement of several properties of material using one sample and one set of equipment. It is highly advantageous to measure several properties of a sample simultaneously. Various aspects of the nature of a substance can be clarified by evaluating its nature in terms of many properties. In particular, advanced techniques for measuring thermal properties of material are needed in the fields of atomic energy industry, aerospace industry, energy industry, electronics industry and academic community. Conventional thermal property measurement techniques which can be applied to multiproperty measurement or minute test sample measurement are outlined focusing on measurement of the thermal conductivity (axial flow method, radial flow method, plate method, unsteady state heating coil method, direct current heating method), specific heat (adiabatic method, drop calorimetry, differential scanning calorimetry, AC calorimetric method, pulse heating method, and laser heating method), thermal diffusivity (laser-flash method), and emissivity (separated black body method, incorporated black body method). (N,K.)

  19. 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.

  20. Determination of structure of oriented samples using two-dimensional solid state NMR techniques

    International Nuclear Information System (INIS)

    Jin Hong; Harbison, G.S.

    1990-01-01

    One dimensional and two-dimensional MAS techniques can give detailed information about the structure and dynamics of oriented systems. We describe the application of such techniques to the liquid-crystalline polymer poly(p-phenyleneterphtalimide) (PPTA), and thence deduce the solid-state structure of the material. (author). 9 refs.; 6 figs

  1. 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.

  2. Ion beam induced defects in solids studied by optical techniques

    International Nuclear Information System (INIS)

    Comins, J.D.; Amolo, G.O.; Derry, T.E.; Connell, S.H.; Erasmus, R.M.; Witcomb, M.J.

    2009-01-01

    Optical methods can provide important insights into the mechanisms and consequences of ion beam interactions with solids. This is illustrated by four distinctly different systems. X- and Y-cut LiNbO 3 crystals implanted with 8 MeV Au 3+ ions with a fluence of 1 x 10 17 ions/cm 2 result in gold nanoparticle formation during high temperature annealing. Optical extinction curves simulated by the Mie theory provide the average nanoparticle sizes. TEM studies are in reasonable agreement and confirm a near-spherical nanoparticle shape but with surface facets. Large temperature differences in the nanoparticle creation in the X- and Y-cut crystals are explained by recrystallisation of the initially amorphised regions so as to recreate the prior crystal structure and to result in anisotropic diffusion of the implanted gold. Defect formation in alkali halides using ion beam irradiation has provided new information. Radiation-hard CsI crystals bombarded with 1 MeV protons at 300 K successfully produce F-type centres and V-centres having the I 3 - structure as identified by optical absorption and Raman studies. The results are discussed in relation to the formation of interstitial iodine aggregates of various types in alkali iodides. Depth profiling of I 3 - and I 5 - aggregates created in RbI bombarded with 13.6 MeV/A argon ions at 300 K is discussed. The recrystallisation of an amorphous silicon layer created in crystalline silicon bombarded with 100 keV carbon ions with a fluence of 5 x 10 17 ions/cm 2 during subsequent high temperature annealing is studied by Raman and Brillouin light scattering. Irradiation of tin-doped indium oxide (ITO) films with 1 MeV protons with fluences from 1 x 10 15 to 250 x 10 15 ions/cm -2 induces visible darkening over a broad spectral region that shows three stages of development. This is attributed to the formation of defect clusters by a model of defect growth and also high fluence optical absorption studies. X-ray diffraction studies show

  3. Ion beam induced defects in solids studied by optical techniques

    Science.gov (United States)

    Comins, J. D.; Amolo, G. O.; Derry, T. E.; Connell, S. H.; Erasmus, R. M.; Witcomb, M. J.

    2009-08-01

    Optical methods can provide important insights into the mechanisms and consequences of ion beam interactions with solids. This is illustrated by four distinctly different systems. X- and Y-cut LiNbO 3 crystals implanted with 8 MeV Au 3+ ions with a fluence of 1 × 10 17 ions/cm 2 result in gold nanoparticle formation during high temperature annealing. Optical extinction curves simulated by the Mie theory provide the average nanoparticle sizes. TEM studies are in reasonable agreement and confirm a near-spherical nanoparticle shape but with surface facets. Large temperature differences in the nanoparticle creation in the X- and Y-cut crystals are explained by recrystallisation of the initially amorphised regions so as to recreate the prior crystal structure and to result in anisotropic diffusion of the implanted gold. Defect formation in alkali halides using ion beam irradiation has provided new information. Radiation-hard CsI crystals bombarded with 1 MeV protons at 300 K successfully produce F-type centres and V-centres having the I3- structure as identified by optical absorption and Raman studies. The results are discussed in relation to the formation of interstitial iodine aggregates of various types in alkali iodides. Depth profiling of I3- and I5- aggregates created in RbI bombarded with 13.6 MeV/A argon ions at 300 K is discussed. The recrystallisation of an amorphous silicon layer created in crystalline silicon bombarded with 100 keV carbon ions with a fluence of 5 × 10 17 ions/cm 2 during subsequent high temperature annealing is studied by Raman and Brillouin light scattering. Irradiation of tin-doped indium oxide (ITO) films with 1 MeV protons with fluences from 1 × 10 15 to 250 × 10 15 ions/cm -2 induces visible darkening over a broad spectral region that shows three stages of development. This is attributed to the formation of defect clusters by a model of defect growth and also high fluence optical absorption studies. X-ray diffraction studies show

  4. Corrosion-resistant coating technique for oxide-dispersion-strengthened ferritic/martensitic steel

    International Nuclear Information System (INIS)

    Sakasegawa, Hideo; Tanigawa, Hiroyasu; Ando, Masami

    2014-01-01

    Oxide-dispersion-strengthened (ODS) steels are attractive materials for application as fuel cladding in fast reactors and first-wall material of fusion blanket. Recent studies have focused more on high-chromium ferritic (12-18 wt% Cr) ODS steels with attractive corrosion resistance properties. However, they have poor material workability, require complicated heat treatments for recrystallization, and possess anisotropic microstructures and mechanical properties. On the other hand, low-chromium ferritic/martensitic (8-9 wt% Cr) ODS steels have no such limitations; nonetheless, they have poor corrosion resistance properties. In our work, we developed a corrosion-resistant coating technique for a low-chromium ferritic/martensitic ODS steel. The ODS steel was coated with the 304 or 430 stainless steel, which has better corrosion resistances than the low-chromium ferritic/martensitic ODS steels. The 304 or 430 stainless steel was coated by changing the canning material from mild steel to stainless steel in the conventional material processing procedure for ODS steels. Microstructural observations and micro-hardness tests proved that the stainless steels were successfully coated without causing a deterioration in the mechanical property of the low-chromium ferritic/martensitic ODS steel. (author)

  5. Effect of particle size of drug on conversion of crystals to an amorphous state in a solid dispersion with crospovidone.

    Science.gov (United States)

    Sugamura, Yuka; Fujii, Makiko; Nakanishi, Sayaka; Suzuki, Ayako; Shibata, Yusuke; Koizumi, Naoya; Watanabe, Yoshiteru

    2011-01-01

    The effect of particle size on amorphization of drugs in a solid dispersion (SD) was investigated for two drugs, indomethacin (IM) and nifedipine (NP). The SD of drugs were prepared in a mixture with crospovidone by a variety of mechanical methods, and their properties investigated by particle sizing, thermal analysis, and powder X-ray diffraction. IM, which had an initial particle size of 1 µm and tends to aggregate, was forced through a sieve to break up the particles. NP, which had a large initial particle size, was jet-milled. In both cases, reduction of the particle size of the drugs enabled transition to an amorphous state below the melting point of the drug. The reduction in particle size is considered to enable increased contact between the crospovidone and drug particles, increasing interactions between the two compounds. © 2011 Pharmaceutical Society of Japan

  6. Development of Tablet Formulation of Amorphous Solid Dispersions Prepared by Hot Melt Extrusion Using Quality by Design Approach.

    Science.gov (United States)

    Agrawal, Anjali; Dudhedia, Mayur; Deng, Weibin; Shepard, Kevin; Zhong, Li; Povilaitis, Edward; Zimny, Ewa

    2016-02-01

    The objective of the study was to identify the extragranular component requirements (level and type of excipients) to develop an immediate release tablet of solid dispersions prepared by hot melt extrusion (HME) process using commonly used HME polymers. Solid dispersions of compound X were prepared using polyvinyl pyrrolidone co-vinyl acetate 64 (PVP VA64), Soluplus, and hypromellose acetate succinate (HPMCAS-LF) polymers in 1:2 ratio by HME through 18 mm extruder. A mixture design was employed to study effect of type of polymer, filler (microcrystalline cellulose (MCC), lactose, and dicalcium phosphate anhydrous (DCPA)), and disintegrant (Crospovidone, croscarmellose sodium, and sodium starch glycolate (SSG)) as well as level of extrudates, filler, and disintegrant on tablet properties such as disintegration time (DT), tensile strength (TS), compactibility, and dissolution. Higher extrudate level resulted in longer DT and lower TS so 60-70% was the maximum amount of acceptable extrudate level in tablets. Fast disintegration was achieved with HPMCAS-containing tablets, whereas Soluplus- and PVP VA64-containing tablets had higher TS. Crospovidone and croscarmellose sodium were more suitable disintegrant than SSG to achieve short DT, and MCC was a suitable filler to prepare tablets with acceptable TS for each studied HME polymer. The influence of extragranular components on dissolution from tablets should be carefully evaluated while finalizing tablet composition, as it varies for each HME polymer. The developed statistical models identified suitable level of fillers and disintegrants for each studied HME polymer to achieve tablets with rapid DT (tablet porosity), and their predictivity was confirmed by conducting internal and external validation studies.

  7. Numerical simulation of hot-melt extrusion processes for amorphous solid dispersions using model-based melt viscosity.

    Science.gov (United States)

    Bochmann, Esther S; Steffens, Kristina E; Gryczke, Andreas; Wagner, Karl G

    2018-03-01

    Simulation of HME processes is a valuable tool for increased process understanding and ease of scale-up. However, the experimental determination of all required input parameters is tedious, namely the melt rheology of the amorphous solid dispersion (ASD) in question. Hence, a procedure to simplify the application of hot-melt extrusion (HME) simulation for forming amorphous solid dispersions (ASD) is presented. The commercial 1D simulation software Ludovic ® was used to conduct (i) simulations using a full experimental data set of all input variables including melt rheology and (ii) simulations using model-based melt viscosity data based on the ASDs glass transition and the physical properties of polymeric matrix only. Both types of HME computation were further compared to experimental HME results. Variation in physical properties (e.g. heat capacity, density) and several process characteristics of HME (residence time distribution, energy consumption) among the simulations and experiments were evaluated. The model-based melt viscosity was calculated by using the glass transition temperature (T g ) of the investigated blend and the melt viscosity of the polymeric matrix by means of a T g -viscosity correlation. The results of measured melt viscosity and model-based melt viscosity were similar with only few exceptions, leading to similar HME simulation outcomes. At the end, the experimental effort prior to HME simulation could be minimized and the procedure enables a good starting point for rational development of ASDs by means of HME. As model excipients, Vinylpyrrolidone-vinyl acetate copolymer (COP) in combination with various APIs (carbamazepine, dipyridamole, indomethacin, and ibuprofen) or polyethylene glycol (PEG 1500) as plasticizer were used to form the ASDs. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. 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.

  9. 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.

  10. 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).

  11. Curcumin-Eudragit® E PO solid dispersion: A simple and potent method to solve the problems of curcumin.

    Science.gov (United States)

    Li, Jinglei; Lee, Il Woo; Shin, Gye Hwa; Chen, Xiguang; Park, Hyun Jin

    2015-08-01

    Using a simple solution mixing method, curcumin was dispersed in the matrix of Eudragit® E PO polymer. Water solubility of curcumin in curcumin-Eudragit® E PO solid dispersion (Cur@EPO) was greatly increased. Based on the results of several tests, curcumin was demonstrated to exist in the polymer matrix in amorphous state. The interaction between curcumin and the polymer was investigated through Fourier transform infrared spectroscopy and (1)H NMR which implied that OH group of curcumin and carbonyl group of the polymer involved in the H bonding formation. Cur@EPO also provided protection function for curcumin as verified by the pH challenge and UV irradiation test. The pH value influenced curcumin release profile in which sustained release pattern was revealed. Additionally, in vitro transdermal test was conducted to assess the potential of Cur@EPO as a vehicle to deliver curcumin through this alternative administration route. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. 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.

  13. 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

  14. Design of sustained-release nitrendipine microspheres having solid dispersion structure by quasi-emulsion solvent diffusion method

    DEFF Research Database (Denmark)

    Cui, Fude; Yang, Mingshi; Jiang, Yanyan

    2003-01-01

    crystallization technique, i.e. quasi-emulsion solvent diffusion method. The factors of effect on micromeritic properties and release profiles of the resultant microspheres were investigated. And the bioavailability of nitrendipine microspheres was evaluated in six healthy dogs. The results showed...... that the particle size of microspheres was determined mainly by the agitation speed. The dissolution rate of nitrendipine from microspheres was enhanced significantly with increasing the amount of dispersing agents, and sustained by adding retarding agents. The release rate of microspheres could be controlled...

  15. Use of conventional-and radioisotope techniques to study the dynamic behavior of a particulate solid

    International Nuclear Information System (INIS)

    Santos Ferreira, L. dos.

    1976-01-01

    The behavior of solids in particlephase is studied with the purpose of determining the drop pressure through orificius of a Hopper, with conventional techniques as well as a new technique with radioisotopes to measure the porosity near the orifice of the Hopper. The rate of discharge was also studied. The use of radioisotopes presented similar results as those obtained elsewhere by conventional techniques. (Author) [pt

  16. 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.

  17. 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.

  18. Solubility enhancement of BCS Class II drug by solid phospholipid dispersions: Spray drying versus freeze-drying.

    Science.gov (United States)

    Fong, Sophia Yui Kau; Ibisogly, Asiye; Bauer-Brandl, Annette

    2015-12-30

    The poor aqueous solubility of BCS Class II drugs represents a major challenge for oral dosage form development. Using celecoxib (CXB) as model drug, the current study adopted a novel solid phospholipid nanoparticle (SPLN) approach and compared the effect of two commonly used industrial manufacturing methods, spray- and freeze-drying, on the solubility and dissolution enhancement of CXB. CXB was formulated with Phospholipoid E80 (PL) and trehalose at different CXB:PL:trehalose ratios, of which 1:10:16 was the optimal formulation. Spherical amorphous SPLNs with average diameters <1μm were produced by spray-drying; while amorphous 'matrix'-like structures of solid PL dispersion with larger particle sizes were prepared by freeze-drying. Formulations from both methods significantly enhanced the dissolution rates, apparent solubility, and molecularly dissolved concentration of CXB in phosphate buffer (PBS, pH 6.5) and in biorelevant fasted state simulated intestinal fluid (FaSSIF, pH 6.5) (p<0.05). While similar dissolution rates were found, the spray-dried SPLNs had a larger enhancement in apparent solubility (29- to 132-fold) as well as molecular solubility (18-fold) of CXB at equilibrium (p<0.05). The strong capability of the spray-dried SPLNs to attain 'true' supersaturation state makes them a promising approach for bioavailability enhancement of poorly soluble drugs. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Dispersing Si{sub 3}N{sub 4} at high solids loading - applied to protein forming

    Energy Technology Data Exchange (ETDEWEB)

    Lyckfeldt, O.; Palmqvist, L. [Swedish Ceramic Inst., Goeteborg (Sweden); Poeydemenge, F. [ENSCI, Limoges (France)

    2002-07-01

    The dispersing of a Si{sub 3}N{sub 4} powder (UBE SN-E10) at high solids loading in aqueous media was investigated. The powder was used in the as-received (raw) state, after thermal (calcinations) and/or mechanical pre-treatments (ball milling{yields}freeze granulation{yields}freeze-drying). Slips were prepared using pH adjustment with NH{sub 4}OH or an addition of Tiron (low-M{sub w} sulphonic acid). Zeta potential measurements of diluted systems and rheological evaluations of concentrated suspensions were conducted. The effect of adding whey protein concentrate (WPC) was also studied. Zeta potential measurements showed a clear decrease in pH{sub iep} by calcination, whereas Tiron slightly increased the pH{sub iep} of calcined powder and decreased the pH{sub iep} of the as-received powder. Rheological data showed that pH adjustment to 10 was more efficient in stabilising the as-received powder than the calcined powder. pH adjustment was also considered to be the most important effect of adding small amounts of Tiron (0.08 wt%). However, for calcined powder, Tiron was shown to be equally efficient as pH adjustment. Pre-milling followed by freeze granulation/freeze-drying resulted in de-agglomerated powders with improved ability to rapidly disperse and, hence, extend the possibility of achieving extreme solids loadings. When approaching the practical limits in solids loading of these pre-milled powders, slips with 49.5 vol% of as-received and 46.6 vol% of calcined powders displayed clear shear thickening behaviour. However, addition of WPC (12 wt% based on water) significantly decreased the degree of shear thickening although the viscosity at lower shear rates increased. The gelling of WPC was distinct and rapid in suspensions with the two pre-milled powders, as-received stabilised at pH 10 and calcined stabilised with Tiron. (orig.)

  20. 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.

  1. 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.

  2. Inventory of oral anticancer agents : Pharmaceutical formulation aspects with focus on the solid dispersion technique

    NARCIS (Netherlands)

    Sawicki, E.; Schellens, J. H M; Beijnen, J. H.; Nuijen, B.

    2016-01-01

    Dissolution from the pharmaceutical formulation is a prerequisite for complete and consistent absorption of any orally administered drug, including anticancer agents (oncolytics). Poor dissolution of an oncolytic can result in low oral bioavailability, high variability in blood concentrations and

  3. Comparison of in situ polymerization and solution-dispersion techniques in the preparation of Polyimide/Montmorillonite (MMT) Nanocomposites.

    Science.gov (United States)

    Ahmad, Mansor Bin; Gharayebi, Yadollah; Salit, Mohd Sapuan; Hussein, Mohd Zobir; Shameli, Kamyar

    2011-01-01

    In this paper, Polyimide/Montmorillonite Nanocomposites (PI/MMT NCs), based on aromatic diamine (4-Aminophenyl sulfone) (APS) and aromatic dianhydride (3,3',4,4'-benzophenonetetracarboxylic dianhydride) (BTDA) were prepared using in situ polymerization and solution-dispersion techniques. The prepared PI/MMT NCs films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The XRD results showed that at the content of 1.0 wt % Organo Montmorillonite (OMMT) for two techniques and 3.0 wt % OMMT for the in situ polymerization technique, the OMMT was well-intercalated, exfoliated and dispersed into polyimide matrix. The OMMT agglomerated when its amount exceeded 10 wt % and 3.0 wt % for solution-dispersion and in situ polymerization techniques respectively. These results were confirmed by the TEM images of the prepared PI/MMT NCs. The TGA thermograms indicated that thermal stability of prepared PI/MMT NCs were increased with the increase of loading that, the effect is higher for the samples prepared by in situ polymerization technique.

  4. 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.

  5. 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.

  6. 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.

  7. 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...

  8. 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.

  9. Seed dispersal into wetlands: Techniques and results for a restored tidal freshwater marsh

    Science.gov (United States)

    Neff, K.P.; Baldwin, A.H.

    2005-01-01

    Although seed dispersal is assumed to be a major factor determining plant community development in restored wetlands, little research exists on density and species richness of seed available through dispersal in these systems. We measured composition and seed dispersal rates at a restored tidal freshwater marsh in Washington, DC, USA by collecting seed dispersing through water and wind. Seed dispersal by water was measured using two methods of seed collection: (1) stationary traps composed of coconut fiber mat along an elevation gradient bracketing the tidal range and (2) a floating surface trawl net attached to a boat. To estimate wind dispersal rates, we collected seed from stationary traps composed of coconut fiber mat positioned above marsh vegetation. We also collected a small number of samples of debris deposited along high tide lines (drift lines) and feces of Canada Goose to explore their seed content. We used the seedling emergence method to determine seed density in all samples, which involved placing the fiber mats or sample material on top of potting soil in a greenhouse misting room and enumerating emerging seedlings. Seedlings from a total of 125 plant species emerged during this study (including 82 in river trawls, 89 in stationary water traps, 21 in drift lines, 39 in wind traps, and 10 in goose feces). The most abundant taxa included Bidens frondosa, Boehmeria cylindrica, Cyperus spp., Eclipta prostrata, and Ludwigia palustris. Total seedling density was significantly greater for the stationary water traps (212 + 30.6 seeds/m2/month) than the equal-sized stationary wind traps (18 + 6.0 seeds/m(2)/month). Lower-bound estimates of total species richness based on the non-parametric Chao 2 asymptotic estimators were greater for seeds in water (106 + 1.4 for stationary water traps and 104 + 5.5 for trawl samples) than for wind (54 + 6.4). Our results indicate that water is the primary source of seeds dispersing to the site and that a species-rich pool

  10. Optical techniques for probing the excited state dynamics of quantum dot solids

    Energy Technology Data Exchange (ETDEWEB)

    Moroz, P.; Kholmicheva, N.; Razgoniaeva, N. [Center for Photochemical Sciences, Bowling Green State University, Bowling Green, OH 43402 (United States); Department of Physics, Bowling Green State University, Bowling Green, OH 43402 (United States); Burchfield, D. [Department of Chemistry, Bowling Green State University, Bowling Green, OH 43402 (United States); Sharma, N.; Acharya, A. [Department of Physics, Bowling Green State University, Bowling Green, OH 43402 (United States); Zamkov, M., E-mail: zamkovm@bgsu.edu [Center for Photochemical Sciences, Bowling Green State University, Bowling Green, OH 43402 (United States); Department of Physics, Bowling Green State University, Bowling Green, OH 43402 (United States)

    2016-06-01

    Highlights: • Optical techniques represent a powerful tool for probing exciton diffusion in QD solids. • Exciton dissociation in QD solids is caused by charge tunneling to traps and other dots. • Exciton and free-carrier lifetimes are given by fast and slow components of PL decay. • Surface PL offers valuable information on the type and density of traps in QD solids. - Abstract: Quantum dot (QD) solids represent an important class of functional materials that holds strong promise for future applications in technology. Their optoelectronic properties are determined by energy diffusion processes, which character can often be inferred from the temporal and spectral analysis of the film’s photoluminescence (PL). Here, optical techniques based on PL lifetime, bulk quenching, and temperature-dependent PL will be discussed. These techniques complement the electrical conductivity measurements by mapping the flow of optically induced excitons through undepleted, contact-free films with an unprecedented temporal and spatial resolution. By correlating the QD solid morphology with the ensuing photoluminescence (PL) dynamics, these methods allow estimating important transport characteristics, including exciton and charge carrier diffusion lengths, the rate of interparticle energy transfer, carrier mobility, and the exciton diffusivity. The review will cover most popular PL-based strategies and summarize the key experimental findings resulting from these works.

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

    Science.gov (United States)

    Mashile, Geaneth Pertunia; Nomngongo, Philiswa N

    2017-03-04

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

  12. Co-ordinated research programme on the use of nuclear and nuclear-related techniques in the study of environmental pollution associated with solid wastes

    International Nuclear Information System (INIS)

    1991-01-01

    A co-ordinated research programme on the use of nuclear and nuclear-related techniques in the study of environmental pollution associated with solid wastes was started by the IAEA in December 1987 and now comprises twenty-three participants from twenty-one countries. Topics of interest in this programme include studies of atmospheric aerosols, coal fly ash, incinerator ash, sewage sludge and a variety of other environmental specimens contaminated with solid wastes. The analytical techniques used include neutron activation analysis, particle-induced X-ray emission and energy-dispersive X-ray fluorescence. This report summarizes the discussions that took place during the second research co-ordination meeting. Working papers presented by the participants are included as annexes and have been indexed separately. Refs, figs and tabs

  13. Co-ordinated research programme on the use of nuclear and nuclear-related techniques in the study of environmental pollution associated with solid wastes

    International Nuclear Information System (INIS)

    1992-01-01

    A co-ordinated research programme on the use of nuclear and nuclear-related techniques in the study of environmental pollution associated with solid wastes was started by the IAEA in December 1987 and now comprises nineteen participants from seventeen countries. Topics of interest in this programme include studies of atmospheric aerosols, coal fly ash, incinerator ash, sewage sludge and a variety of other environmental specimens contaminated with solid wastes. The analytical techniques used include neutron activation analysis, particle-induced X-ray emission and energy-dispersive X-ray fluorescence. This report summarizes the discussions that took place during the third research co-ordination meeting. Working papers presented by the participants are included as annexes and have been indexed separately. Refs, figs and tabs

  14. 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.

  15. 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.

  16. Radioimmunoassay of diagoxin with the aid of the solid phase - microtitre plating technique

    International Nuclear Information System (INIS)

    Scheidt, C.

    1982-01-01

    Preliminary results are reported here on the development of a digoxin-radioimmunoassay with an anti-digoxin antibody (goat) in a solid phase technique (mictrotitre plate). The advantages compared to conventional RIAs are: Cross reactions towards digoxin is minimal, both in vitro and in vivo. The calibraton range extends from 0.25 to 8 ng/ml. The radioactive load could be reduced significantly by use of smaller amounts of tracer (0.004 μCi/single determination) and by reduction of waste volume (solid), waste weight (solid) and liquid waste. The DIGOXIN RIA BIOTEST MTP is, in addition, the only digoxin radioimmunoassay where radioactive waste is produced in a sealed form. The test is a simple one and can be carried out without the need for complicated apparatus and techniques. (orig./MG) [de

  17. Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry.

    Science.gov (United States)

    Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

    2013-12-20

    Solid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about novel methodological and instrumental solutions in relation to different variants of solid phase extraction techniques, solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE) and magnetic solid phase extraction (MSPE) is presented, including practical applications of these techniques and a critical discussion about their advantages and disadvantages. The proposed solutions fulfill the requirements resulting from the concept of sustainable development, and specifically from the implementation of green chemistry principles in analytical laboratories. Therefore, particular attention was paid to the description of possible uses of novel, selective stationary phases in extraction techniques, inter alia, polymeric ionic liquids, carbon nanotubes, and silica- and carbon-based sorbents. The methodological solutions, together with properly matched sampling devices for collecting analytes from samples with varying matrix composition, enable us to reduce the number of errors during the sample preparation prior to chromatographic analysis as well as to limit the negative impact of this analytical step on the natural environment and the health of laboratory employees. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Studies for determining drain solid flow in bed silt, using radioisotope techniques

    International Nuclear Information System (INIS)

    Sanchez, W.

    1976-01-01

    A process for measuring solid flow in silt bed using isotopic technique is studied. Comparative studies for initial movement of grinded glass grains and sand grains is done. The development for determining the minimum mass of radioative grains of sand, used for flow evaluation is also studied. Further experiments in the field of reference confirm technological conditions for the method [pt

  19. What Is the Mechanism Behind Increased Permeation Rate of a Poorly Soluble Drug from Aqueous Dispersions of an Amorphous Solid Dispersion?

    DEFF Research Database (Denmark)

    Frank, K. J.; Westedt, U.; Rosenblatt, K. M.

    2014-01-01

    of amorphous microparticles present in aqueous dispersions induces lasting supersaturation maintaining enhanced permeation. The hypothesis is supported by a slower drug permeation when the microparticles were removed. (c) 2014 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci...

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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

  5. The Preparation and Performances of Self-Dispersed Nanomicron Emulsified Wax Solid Lubricant Ewax for Drilling Fluids

    Directory of Open Access Journals (Sweden)

    Feng-shan Zhou

    2014-01-01

    Full Text Available An oil-in-water nanomicron wax emulsion with oil phase content 45 wt% was prepared by using the emulsifying method of surfactant-in-oil. The optimum prepared condition is 85°C, 20 min, and 5 wt% complex emulsifiers. Then the abovementioned nanomicron emulsifying wax was immersed into a special water-soluble polymer in a certain percentage by the semidry technology. At last, a solidified self-dispersed nanomicron emulsified wax named as Ewax, a kind of solid lubricant for water based drilling fluid, was obtained after dried in the special soluble polymer containing emulsifying wax in low temperature. It is shown that the adhesion coefficient reduced rate (ΔKf is 73.5% and the extreme pressure (E-P friction coefficient reduced rate (Δf is 77.6% when the produced Ewax sample was added to fresh water based drilling fluid at dosage 1.0 wt%. In comparison with other normal similar liquid products, Ewax not only has better performances of lubrication, filtration loss control property, heat resistance, and tolerance to salt and is environmentally friendly, but also can solve the problems of freezing in the winter and poor storage stability of liquid wax emulsion in oilfield applications.

  6. 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.

  7. Polar Quassinoids in Standardized Eurycoma longifolia Extract Formulated into a Lipid-Based Solid Dispersion to Improve Rat Sperm Count.

    Science.gov (United States)

    Ma, Hai-Qiu; Ebrahimi, Forough; Low, Bin-Seng; Khan, Nurzalina Abdul Karim; Chan, Kit-Lam

    2017-12-01

    Eurycoma longifolia Jack is popularly sought in Southeast Asian countries for traditional remedies to improve sexual performance and fertility. 13α(21)-Epoxyeurycomanone and eurycomanone, two major quassinoids in a root extract (TAF2) were reported to improve rat spermatogenesis and fertility. Unfortunately, these quassinoids possess low bioavailability because of high aqueous solubility and low lipid membrane permeability. Often, other possible barriers may be P-glycoprotein (P-gp) efflux in the gut and presystemic hepatic metabolism. The present study attempted to solve these problems by formulating a lipid-based solid dispersion (TAF2-SD) of optimized mixture of TAF2 and emulsifiers, which was then orally administered to rats prior to sperm count analysis. The TAF2-SD-treated rats showed significantly twofold (p < 0.001) and fourfold (p < 0.001) higher sperm count than did TAF2-treated and vehicle-treated (control) rats, respectively. The study also demonstrated no significant in vitro ileal absorption changes of the quassinoids by P-gp efflux inhibitors and concentration change or secondary metabolite formation upon in vitro incubation with rat liver homogenates, suggesting that P-gp-mediated efflux and presystemic metabolism were not limiting their bioavailability. Further study on orally TAF2-treated rats confirmed that the area under the curve and bioavailability curve of each quassinoid in the absence and presence of ketoconazole were unchanged. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  8. Electrospun 4th-Generation Solid Dispersions of Poorly Water-Soluble Drug Utilizing Two Different Processes

    Directory of Open Access Journals (Sweden)

    Zhu Zhang

    2018-01-01

    Full Text Available Different from traditional solid dispersion (SD for improving the dissolution rates of poorly water-soluble drugs, the upgraded 4th SD was developed to furnish a drug sustained-release profile. In this work, two different kinds of 4th SDs were fabricated using two electrospinning processes. One is a ternary SD (nanofibers F2 that consisted of ethyl cellulose (EC, polyethylene glycol 1000 (PEG, and tamoxifen citrate (TAM from a modified coaxial process, and the other is a binary SD (nanofibers F1 which is comprised of EC and TAM from a single-fluid blending process. Scanning electronic microscopic observations demonstrated that F2 (330±50 nm showed a better quality than F1 (870±230 nm in terms of size and size distribution although both of them had a smooth surface morphology and a cross section. X-ray diffraction patterns verified that both SDs were amorphous nanocomposites owing to the favorable secondary interactions among these components, as suggested from the results of FTIR. In vitro dissolution experiments indicated that F2 could furnish an improved drug sustained-release characteristics compared to F1, exhausting all the contained TAM and having weaker leveling-off late release. The molecular behaviors of drug sustained-release from the binary 4th SD were suggested. The protocols reported here paved an alternative way for developing novel functional nanomaterials for effective delivery of poorly water-soluble drugs.

  9. Pediatric suppositories of sulpiride solid dispersion for treatment of Tourette syndrome: in vitro and in vivo investigations.

    Science.gov (United States)

    Zidan, Ahmed S; Emam, Sherif E; Shehata, Tamer M; Ghazy, Fakhr-eldin S

    2015-06-01

    Pharmaceutical development was adopted in the current study to propose a pediatric rectal formulation of sulpiride as a substitute to the available oral or parenteral formulations in the management of Tourette syndrome (TS). The goal was to formulate a product that is easy to use, stable, and highly bioavailable and to achieve a rapid clinical efficacy. Towards this aim, sulpiride solid dispersion (SD) with tartaric acid at a weight ratio of 1:0.25 was incorporated into different suppository bases, namely witepsol W25, witepsol H15, witepsol E75, suppocire NA, suppocire A, glycerogelatin, and polyethylene glycols. The formulae were evaluated in vitro using different pharmacotechnical methods such as visual, melting, weight and content uniformities, drug release, differential scanning calorimetry (DSC), Fourier transform infrared (FTIR), and X-ray diffraction (XRD) analyses. In vivo bioavailability was also assessed in rabbits to compare the bioavailability of either raw sulpiride-incorporated or its SD-incorporated witepsol H15-based suppositories to its oral suspension (reference). Sulpiride SD-incorporated witepsol H15 formulation showed acceptable in vitro characteristics with a bioavailability of 117% relative to oral dosing, which excel that in humans (27% after dosing of oral product). In addition, the proposed formula not only passed the 6-month stability study but also proposed a promising scale-up approach. Hence, it showed a great potential for pediatric product development to manage TS in rural areas.

  10. Electrosprayed core–shell solid dispersions of acyclovir fabricated using an epoxy-coated concentric spray head

    Science.gov (United States)

    Liu, Zhe-Peng; Cui, Lei; Yu, Deng-Guang; Zhao, Zhuan-Xia; Chen, Lan

    2014-01-01

    A novel structural solid dispersion (SD) taking the form of core–shell microparticles for poorly water-soluble drugs is reported for the first time. Using polyvinylpyrrolidone (PVP) as a hydrophilic polymer matrix, the SDs were fabricated using coaxial electrospraying (characterized by an epoxy-coated concentric spray head), although the core fluids were unprocessable using one-fluid electrospraying. Through manipulating the flow rates of the core drug-loaded solutions, two types of core–shell microparticles with tunable drug contents were prepared. They had average diameters of 1.36±0.67 and 1.74±0.58 μm, and were essentially a combination of nanocomposites with the active ingredient acyclovir (ACY) distributed in the inner core, and the sweeter sucralose and transmembrane enhancer sodium dodecyl sulfate localized in the outer shell. Differential scanning calorimetry and X-ray diffraction results demonstrated that ACY, sodium dodecyl sulfate, and sucralose were well distributed in the PVP matrix in an amorphous state because of favorable second-order interactions. In vitro dissolution and permeation studies showed that the core–shell microparticle SDs rapidly freed ACY within 1 minute and promoted nearly eightfold increases in permeation rate across the sublingual mucosa compared with raw ACY powders. PMID:24790437

  11. Optimization of the Büchi B-90 spray drying process using central composite design for preparation of solid dispersions.

    Science.gov (United States)

    Gu, Bing; Linehan, Brian; Tseng, Yin-Chao

    2015-08-01

    A central composite design approach was applied to study the effect of polymer concentration, inlet temperature and air flow rate on the spray drying process of the Büchi B-90 nano spray dryer (B-90). Hypromellose acetate succinate-LF was used for the Design of Experiment (DoE) study. Statistically significant models to predict the yield, spray rate, and drying efficiency were generated from the study. The spray drying conditions were optimized according to the models to maximize the yield and efficiency of the process. The models were further validated using a poorly water-soluble investigational compound (BI064) from Boehringer Ingelheim Pharmaceuticals. The polymer/drug ratio ranged from 1/1 to 3/1w/w. The spray dried formulations were amorphous determined by differential scanning calorimetry and X-ray powder diffraction. The particle size of the spray dried formulations was 2-10 μm under polarized light microscopy. All the formulations were physically stable for at least 3h when suspended in an aqueous vehicle composed of 1% methyl cellulose. This study demonstrates that DoE is a useful tool to optimize the spray drying process, and the B-90 can be used to efficiently produce amorphous solid dispersions with a limited quantity of drug substance available during drug discovery stages. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. 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.

  13. Curcumin-loaded self-nanomicellizing solid dispersion system: part I: development, optimization, characterization, and oral bioavailability.

    Science.gov (United States)

    Parikh, Ankit; Kathawala, Krishna; Song, Yunmei; Zhou, Xin-Fu; Garg, Sanjay

    2018-05-29

    Curcumin (CUR) is considered as one of the most bioactive molecules ever discovered from nature due to its proven anti-inflammatory and antioxidant in both preclinical and clinical studies. Despite its proven safety and efficacy, the clinical translation of CUR into a useful therapeutic agent is still limited due to its poor oral bioavailability. To overcome its limitation and enhance oral bioavailability by improving its aqueous solubility, stability, and intestinal permeability, a novel CUR formulation (NCF) was developed using the self-nanomicellizing solid dispersion strategy. From the initial screening of polymers for their potential to improve the solubility and stability, Soluplus (SOL) was selected. The optimized NCF demonstrated over 20,000-fold improvement in aqueous solubility as a result of amorphization, hydrogen bonding interaction, and micellization determined using differential scanning calorimetry, X-ray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, nuclear magnetic resonance, dynamic light scattering, and transmission electron microscopy. Moreover, the greater stabilizing effect in alkaline pH and light was observed. Furthermore, significant enhancement of dissolution and permeability of CUR across everted sacs of rat small intestine were noticed. Pharmacokinetic studies demonstrated that the oral bioavailability of CUR was increased 117 and 17-fold in case of NCF and physical mixture of CUR and SOL compared to CUR suspension. These results suggest NCF identified as a promising new approach for repositioning of CUR for pharmaceutical application by enhancing the oral bioavailability of CUR. The findings herein stimulate further in vivo evaluations and clinical tests of NCF.

  14. 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.

  15. 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)

  16. Dissolvable layered double hydroxide as an efficient nanosorbent for centrifugeless air-agitated dispersive solid-phase extraction of potentially toxic metal ions from bio-fluid samples

    Energy Technology Data Exchange (ETDEWEB)

    Rajabi, Maryam, E-mail: mrajabi@semnan.ac.ir; Arghavani-Beydokhti, Somayeh; Barfi, Behruz; Asghari, Alireza

    2017-03-08

    In the present work, a novel nanosorbent namely layered double hydroxides with 4-amino-5-hydroxyl-2,7-naphthalendisulfonic acid monosodium salt interlayer anion (Mg-Al-AHNDA-LDH) was synthesized and applied as a dissolvable nanosorbent in a centrifugeless ultrasound-enhanced air-agitated dispersive solid-phase extraction (USE-AA-D-SPE) method. This method was used for the separation and preconcentration of some metal ions including Cd{sup 2+}, Cr{sup 6+}, Pb{sup 2+}, Co{sup 2+}, and Ni{sup 2+} prior to their determination using the micro-sampling flame atomic absorption spectrometry (MS-FAAS) technique. The most interesting aspect of this nanosorbent is its immediate dissolvability at pH values lower than 4. This capability drastically eliminates the elution step, leading to a great improvement in the extraction efficiency and a decrease in the extraction time. Also in this method, the use of a syringe nanofilter eliminates the need for the centrifugation step, which is time-consuming and essentially causes the analysis to be off-line. Several effective parameters governing the extraction efficiency including the sample solution pH, amount of nanosorbent, eluent condition, number of air-agitation cycles, and sonication time were investigated and optimized. Under the optimized conditions, the good linear dynamic ranges of 2–70, 6–360, 7–725, 7–370, and 8–450 ng mL{sup −1} for the Cd{sup 2+}, Cr{sup 6+}, Pb{sup 2+}, Co{sup 2+}and Ni{sup 2+} ions, respectively, with the correlation of determinations (R{sup 2}s) higher than 0.997 were obtained. The limits of detection (LODs) were found to be 0.6, 1.7, 2.0, 2.1, and 2.4 for the Cd{sup 2+}, Cr{sup 6+}, Pb{sup 2+}, Co{sup 2+}, and Ni{sup 2+} ions, respectively. The intra-day and inter-day precisions (percent relative standard deviations (%RSDs) (n = 5)) were below 7.8%. The proposed method was also successfully applied for the extraction and determination of the target ions in different biological fluid

  17. Dissolvable layered double hydroxide as an efficient nanosorbent for centrifugeless air-agitated dispersive solid-phase extraction of potentially toxic metal ions from bio-fluid samples

    International Nuclear Information System (INIS)

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

    2017-01-01

    In the present work, a novel nanosorbent namely layered double hydroxides with 4-amino-5-hydroxyl-2,7-naphthalendisulfonic acid monosodium salt interlayer anion (Mg-Al-AHNDA-LDH) was synthesized and applied as a dissolvable nanosorbent in a centrifugeless ultrasound-enhanced air-agitated dispersive solid-phase extraction (USE-AA-D-SPE) method. This method was used for the separation and preconcentration of some metal ions including Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ , and Ni 2+ prior to their determination using the micro-sampling flame atomic absorption spectrometry (MS-FAAS) technique. The most interesting aspect of this nanosorbent is its immediate dissolvability at pH values lower than 4. This capability drastically eliminates the elution step, leading to a great improvement in the extraction efficiency and a decrease in the extraction time. Also in this method, the use of a syringe nanofilter eliminates the need for the centrifugation step, which is time-consuming and essentially causes the analysis to be off-line. Several effective parameters governing the extraction efficiency including the sample solution pH, amount of nanosorbent, eluent condition, number of air-agitation cycles, and sonication time were investigated and optimized. Under the optimized conditions, the good linear dynamic ranges of 2–70, 6–360, 7–725, 7–370, and 8–450 ng mL −1 for the Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ and Ni 2+ ions, respectively, with the correlation of determinations (R 2 s) higher than 0.997 were obtained. The limits of detection (LODs) were found to be 0.6, 1.7, 2.0, 2.1, and 2.4 for the Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ , and Ni 2+ ions, respectively. The intra-day and inter-day precisions (percent relative standard deviations (%RSDs) (n = 5)) were below 7.8%. The proposed method was also successfully applied for the extraction and determination of the target ions in different biological fluid and tap water samples. - Highlights: • A novel centrifugeless dispersive

  18. 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.

  19. Comparison between energy dispersive X-ray fluorescence and other nuclear analytical techniques in mineral exploration and mining

    International Nuclear Information System (INIS)

    Clayton, C.G.; Packer, T.W.; Wormald, M.R.

    1979-01-01

    At the present time there is an increasing awareness of the value and need for in-situ analytical methods throughout the general area of mineral exploration and mining. Of the alternative techniques, the measurement of natural gamma radiation is well established for uranium exploration and it is now being developed for sea-bed and lake-bed surveying. Energy dispersive X-ray fluorescence equipment is becoming more generally accepted, especially for mine control. Neutron techniques, for so long used routinely in oil well logging, are now being developed for a wide range of applications in all aspects of exploration and mining. It is believed that these techniques will result in major applications in the future. The present paper compares the principal characteristics of energy dispersive X-ray fluorescence and neutron techniques in particular, with special emphasis being given to those factors which affect the accuracy of analytical content; such as elemental resolution, matrix effects, material heterogeneity and neutron transport. A generalised comparison between the techniques is difficult to achieve because of the different nature of radiation interactions, but a range of applications is described and these show the complementary nature of the methods and point to the areas for more active development in the future. (author)

  20. Carbon monoxide MgO from dispersed solids to single crystals: a review and new advances

    Science.gov (United States)

    Spoto, G.; Gribov, E. N.; Ricchiardi, G.; Damin, A.; Scarano, D.; Bordiga, S.; Lamberti, C.; Zecchina, A.

    2004-10-01

    In this review we describe 30 years of research on the surface properties of magnesium oxide, considered as the model prototype oxide of cubic structure. The surface properties of single crystals, thin films and powdered samples (sintered at progressive higher temperatures) are considered and compared, with the aim of demonstrating that the gap between “believed perfect” single crystal surfaces, typical of “pure” Surface Science, and high surface area samples, typical of Catalysis Science, can be progressively reduced. The surface features considered in this review are the structural (morphological), optical, absorptive and reactive properties. As the carbon monoxide molecule is able to probe the surface properties of both anions and cations, it can give a complete information of the surface structure of MgO samples. For this reason the adsorption and spectroscopy of this molecule is preferentially considered in this review. Particular emphasis is given in reviewing results obtained by high resolution transmission microscopy and in situ IR spectroscopy of adsorbed species (in both reflection and transmission modes), but also UV-Vis diffuse reflectance, photoluminescence, TDS, EPR, electron based techniques are mentioned. Reviewed experimental results are also commented in view of the important theoretical literature available on this topic and are complemented by new transmission IR data concerning CO adsorbed, down to 60 K, on powdered MgO samples with increasing surface area. These innovative experiments allow us to perform, on powdered samples, the adsorption experiments typical of single crystals (or films) Surface Science, with an increase of the S/N of the vibrational features higher than two order of magnitude. As far the new results (never published before) are concerned, we report IR spectra of CO dosed at 60 K on polycrystalline MgO samples with different surface area obtained by Mg(OH) 2 decomposition and progressive sintering at high temperature

  1. 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.

  2. Simple Technique of Exfoliation and Dispersion of Multilayer Graphene from Natural Graphite by Ozone-Assisted Sonication.

    Science.gov (United States)

    Lin, Zaw; Karthik, Paneer Selvam; Hada, Masaki; Nishikawa, Takeshi; Hayashi, Yasuhiko

    2017-05-27

    Owing to its unique properties, graphene has attracted tremendous attention in many research fields. There is a great space to develop graphene synthesis techniques by an efficient and environmentally friendly approach. In this paper, we report a facile method to synthesize well-dispersed multilayer graphene (MLG) without using any chemical reagents or organic solvents. This was achieved by the ozone-assisted sonication of the natural graphite in a water medium. The frequency or number of ozone treatments plays an important role for the dispersion in the process. The possible mechanism of graphene exfoliation and the introduction of functional groups have been postulated. The experimental setup is unique for ozone treatment and enables the elimination of ozone off-gas. The heat generated by the dissipation of ultrasonic waves was used as it is, and no additional heat was supplied. The graphene dispersion was stable, and no evidence of aggregation was observed---even after several months. The characterization results show that well-dispersed MLG was successfully synthesized without any significant damage to the overall structure. The graphene obtained by this method has potential applications in composite materials, conductive coatings, energy storage, and electronic devices.

  3. Simple Technique of Exfoliation and Dispersion of Multilayer Graphene from Natural Graphite by Ozone-Assisted Sonication

    Directory of Open Access Journals (Sweden)

    Zaw Lin

    2017-05-01

    Full Text Available Owing to its unique properties, graphene has attracted tremendous attention in many research fields. There is a great space to develop graphene synthesis techniques by an efficient and environmentally friendly approach. In this paper, we report a facile method to synthesize well-dispersed multilayer graphene (MLG without using any chemical reagents or organic solvents. This was achieved by the ozone-assisted sonication of the natural graphite in a water medium. The frequency or number of ozone treatments plays an important role for the dispersion in the process. The possible mechanism of graphene exfoliation and the introduction of functional groups have been postulated. The experimental setup is unique for ozone treatment and enables the elimination of ozone off-gas. The heat generated by the dissipation of ultrasonic waves was used as it is, and no additional heat was supplied. The graphene dispersion was stable, and no evidence of aggregation was observed---even after several months. The characterization results show that well-dispersed MLG was successfully synthesized without any significant damage to the overall structure. The graphene obtained by this method has potential applications in composite materials, conductive coatings, energy storage, and electronic devices.

  4. The use of solid sorbents for direct accumulation of organic compounds from water matrices : a review of solid-phase extraction techniques

    NARCIS (Netherlands)

    Liska, I.; Krupcik, J.; Leclercq, P.A.

    1989-01-01

    The main principles of solid-phase extraction techniques are reviewed in this paper. Various solid sorbents can be used as a suitable trap for direct accumulation of organic compounds from aqueous solutions. The trapped analytes can be desorbed by elution with suitably chosen liquid phases. These

  5. 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.

  6. [Preparation of Oenothera biennis Oil Solid Lipid Nanoparticles Based on Microemulsion Technique].

    Science.gov (United States)

    Piao, Lin-mei; Jin, Yong; Cui, Yan-lin; Yin, Shou-yu

    2015-06-01

    To study the preparation of Oenothera biennis oil solid lipid nanoparticles and its quality evaluation. The solid lipid nanoparticles were prepared by microemulsion technique. The optimum condition was performed based on the orthogonal design to examine the entrapment efficiency, the mean diameter of the particles and so on. The optimal preparation of Oenothera biennis oil solid lipid nanoparticles was as follows: Oenothera biennis dosage 300 mg, glycerol monostearate-Oenothera biennis (2: 3), Oenothera biennis -RH/40/PEG-400 (1: 2), RH-40/PEG-400 (1: 2). The resulting nanoparticles average encapsulation efficiency was (89.89 ± 0.71)%, the average particle size was 44.43 ± 0.08 nm, and the Zeta potential was 64.72 ± 1.24 mV. The preparation process is simple, stable and feasible.

  7. 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.

  8. Measurement of soluble solids content in watermelon by Vis/NIR diffuse transmittance technique*

    OpenAIRE

    Tian, Hai-qing; Ying, Yi-bin; Lu, Hui-shan; Fu, Xia-ping; Yu, Hai-yan

    2007-01-01

    Watermelon is a popular fruit in the world with soluble solids content (SSC) being one of the major characteristics used for assessing its quality. This study was aimed at obtaining a method for nondestructive SSC detection of watermelons by means of visible/near infrared (Vis/NIR) diffuse transmittance technique. Vis/NIR transmittance spectra of intact watermelons were acquired using a low-cost commercially available spectrometer operating over the range 350~1000 nm. Spectra data were analyz...

  9. 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.

  10. Investigation of physicochemical factors affecting the stability of a pH-modulated solid dispersion and a tablet during storage.

    Science.gov (United States)

    Tran, Phuong Ha-Lien; Tran, Thao Truong-Dinh; Park, Jun-Bom; Min, Dong Hun; Choi, Han-Gon; Han, Hyo-Kyung; Rhee, Yun-Seok; Lee, Beom-Jin

    2011-07-29

    The stability of solid dispersions (SD) during storage is of concern. We prepared the pH-modulated SD (pSD) and compressed tablets consisting of polyethylene glycol (PEG) 6000 as a carrier, drug and MgO (alkalizer). Telmisartan (TEL), an ionizable poorly water-soluble drug, was chosen as a model drug. The changes in physicochemical factors such as the dissolution rate, drug crystallinity, microenvironmental pH (pH(M)) and intermolecular interactions of the pSD and the tablets were investigated over 3 months under different temperature and relative humidity (RH) conditions: refrigerator (5-8 °C), 25 °C/32% RH, 25 °C/55% RH, 25 °C/75% RH, 40°C/32% RH, 40 °C/55% RH, and 40 °C/75% RH. Differential scanning calorimetry (DSC) analysis of all samples revealed no distinct changes in the drug melting point. In contrast, powder X-ray diffraction (PXRD) diffractograms revealed that samples stored at 40 °C/75% RH for 1 month, 25 °C/75% RH for 3 months and 40 °C at all humidity conditions for 3 months showed gradual recrystallization of the drug. Fourier transform infrared (FTIR) spectra indicated a reduced intensity of intermolecular interactions between TEL and MgO in the pSD and tablet. The pH(M) also gradually decreased. These altered physicochemical factors under the stressed conditions resulted in decreased dissolution profiles in intestinal fluid (pH 6.8). In contrast, the dissolution rate in gastric fluid (pH 1.2) was almost unchanged because of the high intrinsic solubility of TEL at this pH. Copyright © 2011 Elsevier B.V. All rights reserved.

  11. Solid dispersion of dutasteride using the solvent evaporation method: Approaches to improve dissolution rate and oral bioavailability in rats.

    Science.gov (United States)

    Choi, Jin-Seok; Lee, Sang-Eun; Jang, Woo Suk; Byeon, Jong Chan; Park, Jeong-Sook

    2018-09-01

    The aim of this study was to develop a dutasteride (DUT) solid dispersion (SD) using hydrophilic substances to enhance its dissolution (%) and oral bioavailability in rats. DUT-SD formulations were prepared with various co-polymers using a solvent evaporation method. The physical properties of DUT-SD formulations were confirmed using field emission scanning electron microscopy (FE-SEM), differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), and attenuated total reflectance Fourier transform infrared (ATR-FT-IR) spectroscopy. The toxicity and oral bioavailability of DUT-SD formulations were evaluated. Tocopheryl polyethylene glycol-1000-succinate (TPGS) was chosen as the solubilizer; and methylene chloride, and Aerosil® 200 or microcrystalline cellulose (MCC) were chosen as the solvent and carrier, respectively, based on a solubility test and pre-dissolution study. The dissolution levels of DUT-SD formulations were 86.3 ± 2.3% (F15) and 95.1 ± 1.9% (F16) after 1 h, which were higher than those of the commercial product, i.e., Avodart® (75.8 ± 1.5%) in 0.1 N HCl containing 1% (w/v) sodium lauryl sulfate (SLS). The F16 formulation was found to be stable, after assessing its dissolution (%) and drug content (%) for 6 months. The DUT-SD formulations resulted in relative bioavailability (BA) values of 126.4% (F15) and 132.1% (F16), which were enhanced compared to that of Avodart®. Dissolution (%) and relative BA values were both increased by hydrogen interaction between TPGS and DUT. This study might contribute to a new formulation (powder) whose oral bioavailability is greater than that of Avodart® (soft capsule), which could facilitate to the use of the SD system during the production process. Copyright © 2018 Elsevier B.V. All rights reserved.

  12. Ultrasonic techniques for the in situ characterisation of 'legacy' Waste sludges and dispersions - 59111

    International Nuclear Information System (INIS)

    Hunter, Timothy; Biggs, Simon; Young, James; Fairweather, Michael; Peakall, Jeff

    2012-01-01

    Research being undertaken at the University of Leeds, as part of the DIAMOND university consortium, is exploring the effectiveness of various ultrasonic technologies as in situ probes to characterize and monitor nuclear waste slurries, such as the 'Legacy' Magnesium hydroxide sludges found in Sellafield, U.K. Through use of a commercial Acoustic Backscatter Sensor (ABS) with 1 - 5 MHz transducers, various properties of free-settling oxide simulant sludges were determined. Work was focused upon characterizing essentially 'static' sludges (to give prospective use as tools for the wastes in current deposits); although, the sensors also have potential as dispersion monitors during any future processing and storage of the Legacy wastes, as well as many other storage, clarifier or thickener systems across a wide range of industrial processing operations. ABS data of mixed glass powder dispersions was analysed and compared to scattering theory, to understand the correlations between acoustic attenuation and particulate concentration. The ABS was also calibrated to measure changes in average particulate concentration within a settling suspension over time, and showed the depth-wise segregation of the dispersion through the settling column at different particular time intervals. It was found that observed hindered settling also led to an increase in particulate concentration over the sludge zone and significant segregation occurred at moderate time intervals, due to the broad size distribution of the aggregates measured. It is hoped in future that these sensors may be able to be fitted to robotic handlers that have been installed onsite (and previously used for sampling), allowing fully automatic in situ sludge analysis. (authors)

  13. Analysis of Atorvastatin in Commercial Solid Drugs using the TT-PIGE Technique

    International Nuclear Information System (INIS)

    Younes, G; Zahraman, K; Nsouli, B; Bejjani, A; Mahmoud, R; El-Yazbi, F

    2008-01-01

    The quantification of the active ingredient (Al) in drugs is a crucial and important step in the drug quality control process. This is usually performed by using wet chemical techniques like LC-MS, UV spectrophotometry and other appropriate organic analytical methods. In the case of an active ingredient contains specific heteroatoms (F, S, Cl), elemental IBA techniques can be explored for molecular quantification. IBA techniques permit the analysis of the sample under solid form, without any laborious sample preparations. This is an advantage when the number of sample is relatively large. In this work, we demonstrate the ability of the Thick Target PIGE technique for rapid and accurate quantification of low concentration AtorvastatinTM in three commercial anti-hyperlipidemic drugs (Lipitor, Liponorm and Storvas). (author)

  14. Analysis of Atorvastatin in Commercial Solid Drugs using the TT-PIGE Technique

    Energy Technology Data Exchange (ETDEWEB)

    Younes, G [Beirut Arab University, Faculty of Science, Chemistry Department Beirut (Lebanon); Zahraman, K; Nsouli, B; Bejjani, A [Lebanese Atomic Energy Commission, National Council for Scientific Research, Beirut (Lebanon); Mahmoud, R; El-Yazbi, F [Beirut Arab University, Faculty of Pharmacy, Department of Pharmaceutical and Analytical Chemistry, Beirut (Lebanon)

    2008-07-01

    The quantification of the active ingredient (Al) in drugs is a crucial and important step in the drug quality control process. This is usually performed by using wet chemical techniques like LC-MS, UV spectrophotometry and other appropriate organic analytical methods. In the case of an active ingredient contains specific heteroatoms (F, S, Cl), elemental IBA techniques can be explored for molecular quantification. IBA techniques permit the analysis of the sample under solid form, without any laborious sample preparations. This is an advantage when the number of sample is relatively large. In this work, we demonstrate the ability of the Thick Target PIGE technique for rapid and accurate quantification of low concentration AtorvastatinTM in three commercial anti-hyperlipidemic drugs (Lipitor, Liponorm and Storvas). (author)

  15. Determination of heavy metals at traces level in leached samples by energy dispersive x-ray fluorescence technique

    International Nuclear Information System (INIS)

    Simabuco, Silvana M.; Nascimento Filho, Virgilio F. do; Inacio, Graziela R.; Navarro, Angela N.

    1996-01-01

    In landfill solid residues are disposed in the soil. When made based on technical criteria and specifically operation patterns a safe confinement is warranted according to environmental and public health protection. However, when the disposal is made by a random and unsuitable way serious problems can be caused as groundwater and superficial water contamination through leach action, indicating the usefulness of monitoring landfills. In this way energy dispersive X-ray fluorescence analysis with radioisotopic excitation was applied to evaluate the concentrations of heavy metals at trace levels in leached samples from the Americana City Landfill with pre-concentration of the elements by a non-specific precipitating agent, called ammonium pyrrolidine dithiocarbamate (APDC). (author)

  16. A novel osmotic pump-based controlled delivery system consisting of pH-modulated solid dispersion for poorly soluble drug flurbiprofen: in vitro and in vivo evaluation.

    Science.gov (United States)

    Li, Shujuan; Wang, Xiaoyu; Wang, Yingying; Zhao, Qianqian; Zhang, Lina; Yang, Xinggang; Liu, Dandan; Pan, Weisan

    2015-01-01

    In this study, a novel controlled release osmotic pump capsule consisting of pH-modulated solid dispersion for poorly soluble drug flurbiprofen (FP) was developed to improve the solubility and oral bioavailability of FP and to minimize the fluctuation of plasma concentration. The pH-modulated solid dispersion containing FP, Kollidon® 12 PF and Na2CO3 at a weight ratio of 1/4.5/0.02 was prepared using the solvent evaporation method. The osmotic pump capsule was assembled by semi-permeable capsule shell of cellulose acetate (CA) prepared by the perfusion method. Then, the solid dispersion, penetration enhancer, and suspending agents were tableted and filled into the capsule. Central composite design-response surface methodology was used to evaluate the influence of factors on the responses. A second-order polynomial model and a multiple linear model were fitted to correlation coefficient of drug release profile and ultimate cumulative release in 12 h, respectively. The actual response values were in good accordance with the predicted ones. The optimized formulation showed a complete drug delivery and zero-order release rate. Beagle dogs were used to be conducted in the pharmacokinetic study. The in vivo study indicated that the relative bioavailability of the novel osmotic pump system was 133.99% compared with the commercial preparation. The novel controlled delivery system with combination of pH-modulated solid dispersion and osmotic pump system is not only a promising strategy to improve the solubility and oral bioavailability of poorly soluble ionizable drugs but also an effective way to reduce dosing frequency and minimize the plasma fluctuation.

  17. Importance of in vitro dissolution conditions for the in vivo predictability of an amorphous solid dispersion containing a pH-sensitive carrier

    DEFF Research Database (Denmark)

    Wendelboe, Johan; Knopp, Matthias Manne; Khan, Fauzan

    2017-01-01

    as a carrier in amorphous solid dispersions of CCX. In vitro-in vivo correlation demonstrated that the in vitro data obtained in FaSSIF pH 7.4 was more predictive for the in vivo performance than that obtained in FaSSIF pH 6.5. Consequently, the findings of this study underline that when predicting the in vivo...

  18. Soluplus®/TPGS-based solid dispersions prepared by hot-melt extrusion equipped with twin-screw systems for enhancing oral bioavailability of valsartan.

    Science.gov (United States)

    Lee, Jae-Young; Kang, Wie-Soo; Piao, Jingpei; Yoon, In-Soo; Kim, Dae-Duk; Cho, Hyun-Jong

    2015-01-01

    Soluplus(®) (SP) and D-alpha-tocopherol polyethylene glycol 1000 succinate (TPGS)-based solid dispersion (SD) formulations were developed by hot-melt extrusion (HME) to improve oral bioavailability of valsartan (VST). HME process with twin-screw configuration for generating a high shear stress was used to prepare VST SD formulations. The thermodynamic state of the drug and its dispersion in the polymers were evaluated by solid-state studies, including Fourier-transform infrared, X-ray diffraction, and differential scanning calorimetry. Drug release from the SD formulations was assessed at pH values of 1.2, 4.0, and 6.8. Pharmacokinetic study was performed in rats to estimate the oral absorption of VST. HME with a high shear rate produced by the twin-screw system was successfully applied to prepare VST-loaded SD formulations. Drug amorphization and its molecular dispersion in the polymer matrix were verified by several solid-state studies. Drug release from SD formulations was improved, compared to the pure drug, particularly at pH 6.8. Oral absorption of drug in rats was also enhanced in SP and TPGS-based SD groups compared to that in the pure drug group. SP and TPGS-based SDs, prepared by the HME process, could be used to improve aqueous solubility, dissolution, and oral absorption of poorly water-soluble drugs.

  19. 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.

  20. A study of preparation techniques and properties of bulk nanocomposites based on aqueous albumin dispersion

    Science.gov (United States)

    Gerasimenko, A. Yu.; Dedkova, A. A.; Ichkitidze, L. P.; Podgaetskii, V. M.; Selishchev, S. V.

    2013-08-01

    Bulk nanocomposites prepared from an aqueous albumin dispersion with carbon nanotubes by removing the liquid component from the dispersion have been investigated. The composites were obtained by thermostating and exposure to LED and IR diode laser radiation. The nanocomposites obtained under laser irradiation retain their shape and properties for several years, in contrast to the composites fabricated in different ways (which decompose into small fragments immediately after preparation). The low density of the composites under study (˜1200 kg/m3), which is close to the density of water, is due to their high porosity. The hardness of stable nanocomposites (˜300 MPa) was found to be at the same level as the hardness of polymethylmethacrylate, aluminum, and iron and close to the hardness of human bone tissue. The cluster quasiordering of the inner structure of nanocomposites revealed by atomic force microscopy indicates the possibility of forming a bulk nanotube framework in them, which can be caused by the effect of the electric field of laser radiation and ensure their stability and hardness. The presence of a framework in nanocomposites provides conditions for self-assembly of biological tissues and makes it possible to apply laser-prepared nanocomposites as a component of surgical implants.

  1. Use of the co-grinding method to enhance the dissolution behavior of a poorly water-soluble drug: generation of solvent-free drug-polymer solid dispersions.

    Science.gov (United States)

    Yang, Caiqin; Xu, Xiujuan; Wang, Jing; An, Zhiqian

    2012-01-01

    The solid dispersion (SD) technique is the most effective method for improving the dissolution rate of poorly water-soluble drugs. In the present work, SDs of the Ca2+ channel blocker dipfluzine (DF) with polyvinylpyrrolidone K30 (PVP) and poloxamer 188 (PLXM) were prepared by the powder solid co-grinding method under a solvent-free condition. The properties of all SDs and physical mixtures were investigated by X-ray diffraction, Fourier-transform infrared, differential scanning calorimetry, scanning electron microscopy, dissolution test, and particles size determination. Eutectic compounds were produced between the DF and PLXM matrix during the co-grinding process, whereas glass suspension formed in the SDs with PVP carrier. Hydrogen bond formation was not observed between DF and carriers and DF was microcrystalline state in the PVP and PLXM matrices. The solubility of DF in different concentration of carriers at 25, 31, and 37°C was investigated; the values obtained were used to calculate the thermodynamic parameters of interaction between DF and carriers. The Gibbs free energy (ΔrGθ) values were negative, indicating the spontaneous nature of dispersing DF into the carriers. Moreover, entropy is the drive force when DF disperses into the matrix of PVP, while, enthalpy-driven dispersing encounters in the PLXM carrier. All the SDs of DF/carriers showed a considerably higher dissolution rate than pure DF and the corresponding physical mixtures. The cumulative dissolution rate at 10 min of the SD with a 1 : 3 DF/carrier ratio increased 5.1-fold for PVP and 5.5-fold for PLXM.

  2. Characterization of sediments laid on Solimoes/Amazonas river flood plains, using energy dispersive X-ray fluorescence technique

    International Nuclear Information System (INIS)

    Carneiro, Ana E.V.; Nascimento Filho, Virgilio F. do

    1997-01-01

    This paper proposes sediment analysis with high light elements fraction using dispersive energy X-ray fluorescence technique with radioisotopic excitation, The proposed procedure is based on the Fundamental Parameters for analytical elements (Z ≥ 13) evaluation, and coherent and incoherent scattered radiation for quantification of the light fraction of the matrix (Z < 13). Laid sediments samples on Solimoes/Amazonas river flood plains were analyzed, determining simultaneously the Al, Si, K, Ca, Ti, Fe, Sc, V, Mn, Cu, Zn, Rb, Sr and Zr element concentrations, thus allowing chemical characterization and spatial variability, and some mineralogical and weathering sediments aspects. (author). 15 refs., 11 tabs

  3. Novel method for the production of spin-aligned RI beams in projectile fragmentation reaction with the dispersion matching technique

    Energy Technology Data Exchange (ETDEWEB)

    Ichikawa, Y., E-mail: yuichikawa@phys.titech.ac.jp [Tokyo Institute of Technology, Department of Physics (Japan); Ueno, H. [RIKEN Nishina Center (Japan); Ishii, Y. [Tokyo Institute of Technology, Department of Physics (Japan); Furukawa, T. [Tokyo Metropolitan University, Department of Physics (Japan); Yoshimi, A. [Okayama University, Research Core for Extreme Quantum World (Japan); Kameda, D.; Watanabe, H.; Aoi, N. [RIKEN Nishina Center (Japan); Asahi, K. [Tokyo Institute of Technology, Department of Physics (Japan); Balabanski, D. L. [Bulgarian Academy of Sciences, Institute for Nuclear Research and Nuclear Energy (Bulgaria); Chevrier, R.; Daugas, J. M. [CEA, DAM, DIF (France); Fukuda, N. [RIKEN Nishina Center (Japan); Georgiev, G. [CSNSM, IN2P3-CNRS, Universite Paris-sud (France); Hayashi, H.; Iijima, H. [Tokyo Institute of Technology, Department of Physics (Japan); Inabe, N. [RIKEN Nishina Center (Japan); Inoue, T. [Tokyo Institute of Technology, Department of Physics (Japan); Ishihara, M.; Kubo, T. [RIKEN Nishina Center (Japan); and others

    2013-05-15

    A novel method to produce spin-aligned rare-isotope (RI) beam has been developed, that is the two-step projectile fragmentation method with a technique of dispersion matching. The present method was verified in an experiment at the RIKEN RIBF, where an RI beam of {sup 32}Al with spin alignment of 8(1) % was successfully produced from a primary beam of {sup 48}Ca, with {sup 33}Al as an intermediate nucleus. Figure of merit of the present method was found to be improved by a factor larger than 50 compared with a conventional method employing single-step projectile fragmentation.

  4. Optical transmission testing based on asynchronous sampling techniques: images analysis containing chromatic dispersion using convolutional neural network

    Science.gov (United States)

    Mrozek, T.; Perlicki, K.; Tajmajer, T.; Wasilewski, P.

    2017-08-01

    The article presents an image analysis method, obtained from an asynchronous delay tap sampling (ADTS) technique, which is used for simultaneous monitoring of various impairments occurring in the physical layer of the optical network. The ADTS method enables the visualization of the optical signal in the form of characteristics (so called phase portraits) that change their shape under the influence of impairments such as chromatic dispersion, polarization mode dispersion and ASE noise. Using this method, a simulation model was built with OptSim 4.0. After the simulation study, data were obtained in the form of images that were further analyzed using the convolutional neural network algorithm. The main goal of the study was to train a convolutional neural network to recognize the selected impairment (distortion); then to test its accuracy and estimate the impairment for the selected set of test images. The input data consisted of processed binary images in the form of two-dimensional matrices, with the position of the pixel. This article focuses only on the analysis of images containing chromatic dispersion.

  5. Observation of the dispersion of wedge waves propagating along cylinder wedge with different truncations by laser ultrasound technique

    Science.gov (United States)

    Jia, Jing; Zhang, Yu; Han, Qingbang; Jing, Xueping

    2017-10-01

    The research focuses on study the influence of truncations on the dispersion of wedge waves propagating along cylinder wedge with different truncations by using the laser ultrasound technique. The wedge waveguide models with different truncations were built by using finite element method (FEM). The dispersion curves were obtained by using 2D Fourier transformation method. Multiple mode wedge waves were observed, which was well agreed with the results estimated from Lagasse's empirical formula. We established cylinder wedge with radius of 3mm, 20° and 60°angle, with 0μm, 5μm, 10μm, 20μm, 30μm, 40μm, and 50μm truncations, respectively. It was found that non-ideal wedge tip caused abnormal dispersion of the mode of cylinder wedge, the modes of 20° cylinder wedge presents the characteristics of guide waves which propagating along hollow cylinder as the truncation increasing. Meanwhile, the modes of 60° cylinder wedge with truncations appears the characteristics of guide waves propagating along hollow cylinder, and its mode are observed clearly. The study can be used to evaluate and detect wedge structure.

  6. Étude de la technique d'échange ionique avec compétition. Cas du dépôt de platine sur support solide acide par échange cationique Research on the Ion Exchange Technique with Competition. Case of Platinum Deposit on a Solid Acid Support by Cation Exchange

    Directory of Open Access Journals (Sweden)

    Ribeiro F.

    2006-11-01

    Full Text Available Cet article présente une étude détaillée de la technique de dépôt de platine sur support acide par échange cationique avec compétition. Cette technique permet d'obtenir à la fois une dispersion quasi atomique et une répartition macroscopique homogène du métal sur la surface du solide. En l'absence de limitations diffusionnelles extra-granulaires, les résultats expérimentaux sont en bon accord avec les prévisions théoriques . This article is a detailed examination of the technique of depositing platinum on an acid support by cation exchange with compétition. This technique produces both a quasi-atomic dispersion and a homogeneous macroscopic distribution of the métal onthe surface of the solid. In the absence of extragranular diffusion limitations, experimental findings are in good agreement with theoretical predictions.

  7. Localisation and identification of radioactive particles in solid samples by means of a nuclear track technique

    International Nuclear Information System (INIS)

    Boehnke, Antje; Treutler, Hanns-Christian; Freyer, Klaus; Schubert, Michael; Holger Weiss

    2005-01-01

    This study is aimed to develop a generally applicable methodology of investigation that can be used for the localisation of single alpha-active particles in solid samples, such as industrial dust or natural soils, sediments and rocks by autoradiography using solid-state nuclear track detectors. The developed technique allows the detection of local enrichments of alpha-emitters in any solid material. The results of such an investigation are of interest from technical, biological and environmental points of view. The idea behind the methodology is to locate the position of alpha-active spots in a sample by attaching the track detector to the sample in a defined manner, thoroughly described in the paper. The located alpha-active particles are subsequently analysed by an electron microscope and an electron microprobe. An example of the application of this methodology is also given. An ultra-fine -grained ore-processing residue, which causes serious environmental pollution in the respective mining district and thus limits possible land use and affects quality of life in the area, was examined using the described technique. The investigation revealed considerable amounts of alpha-active particles in this material

  8. Characterization and evaluation of 5-fluorouracil-loaded solid lipid nanoparticles prepared via a temperature-modulated solidification technique.

    Science.gov (United States)

    Patel, Meghavi N; Lakkadwala, Sushant; Majrad, Mohamed S; Injeti, Elisha R; Gollmer, Steven M; Shah, Zahoor A; Boddu, Sai Hanuman Sagar; Nesamony, Jerry

    2014-12-01

    The aim of this research was to advance solid lipid nanoparticle (SLN) preparation methodology by preparing glyceryl monostearate (GMS) nanoparticles using a temperature-modulated solidification process. The technique was reproducible and prepared nanoparticles without the need of organic solvents. An anticancer agent, 5-fluorouracil (5-FU), was incorporated in the SLNs. The SLNs were characterized by particle size analysis, zeta potential analysis, differential scanning calorimetry (DSC), infrared spectroscopy, atomic force microscopy (AFM), transmission electron microscopy (TEM), drug encapsulation efficiency, in vitro drug release, and in vitro cell viability studies. Particle size of the SLN dispersion was below 100 nm, and that of redispersed lyophilizates was ~500 nm. DSC and infrared spectroscopy suggested that the degree of crystallinity did not decrease appreciably when compared to GMS. TEM and AFM images showed well-defined spherical to oval particles. The drug encapsulation efficiency was found to be approximately 46%. In vitro drug release studies showed that 80% of the encapsulated drug was released within 1 h. In vitro cell cultures were biocompatible with blank SLNs but demonstrated concentration-dependent changes in cell viability to 5-FU-loaded SLNs. The 5-FU-loaded SLNs can potentially be utilized in an anticancer drug delivery system.

  9. Polypyrrole/magnetic nanoparticles composite as an efficient sorbent for dispersive micro-solid-phase extraction of antidepressant drugs from biological fluids.

    Science.gov (United States)

    Asgharinezhad, Ali Akbar; Karami, Sara; Ebrahimzadeh, Homeira; Shekari, Nafiseh; Jalilian, Niloofar

    2015-10-15

    In this study, polypyrrole/magnetic nanoparticles composites in the presence of two different dopants were synthesized with the aid of chemical oxidative polymerization process for dispersive-μ-solid phase extraction (D-μ-SPE). The synthesized magnetic sorbents were characterized by various techniques. The results exhibited that the nanocomposite modified by polypyrrole with sodium perchlorate as a dopant demonstrated higher extraction efficiency for citalopram (CIT) and sertraline (STR) as the model compounds. This nanosorbent in combination with high performance liquid chromatography-UV detection was applied for extraction, preconcentration and determination of CIT and STR in urine and plasma samples. The effect of various parameters on the extraction efficiency including: sample pH, amount of sorbent, sorption time, eluent and its volume, salt content, and elution time were investigated and optimized. The opted conditions were: sample pH, 9.0; sorbent dosage, 10mg; sorption time, 7 min; elution solvent and its volume, 0.06 mol L(-1) HCl in methanol, 120 μL; elution time, 2 min and without addition of salt to the sample. The calibration curves were linear in the concentration range of 1-800 μg L(-1). The limits of detection (LODs) were obtained in the range of 0.2-1.0 μg L(-1) for CIT and 0.3-0.7 μg L(-1) for STR, respectively. The percent of extraction recoveries and relative standard deviations (n=5) were in the range of 93.4-99, 4.8-8.4 for CIT and 94-98.4, 4.3-9.2 for STR, respectively. Finally, the applicability of the method was successfully confirmed by the extraction and determination of CIT and STR in human urine and plasma samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Aspects and application of etch-pit technique in the distribution detection of uranium in solids

    International Nuclear Information System (INIS)

    Sachett, I.A.

    1973-01-01

    Some aspects related to the use of standard glass microscope slide as solid state track detector are presented, as well as studies of measurement of distribution of uranium in various solids determined by means of this technique. The behavior of the various parameters related to the properties of the detector and the results of their measurements are treated. Results obtained on the determination of distribution of uranium in samples of fuel elements of the 'ARGONAUTA' research reactor of Instituto de Engenharia Nuclear - Rio de Janeiro, are included. The samples were taken from the fuel-cladding interface. Finally, some data on levels of contamination of the laboratory equipment in use by uranium during the course of this work are presented [pt

  11. Fast Measurement of Soluble Solid Content in Mango Based on Visible and Infrared Spectroscopy Technique

    Science.gov (United States)

    Yu, Jiajia; He, Yong

    Mango is a kind of popular tropical fruit, and the soluble solid content is an important in this study visible and short-wave near-infrared spectroscopy (VIS/SWNIR) technique was applied. For sake of investigating the feasibility of using VIS/SWNIR spectroscopy to measure the soluble solid content in mango, and validating the performance of selected sensitive bands, for the calibration set was formed by 135 mango samples, while the remaining 45 mango samples for the prediction set. The combination of partial least squares and backpropagation artificial neural networks (PLS-BP) was used to calculate the prediction model based on raw spectrum data. Based on PLS-BP, the determination coefficient for prediction (Rp) was 0.757 and root mean square and the process is simple and easy to operate. Compared with the Partial least squares (PLS) result, the performance of PLS-BP is better.

  12. Probing the mechanisms of drug release from amorphous solid dispersions in medium-soluble and medium-insoluble carriers.

    Science.gov (United States)

    Sun, Dajun D; Lee, Ping I

    2015-08-10

    The objective of the current study is to mechanistically differentiate the dissolution and supersaturation behaviors of amorphous drugs from amorphous solid dispersions (ASDs) based on medium-soluble versus medium-insoluble carriers under nonsink dissolution conditions through a direct head-to-head comparison. ASDs of indomethacin (IND) were prepared in several polymers which exhibit different solubility behaviors in acidic (pH1.2) and basic (pH7.4) dissolution media. The selected polymers range from water-soluble (e.g., PVP and Soluplus) and water-insoluble (e.g., ethylcellulose and Eudragit RL PO) to those only soluble in an acidic or basic dissolution medium (e.g., Eudragit E100, Eudragit L100, and HPMCAS). At 20wt.% drug loading, DSC and powder XRD analysis confirmed that the majority of incorporated IND was present in an amorphous state. Our nonsink dissolution results confirm that whether the carrier matrix is medium soluble determines the release mechanism of amorphous drugs from ASD systems which has a direct impact on the rate of supersaturation generation, thus in turn affecting the evolution of supersaturation in amorphous systems. For example, under nonsink dissolution conditions, the release of amorphous IND from medium-soluble carriers is governed by a dissolution-controlled mechanism leading to an initial surge of supersaturation followed by a sharp decline in drug concentration due to rapid nucleation and crystallization. In contrast, the dissolution of IND ASD from medium-insoluble carriers is more gradual as drug release is regulated by a diffusion-controlled mechanism by which drug supersaturation is built up gradually and sustained over an extended period of time without any apparent decline. Since several tested carrier polymers can be switched from soluble to insoluble by simply changing the pH of the dissolution medium, the results obtained here provide unequivocal evidence of the proposed transition of kinetic solubility profiles from the

  13. A study of radionuclide dispersion by river systems, using GIS and remote sensing techniques

    International Nuclear Information System (INIS)

    Borghuis, Sander; Brown, Justin; Steenhuisen, Frits; Skorve, Johnny

    2000-01-01

    The Krasnoyarsk Mining and Chemical Combine in Zheleznogorsk, Russia, is situated on the banks of the Yenisey river. The combine consists of three RBMK-type graphite moderate reactors, a reprocessing plant for the production of weapons-grade plutonium and storage facilities for nuclear waste. Discharges of radionuclides into the Yenisey river were either part of normal operation procedures or caused by accidental releases (Strand et al., 1997). So far, little is known about the transport and fate of the radioactive contaminants in the areas downstream of the Krasnoyarsk CC that are influenced by the Yenisey river system. Aim is to comprehend the dispersion of radionuclides through the river system. Remotely sensed and field study information are combined in a geographical information system (GIS) to study the processes leading to the dispersion of sediment-bound radionuclides carried by the river system. Since the extent of the study area is several thousands or kilometres of river and adjacent flood plains, use is made of a record of remotely sensed (satellite) images that are handled by the GIS. Panchromatic, high resolution satellite images as well as multispectral Landsat MSS and TM images were compiled for the area of interest. The panchromatic images were taken in a period during which the facility was in operation (1960-1972) and obtained for intervals of circa 6 months. A time series of satellite images enables the identification of erosion and sedimentation zones. The behaviour and fate of particle-reactive radionuclides, e.g. 239,240 Pu and to large extent 137 Cs, will be closely related to the movement of sediment. With respect to the behaviour and fate of more conservative radionuclides as 90 Sr, information is required accounting for fractionation between the particulate and aqueous phases. Stereo images are used to comprehend the geomorphology of the Yenisey river systems, focused on classification of sedimentary deposits. Landsat MSS and TM with five

  14. Application of energy dispersive X-ray fluorescent technique in the pollution study of water

    Energy Technology Data Exchange (ETDEWEB)

    Htun, Kyi

    1993-03-01

    The abundance of major trace elements in water in the surface well, tube well, lake and river were measured. The technique outlined here is very useful in the study of the pollution of environmental radioactivity. For the above measurements the Si(Li) X-ray detection system was used in conjunction with a personal computer

  15. Complementary techniques for solid oxide cell characterisation on micro- and nano-scale

    International Nuclear Information System (INIS)

    Wiedenmann, D.; Hauch, A.; Grobety, B.; Mogensen, M.; Vogt, U.

    2009-01-01

    High temperature steam electrolysis by solid oxide electrolysis cells (SOEC) is a way with great potential to transform clean and renewable energy from non-fossil sources to synthetic fuels such as hydrogen, methane or dimethyl ether, which have been identified as promising alternative energy carriers. Also, as SOEC can operate in the reverse mode as solid oxide fuel cells (SOFC), during high peak hours e.g. hydrogen can be used in a very efficient way to reconvert chemically stored energy into electrical energy. As solid oxide cells (SOC) are working at high temperatures (700-900 o C), material degradation and evaporation can occur e.g. from the cell sealing material, leading to poisoning effects and aging mechanisms which are decreasing the cell efficiency and long-term durability. In order to investigate such cell degradation processes, thorough examination on SOC often requires the chemical and structural characterisation on the microscopic and the nanoscopic level. The combination of different microscope techniques like conventional scanning electron microscopy (SEM), electron-probe microanalysis (EPMA) and the focused ion-beam (FIB) preparation technique for transmission electron microscopy (TEM) allows performing post mortem analysis on a multi scale level of cells after testing. These complementary techniques can be used to characterize structural and chemical changes over a large and representative sample area (micro-scale) on the one hand, and also on the nano-scale level for selected sample details on the other hand. This article presents a methodical approach for the structural and chemical characterisation of changes in aged cathode-supported electrolysis cells produced at Riso DTU, Denmark. Also, results from the characterisation of impurities at the electrolyte/hydrogen interface caused by evaporation from sealing material are discussed. (author)

  16. Simulation technique for slurries interacting with moving parts and deformable solids with applications

    Science.gov (United States)

    Mutabaruka, Patrick; Kamrin, Ken

    2018-04-01

    A numerical method for particle-laden fluids interacting with a deformable solid domain and mobile rigid parts is proposed and implemented in a full engineering system. The fluid domain is modeled with a lattice Boltzmann representation, the particles and rigid parts are modeled with a discrete element representation, and the deformable solid domain is modeled using a Lagrangian mesh. The main issue of this work, since separately each of these methods is a mature tool, is to develop coupling and model-reduction approaches in order to efficiently simulate coupled problems of this nature, as in various geological and engineering applications. The lattice Boltzmann method incorporates a large eddy simulation technique using the Smagorinsky turbulence model. The discrete element method incorporates spherical and polyhedral particles for stiff contact interactions. A neo-Hookean hyperelastic model is used for the deformable solid. We provide a detailed description of how to couple the three solvers within a unified algorithm. The technique we propose for rubber modeling/coupling exploits a simplification that prevents having to solve a finite-element problem at each time step. We also developed a technique to reduce the domain size of the full system by replacing certain zones with quasi-analytic solutions, which act as effective boundary conditions for the lattice Boltzmann method. The major ingredients of the routine are separately validated. To demonstrate the coupled method in full, we simulate slurry flows in two kinds of piston valve geometries. The dynamics of the valve and slurry are studied and reported over a large range of input parameters.

  17. 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.

  18. 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.

  19. Sardine (Sardina pilchardus) larval dispersal in the Iberian upwelling system, using coupled biophysical techniques

    Science.gov (United States)

    Santos, A. M. P.; Nieblas, A.-E.; Verley, P.; Teles-Machado, A.; Bonhommeau, S.; Lett, C.; Garrido, S.; Peliz, A.

    2018-03-01

    The European sardine (Sardina pilchardus) is the most important small pelagic fishery of the Western Iberia Upwelling Ecosystem (WIUE). Recently, recruitment of this species has declined due to changing environmental conditions. Furthermore, controversies exist regarding its population structure with barriers thought to exist between the Atlantic-Iberian Peninsula, Northern Africa, and the Mediterranean. Few studies have investigated the transport and dispersal of sardine eggs and larvae off Iberia and the subsequent impact on larval recruitment variability. Here, we examine these issues using a Regional Ocean Modeling System climatology (1989-2008) coupled to the Lagrangian transport model, Ichthyop. Using biological parameters from the literature, we conduct simulations that investigate the effects of spawning patchiness, diel vertical migration behaviors, and egg buoyancy on the transport and recruitment of virtual sardine ichthyoplankton on the continental shelf. We find that release area, release depth, and month of release all significantly affect recruitment. Patchiness has no effect and diel vertical migration causes slightly lower recruitment. Egg buoyancy effects are significant and act similarly to depth of release. As with other studies, we find that recruitment peaks vary by latitude, explained here by the seasonal variability of offshore transport. We find weak, continuous alongshore transport between release areas, though a large proportion of simulated ichthyoplankton transport north to the Cantabrian coast (up to 27%). We also show low level transport into Morocco (up to 1%) and the Mediterranean (up to 8%). The high proportion of local retention and low but consistent alongshore transport supports the idea of a series of metapopulations along this coast.

  20. 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

  1. Conductivity enhancement in K{sup +}-ion conducting dry Solid Polymer Electrolyte (SPE): [PEO: KNO{sub 3}]: A consequence of KI dispersal and nano-ionic effect

    Energy Technology Data Exchange (ETDEWEB)

    Kesharwani, Priyanka; Sahu, Dinesh K.; Mahipal, Y.K.; Agrawal, R.C., E-mail: rakesh_c_agrawal@yahoo.co.in

    2017-06-01

    Solid–State batteries. Ion transport behaviour has been characterized in terms of ionic conductivity (σ), total ionic (t{sub ion}) and cation (t{sub +}) transference numbers, evaluated using different ac/dc techniques. Temperature dependent conductivity measurements have also been done to compute activation energy (E{sub a}) value by linear least square fitting of respective ‘log σ -1/T’ plots. Materials characterization vis-a-vis complexation of salt in polymeric host has been confirmed by SEM/XRD/FTIR/DSC analysis. - Highlights: • Non-lithium chemical based SPE films: [95PEO:5KNO{sub 3}] & [70PEO:30KNO{sub 3}] investigated. • Substantial enhancement in σ{sub rt} and t{sub +} achieved adopting two approaches. • As first approach, CPEs prepared dispersing IInd-phase active filler into Ist-phase SPE. • As second approach, Nano–ionic effect introduced by ball milling prior to casting CPE film. • Dry polymer electrolytes can be used for All-Solid-State battery applications.

  2. Amorphization of thiamine chloride hydrochloride: A study of the crystallization inhibitor properties of different polymers in thiamine chloride hydrochloride amorphous solid dispersions.

    Science.gov (United States)

    Arioglu-Tuncil, Seda; Bhardwaj, Vivekanand; Taylor, Lynne S; Mauer, Lisa J

    2017-09-01

    Amorphous solid dispersions of thiamine chloride hydrochloride (THCl) were created using a variety of polymers with different physicochemical properties in order to investigate how effective the various polymers were as THCl crystallization inhibitors. THCl:polymer dispersions were prepared by lyophilizing solutions of THCl and amorphous polymers (guar gum, pectin, κ-carrageenan, gelatin, and polyvinylpyrrolidone (PVP)). These dispersions were stored at select temperature (25 and 40°C) and relative humidity (0, 23, 32, 54, 75, and 85% RH) conditions and monitored at different time points using powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), and differential scanning calorimetry (DSC). Moisture sorption isotherms of all samples were also obtained. Initially amorphous THCl was produced in the presence of ≥40% w/w pectin, κ-carrageenan, gelatin, and guar gum or ≥60% w/w PVP. Trends in polymer THCl crystallization inhibition (pectin≥κ-carrageenan>gelatin>guar gum≫PVP) were primarily based on the ability of the polymer to interact with THCl via hydrogen bonding and/or ionic interactions. The onset of THCl crystallization from the amorphous dispersions was also related to storage conditions. THCl remained amorphous at low RH conditions (0 and 23% RH) in all 1:1 dispersions except THCl:PVP. THCl crystallized in some dispersions below the glass transition temperature (T g ) but remained amorphous in others at T~T g . At high RHs (75 and 85% RH), THCl crystallized within one day in all samples. Given the ease of THCl amorphization in the presence of a variety of polymers, even at higher vitamin concentrations than would be found in foods, it is likely that THCl is amorphous in many low moisture foods. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Atmospheric and dispersion modeling in areas of highly complex terrain employing a four-dimensional data assimilation technique

    International Nuclear Information System (INIS)

    Fast, J.D.; O'Steen, B.L.

    1994-01-01

    The results of this study indicate that the current data assimilation technique can have a positive impact on the mesoscale flow fields; however, care must be taken in its application to grids of relatively fine horizontal resolution. Continuous FDDA is a useful tool in producing high-resolution mesoscale analysis fields that can be used to (1) create a better initial conditions for mesoscale atmospheric models and (2) drive transport models for dispersion studies. While RAMS is capable of predicting the qualitative flow during this evening, additional experiments need to be performed to improve the prognostic forecasts made by RAMS and refine the FDDA procedure so that the overall errors are reduced even further. Despite the fact that a great deal of computational time is necessary in executing RAMS and LPDM in the configuration employed in this study, recent advances in workstations is making applications such as this more practical. As the speed of these machines increase in the next few years, it will become feasible to employ prognostic, three-dimensional mesoscale/transport models to routinely predict atmospheric dispersion of pollutants, even to highly complex terrain. For example, the version of RAMS in this study could be run in a ''nowcasting'' model that would continually assimilate local and regional observations as soon as they become available. The atmospheric physics in the model would be used to determine the wind field where no observations are available. The three-dimensional flow fields could be used as dynamic initial conditions for a model forecast. The output from this type of modeling system will have to be compared to existing diagnostic, mass-consistent models to determine whether the wind field and dispersion forecasts are significantly improved

  4. New metastable form of glibenclamide prepared by redispersion from ternary solid dispersions containing polyvinylpyrrolidone-K30 and sodium lauryl sulfate.

    Science.gov (United States)

    Thongnopkoon, Thanu; Puttipipatkhachorn, Satit

    2016-01-01

    Modification of polymorphic forms of poorly water-soluble drugs is one way to achieve the desirable properties. In this study, glibenclamide (GBM) particles with different polymorphic forms, including a new metastable form, were obtained from redispersion of ternary solid dispersion systems. The ternary solid dispersion systems, consisting of GBM, polyvinylpyrrolidone-K30 (PVP-K30) and sodium lauryl sulfate (SLS), were prepared by solvent evaporation method and subsequently redispersed in deionized water. The precipitated drug particles were then collected at a given time period. The drug particles with different polymorphic forms could be achieved depending on the polymer/surfactant ratio. Amorphous drug nanoparticles could be obtained by using a high polymer/surfactant ratio, whereas two different crystalline forms were obtained from the systems containing low polymer/surfactant ratios. Interestingly, a new metastable form IV of GBM with improved dissolution behavior could be obtained from the system of GBM:PVP-K30:SLS with the weight ratio of 2:2:4. This new polymorphic form IV of GBM was confirmed by differential scanning calorimetry (DSC), Fourier transform infrared (FT-IR) spectroscopy, powder X-ray diffractometry (PXRD) and solid state 13 C nuclear magnetic resonance (NMR) spectroscopy. The molecular arrangement of the new polymorphic form IV of GBM was proposed. The GBM particles with polymorphic form IV also showed an improved dissolution behavior. In addition, it was found that the formation of the new polymorphic form IV of GBM by this process was reproducible.

  5. 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.

  6. A technique for measurement of vector and tensor polarization in solid spin one polarized targets

    International Nuclear Information System (INIS)

    Kielhorn, W.F.

    1991-06-01

    Vector and tensor polarizations are explicitly defined and used to characterize the polarization states of spin one polarized targets, and a technique for extracting these polarizations from nuclear magnetic resonance (NMR) data is developed. This technique is independent of assumptions about spin temperature, but assumes the target's crystal structure induces a quadrupole interaction with the spin one particles. Analysis of the NMR signals involves a computer curve fitting algorithm implemented with a fast Fourier transform method which speeds and simplifies curve fitting algorithms used previously. For accurate curve fitting, the NMR electronic circuit must be modeled by the fitting algorithm. Details of a circuit, its model, and data collected from this circuit are given for a solid deuterated ammonia target. 37 refs., 19 figs., 3 tabs

  7. On the use of the spectroscopic techniques to model the interactions between radionuclides and solid minerals

    Energy Technology Data Exchange (ETDEWEB)

    Simoni, E. [IPN, Paris XI University, 91406 Orsay (France)]. e-mail: simoni@ipno.in2p3.fr

    2004-07-01

    In order to determine the radionuclides sorption constants on solid natural minerals, both thermodynamic and structural investigations, using spectroscopic techniques, are presented. The natural clays, that could be used as engineering barrier in the nuclear waste geological repository, are rather complex minerals. Therefore, in order to understand how these natural materials retain the radionuclides, it is necessary first to perform these studies on simple substrates such as phosphates, oxides and silicates (as powder and single crystal as well) and then extrapolate the obtained results on the natural minerals. As examples, the main results on the sorption processes of the hexavalent uranium onto zircon (ZrSiO{sub 4}) and lanthanum phosphate (LaPO{sub 4}) are presented. The corresponding sorption curves are simulated using the results obtained with the following spectroscopic techniques: laser induced spectro fluorimetry, X-ray photoelectron spectroscopy (XP S), X-ray absorption spectroscopy (Exafs). Finally, the thermodynamic sorption constants are calculated. (Author)

  8. A technique for measurement of vector and tensor polarization in solid spin one polarized targets

    Energy Technology Data Exchange (ETDEWEB)

    Kielhorn, W.F.

    1991-06-01

    Vector and tensor polarizations are explicitly defined and used to characterize the polarization states of spin one polarized targets, and a technique for extracting these polarizations from nuclear magnetic resonance (NMR) data is developed. This technique is independent of assumptions about spin temperature, but assumes the target's crystal structure induces a quadrupole interaction with the spin one particles. Analysis of the NMR signals involves a computer curve fitting algorithm implemented with a fast Fourier transform method which speeds and simplifies curve fitting algorithms used previously. For accurate curve fitting, the NMR electronic circuit must be modeled by the fitting algorithm. Details of a circuit, its model, and data collected from this circuit are given for a solid deuterated ammonia target. 37 refs., 19 figs., 3 tabs.

  9. Time-Domain Fluorescence Lifetime Imaging Techniques Suitable for Solid-State Imaging Sensor Arrays

    Directory of Open Access Journals (Sweden)

    Robert K. Henderson

    2012-05-01

    Full Text Available We have successfully demonstrated video-rate CMOS single-photon avalanche diode (SPAD-based cameras for fluorescence lifetime imaging microscopy (FLIM by applying innovative FLIM algorithms. We also review and compare several time-domain techniques and solid-state FLIM systems, and adapt the proposed algorithms for massive CMOS SPAD-based arrays and hardware implementations. The theoretical error equations are derived and their performances are demonstrated on the data obtained from 0.13 μm CMOS SPAD arrays and the multiple-decay data obtained from scanning PMT systems. In vivo two photon fluorescence lifetime imaging data of FITC-albumin labeled vasculature of a P22 rat carcinosarcoma (BD9 rat window chamber are used to test how different algorithms perform on bi-decay data. The proposed techniques are capable of producing lifetime images with enough contrast.

  10. Application of London-type dispersion corrections to the solid-state density functional theory simulation of the terahertz spectra of crystalline pharmaceuticals.

    Science.gov (United States)

    King, Matthew D; Buchanan, William D; Korter, Timothy M

    2011-03-14

    The effects of applying an empirical dispersion correction to solid-state density functional theory methods were evaluated in the simulation of the crystal structure and low-frequency (10 to 90 cm(-1)) terahertz spectrum of the non-steroidal anti-inflammatory drug, naproxen. The naproxen molecular crystal is bound largely by weak London force interactions, as well as by more prominent interactions such as hydrogen bonding, and thus serves as a good model for the assessment of the pair-wise dispersion correction term in systems influenced by intermolecular interactions of various strengths. Modifications to the dispersion parameters were tested in both fully optimized unit cell dimensions and those determined by X-ray crystallography, with subsequent simulations of the THz spectrum being performed. Use of the unmodified PBE density functional leads to an unrealistic expansion of the unit cell volume and the poor representation of the THz spectrum. Inclusion of a modified dispersion correction enabled a high-quality simulation of the THz spectrum and crystal structure of naproxen to be achieved without the need for artificially constraining the unit cell dimensions.

  11. A radioisotope technique for laboratory studies of the dispersal of rice weevil in grain

    International Nuclear Information System (INIS)

    Khan, M.Z.A.; Robertson, G.B.

    1979-01-01

    Adult rice weevils (Sitophilus oryzae (L.)) were marked with paint containing Scandium-46 and detected in a column of wheat 4.5 cm diam by means of a γ-scintillation counter. The radioactive paint had no effect on the mobility and longevity of the insects. Two weevils marked with Sc-46 could be located if they were more than 2.5 cm apart. An account is given of the use of the technique to follow the movements of a single pair of male and female weevils over 8 days. (Auth.)

  12. Improvement of Dispersion and Color Effect of Organic Pigments in Polymeric Films via Microencapsulation by the Miniemulsion Technique

    Directory of Open Access Journals (Sweden)

    Dongming Qi

    2013-01-01

    Full Text Available Three primary pigment/poly(n-butyl acrylate-co-styrene (P(BA+St nanocomposites were prepared via encapsulation of the corresponding organic pigments via the miniemulsion technique. The resulting latexes of the P(BA+St/pigment nanocomposites were filmed in a PTFE mould or printed onto cotton fabric. The morphology of the P(BA+St/pigment nanocomposites and the dispersion of pigment particles in the latex film and on the printed fabric surface, as well as the adhesion between pigment and adhesive film, were evaluated by transmission electron microscopy (TEM, field emission scanning electron microscopy (FESEM, 3D digital microscope system (3D-POM, and printing results tests. Attributing to the preprotection of adhesive polymer shell, the self-adhesive P(BA+St/pigment nanocomposites were homogeneously and firmly dispersed both in the thin latex film and in the adhesive layer on the fiber surface. As a result, the color strength, color fastness, and handle of the fabrics printed by the P(BA+St/pigment nanocomposites latex were significantly improved, compared to the fabrics printed by the conventional pigment blended latex.

  13. Determination of twelve herbicides in tobacco by a combination of solid–liquid–solid dispersive extraction using multi-walled carbon nanotubes, dispersive liquid-liquid micro-extraction, and detection by GC with triple quadrupole mass spectrometry

    International Nuclear Information System (INIS)

    Liao, Qie Gen; Zhou, Yao Min; Luo, Lin Guang; Wang, Li Bing; Feng, Xiao Hu

    2014-01-01

    We report on a method for the determination of twelve herbicides using solid–liquid–solid dispersive extraction (SLSDE), followed by dispersive liquid-liquid micro-extraction (DLLME) and quantitation by gas chromatography with triple quadrupole mass spectrometric detection. SLSDE was applied to the extraction of herbicides from tobacco samples using multi-walled carbon nanotubes (MWCNTs) as clean-up adsorbents. The effect of the quantity of MWCNTs on SLSDE, and of type and volume of extraction and disperser solvents and of salt effect on DLLME were optimized. Good linearity is obtained in the 5.0 - 500 μg kg −1 concentration range, with regression coefficients of >0.99. Intra-day and inter-day repeatability, expressed as relative standard deviations, are between 3 and 9 %. The recoveries in case of herbicide-spiked tobacco at concentration levels of 20.0, 50.0 and 100.0 g kg −1 ranged from 79 to 105 %, and LODs are between 1.5 and 6.1 μg kg −1 . All the tobacco samples were found to contain butralin and pendimethalin at levels ranging from 15.8 to 500.0 μg kg −1 . (author)

  14. Facile solid-state synthesis of highly dispersed Cu nanospheres anchored on coal-based activated carbons as an efficient heterogeneous catalyst for the reduction of 4-nitrophenol

    Science.gov (United States)

    Wang, Shan; Gao, Shasha; Tang, Yakun; Wang, Lei; Jia, Dianzeng; Liu, Lang

    2018-04-01

    Coal-based activated carbons (AC) were acted as the support, Cu/AC catalysts were synthesized by a facile solid-state reaction combined with subsequent heat treatment. In Cu/AC composites, highly dispersed Cu nanospheres were anchored on AC. The catalytic activity for 4-nitrophenol (4-NP) was investigated, the effects of activation temperature and copper loading on the catalytic performance were studied. The catalysts exhibited very high catalytic activity and moderate chemical stability due to the unique characteristics of the particle-assembled nanostructures, the high surface area and the porous structure of coal-based AC and the good dispersion of metal particles. Design and preparation of non-noble metal composite catalysts provide a new direction for improving the added value of coal.

  15. 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.

  16. 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.

  17. 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.

  18. 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%.

  19. Study of axial mixing, holdup and slip velocity of dispersed phase in a pulsed sieve plate extraction column using radiotracer technique.

    Science.gov (United States)

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

    2009-01-01

    Axial mixing, holdup and slip velocity of dispersed phase which are parameters of fundamental importance in the design and operation of liquid-liquid extraction pulsed sieve plate columns have been investigated. Experiments for residence time distribution (RTD) analysis have been carried out for a range of pulsation frequency and amplitude in a liquid-liquid extraction pulsed sieve plate column with water as dispersed and kerosene as continuous phase using radiotracer technique. The column was operated in emulsion region and (99m)Tc in the form of sodium pertechnetate eluted from a (99)Mo/(99m)Tc generator was used to trace the dispersed phase. Axial dispersed plug flow model with open-open boundary condition and two points measurement method was used to simulate the hydrodynamics of dispersed phase. It has been observed that the axial mixing and holdup of dispersed phase increases with increase in pulsation frequency and amplitude until a maximum value is achieved while slip velocity decreases with increase in pulsation frequency and amplitude until it approaches a minimum value. Short lived and low energy radiotracer (99m)Tc in the form of sodium pertechnetate was found to be a good water tracer to study the hydrodynamics of a liquid-liquid extraction pulsed sieve plate column operating with two immiscible liquids, water and kerosene. Axial dispersed plug flow model with open-open boundary condition was found to be a suitable model to describe the hydrodynamics of dispersed phase in the pulsed sieve plate extraction column.

  20. Study of axial mixing, holdup and slip velocity of dispersed phase in a pulsed sieve plate extraction column using radiotracer technique

    International Nuclear Information System (INIS)

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

    2009-01-01

    Axial mixing, holdup and slip velocity of dispersed phase which are parameters of fundamental importance in the design and operation of liquid-liquid extraction pulsed sieve plate columns have been investigated. Experiments for residence time distribution (RTD) analysis have been carried out for a range of pulsation frequency and amplitude in a liquid-liquid extraction pulsed sieve plate column with water as dispersed and kerosene as continuous phase using radiotracer technique. The column was operated in emulsion region and 99m Tc in the form of sodium pertechnetate eluted from a 99 Mo/ 99m Tc generator was used to trace the dispersed phase. Axial dispersed plug flow model with open-open boundary condition and two points measurement method was used to simulate the hydrodynamics of dispersed phase. It has been observed that the axial mixing and holdup of dispersed phase increases with increase in pulsation frequency and amplitude until a maximum value is achieved while slip velocity decreases with increase in pulsation frequency and amplitude until it approaches a minimum value. Short lived and low energy radiotracer 99m Tc in the form of sodium pertechnetate was found to be a good water tracer to study the hydrodynamics of a liquid-liquid extraction pulsed sieve plate column operating with two immiscible liquids, water and kerosene. Axial dispersed plug flow model with open-open boundary condition was found to be a suitable model to describe the hydrodynamics of dispersed phase in the pulsed sieve plate extraction column.

  1. Structural characterization of the phospholipid stabilizer layer at the solid-liquid interface of dispersed triglyceride nanocrystals with small-angle x-ray and neutron scattering

    Science.gov (United States)

    Schmiele, Martin; Schindler, Torben; Unruh, Tobias; Busch, Sebastian; Morhenn, Humphrey; Westermann, Martin; Steiniger, Frank; Radulescu, Aurel; Lindner, Peter; Schweins, Ralf; Boesecke, Peter

    2013-06-01

    Dispersions of crystalline nanoparticles with at least one sufficiently large unit cell dimension can give rise to Bragg reflections in the small-angle scattering range. If the nanocrystals possess only a small number of unit cells along these particular crystallographic directions, the corresponding Bragg reflections will be broadened. In a previous study of phospholipid stabilized dispersions of β-tripalmitin platelets [Unruh, J. Appl. Crystallogr.JACGAR0021-889810.1107/S0021889807044378 40, 1008 (2007)], the x-ray powder pattern simulation analysis (XPPSA) was developed. The XPPSA method facilitates the interpretation of the rather complicated small-angle x-ray scattering (SAXS) curves of such dispersions of nanocrystals. The XPPSA method yields the distribution function of the platelet thicknesses and facilitates a structural characterization of the phospholipid stabilizer layer at the solid-liquid interface between the nanocrystals and the dispersion medium from the shape of the broadened 001 Bragg reflection. In this contribution an improved and extended version of the XPPSA method is presented. The SAXS and small-angle neutron scattering patterns of dilute phospholipid stabilized tripalmitin dispersions can be reproduced on the basis of a consistent simulation model for the particles and their phospholipid stabilizer layer on an absolute scale. The results indicate a surprisingly flat arrangement of the phospholipid molecules in the stabilizer layer with a total thickness of only 12 Å. The stabilizer layer can be modeled by an inner shell for the fatty acid chains and an outer shell including the head groups and additional water. The experiments support a dense packing of the phospholipid molecules on the nanocrystal surfaces rather than isolated phospholipid domains.

  2. Analysis of SHLW by Energy Dispersive X-Ray Fluorescence (EDXRF) technique

    International Nuclear Information System (INIS)

    Vadivu, Senthil; Seshadreesan, N.P.; Kumar, R.; Venkatasubramani, C.R.

    2012-01-01

    The simulated high level liquid waste (SHLW) sample expected from fuel reprocessing experiments containing uranium and about 20 various other elements were analysed by EDXRF technique. An investigation with respect to Nd estimation, a burn up monitor, in presence of varying concentrations of U was also carried out. The simulated raffinate solution with a mixture of 20 expected elements was used as standard solution. Four samples of varying concentrations were prepared by appropriate dilution from the standard solution. Calibrations were carried out for its various constituent elements. The elements such as Cs, Mo, Sr,Y, Cd, Ba, Ce, U and La were analysed using W-filter whereas the elements such as Nd, Fe and Ni were analysed using Ge secondary target. The results of 4 simulated samples analysed using FDXRF are given. These values for each element are the mean of the three values obtained. The results obtained for different simulated waste are also shown. These solutions are of different compositions and therefore, vary in their matrix effects. Nevertheless, the medium of second simulated waste is in 3.5N HNO 3 where as the calibration is done with 0.1N HNO 3 medium and hence this might be the cause for large deviations observed in some of the results. A trend of the non-interference of the Uranium matrix in the assay of Nd was demonstrated typically at a fixed concentration of 92.3 ppm in uranium matrix of 900 and 6000 ppm. In both the cases, it was observed that the concentration of Nd measured remained same. This is in accordance to the fact that the characteristic X-ray energy peaks of Nd (L-lines) and U (M-lines) are well separated in the spectrum and the contribution of the low energy peak of Uranium to the higher energy peak of Nd is negligible. But the limiting concentration of Uranium may be the one in which a overlapping of its peak occurs

  3. Axial Dispersion Model for Solid Flow in Liquid Suspension in System of Two Mixers in Total Recycle

    Czech Academy of Sciences Publication Activity Database

    Čermáková, Jiřina; Scargiali, F.; Siyakatshana, N.; Kudrna, V.; Brucato, A.; Machoň, V.

    2006-01-01

    Roč. 117, č. 2 (2006), s. 101-107 ISSN 1385-8947 R&D Projects: GA AV ČR(CZ) IAA4072402 Institutional research plan: CEZ:AV0Z40720504 Keywords : residence time distribution * dispersion model * flow mixer Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 1.594, year: 2006

  4. Cellulose nanocrystal/polyolefin biocomposites prepared by solid-state shear pulverization: Superior dispersion leading to synergistic property enhancements

    Science.gov (United States)

    Krishnan A. Iyer; Gregory T. Schueneman; John M. Torkelson

    2015-01-01

    Cellulose nanocrystals (CNCs), a class of renewable bionanomaterials with excellent mechanical properties, have gained major interest as filler for polymers. However, challenges associated with effective CNC dispersion have hindered the production of composites with desired property enhancements. Here, composites of polypropylene (PP) and low density polyethylene (LDPE...

  5. Observation on the stability of the solid phase microparticles separating technique in T3, T4 radioimmunoassay

    International Nuclear Information System (INIS)

    Chen Guangliang; Chen Xunmin

    1995-01-01

    The solid phase T 3 ,T 4 RIA is adopted at various laboratories. The data analysis from the effective dose and quality control of samples indicates that the separation technique is of good effect and high stability. It is an effective separation technique for the quality control in RIA

  6. A Noncontact Measurement Technique for the Density and Thermal Expansion Coefficient of Solid and Liquid Materials

    Science.gov (United States)

    Chung, Sang K.; Thiessen, David B.; Rhim, Won-Kyu

    1996-01-01

    A noncontact measurement technique for the density and the thermal expansion refractory materials in their molten as well as solid phases is presented. This technique is based on the video image processing of a levitated sample. Experiments were performed using the high-temperature electrostatic levitator (HTESL) at the Jet Propulsion Laboratory in which 2-3 mm diameter samples can be levitated, melted, and radiatively cooled in a vacuum. Due to the axisymmetric nature of the molten samples when levitated in the HTESL, a rather simple digital image analysis can be employed to accurately measure the volumetric change as a function of temperature. Density and the thermal expansion coefficient measurements were made on a pure nickel sample to test the accuracy of the technique in the temperature range of 1045-1565 C. The result for the liquid phase density can be expressed by p = 8.848 + (6.730 x 10(exp -4)) x T (degC) g/cu cm within 0.8% accuracy, and the corresponding thermal expansion coefficient can be expressed by Beta=(9.419 x 10(exp -5)) - (7.165 x 10(exp -9) x T (degC)/K within 0.2% accuracy.

  7. Dissolvable layered double hydroxide as an efficient nanosorbent for centrifugeless air-agitated dispersive solid-phase extraction of potentially toxic metal ions from bio-fluid samples.

    Science.gov (United States)

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

    2017-03-08

    In the present work, a novel nanosorbent namely layered double hydroxides with 4-amino-5-hydroxyl-2,7-naphthalendisulfonic acid monosodium salt interlayer anion (Mg-Al-AHNDA-LDH) was synthesized and applied as a dissolvable nanosorbent in a centrifugeless ultrasound-enhanced air-agitated dispersive solid-phase extraction (USE-AA-D-SPE) method. This method was used for the separation and preconcentration of some metal ions including Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ , and Ni 2+ prior to their determination using the micro-sampling flame atomic absorption spectrometry (MS-FAAS) technique. The most interesting aspect of this nanosorbent is its immediate dissolvability at pH values lower than 4. This capability drastically eliminates the elution step, leading to a great improvement in the extraction efficiency and a decrease in the extraction time. Also in this method, the use of a syringe nanofilter eliminates the need for the centrifugation step, which is time-consuming and essentially causes the analysis to be off-line. Several effective parameters governing the extraction efficiency including the sample solution pH, amount of nanosorbent, eluent condition, number of air-agitation cycles, and sonication time were investigated and optimized. Under the optimized conditions, the good linear dynamic ranges of 2-70, 6-360, 7-725, 7-370, and 8-450 ng mL -1 for the Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ and Ni 2+ ions, respectively, with the correlation of determinations (R 2 s) higher than 0.997 were obtained. The limits of detection (LODs) were found to be 0.6, 1.7, 2.0, 2.1, and 2.4 for the Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ , and Ni 2+ ions, respectively. The intra-day and inter-day precisions (percent relative standard deviations (%RSDs) (n = 5)) were below 7.8%. The proposed method was also successfully applied for the extraction and determination of the target ions in different biological fluid and tap water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Investigation of Different Colloidal Porous Silicon Solutions and Their Composite Solid Matrix Rods by Optical Techniques

    Science.gov (United States)

    Khan, M. Naziruddin; Aldalbahi, Ali; Almohammedi, Abdullah

    2018-03-01

    Colloidal porous silicon (PSi) in different solvents was synthesized by simple chemical etching. Colloidal solutions were then prepared using different quantities of silicon wafer pieces (Pcs) and chloroplatinic (Pt) acid in catalyst solution. The effect on the properties of the colloidal solutions and composite rods were investigated using various optical characterization techniques. Absorption and photoluminescence (PL) intensity of the colloidal PSi solutions are observed to depend on the quantity of wafer Pcs, the Pt-solution, and the porosity formation on the wafer surface. The morphological structure of the PSi in a solvent and the solid-rod environments were studied using field-emission scanning electron microscopy (FE-SEM) and were observed to have different structures. A mono-oriented structure of PSi exists in tetrahydrofuran, which has stereo orientation in dioxane and dimethylsulfoxide (approximately 5-8 nm as confirmed using high resolution transmission electron microscopy). Subsequently, some colloidal PSi solutions were directly embedded in three types of sol-gel-based matrices, silica, ormosils (or organically modified silica) and polymer, which easily generated solid rods. Spontaneous emission (SE) of the PSi solutions and their composite rods were examined using a high power picosecond 355 nm laser source. The emitted PL and SE signals of the colloidal PSi solutions were dependent on the Pt volume, nature of the solvent, quantity of Si wafer piece, and pumping energy. The response of SE signals from the PSi composites rods is an interesting phenomenon, and such nanocomposites may be used for future research on light amplification.

  9. Studies of atomic collisions in solids by means of calorimetric techniques

    International Nuclear Information System (INIS)

    Andersen, H.H.

    1974-10-01

    The results of the application of the calorimetric technique to measure the way in which the energy of particles passed through a thin foil and stopped within a solid block is disturbed between the foil and the block are presented. This measurement gives the relative energy loss of the projectile in the foil and hence, since the foil thickness is measured independently, the stopping power. Radiation-damage measurements are discussed. In these measurements, the same cryostat as that employed in the stopping-power measurements was used. The foil was left out and the block remained as a very efficient dosimetry device. Furthermore, a number of experimental complications must be taken into account when damage is measured. Finally, results are presented of the measurement of energy distribution between two systems, this time performed at room temperature. The measurements are not nearly as accurate as those performed at low temperatures, but the physical property studied, the energy reflected from a solid surface bombarded with low-energy heavy ions (sputtering efficiency) could hardly be studied in any other way. The thesis is a summary of thirteen publications on energetic-particle calorimetry, all these papers being reproduced as appendices to the main text. (B.R.H.)

  10. Development of novel cilostazol-loaded solid SNEDDS using a SPG membrane emulsification technique: Physicochemical characterization and in vivo evaluation.

    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; Lee, Beom-Jin; Park, Young Joon; Yong, Chul Soon; Kim, Jong Oh; Choi, Han-Gon

    2017-02-01

    The objective of this study was to develop a novel solid self-nanoemulsifying drug delivery system (SNEDDS) using a membrane emulsification technique involving Shirasu porous glass (SPG) which produced very small and uniform emulsion droplets, resulting in enhanced solubility, dissolution and oral bioavailability of poorly water-soluble cilostazol. The effects of carriers on the drug solubility were assessed, and pseudo-ternary phase diagrams were plotted. Among the liquid SNEDDS formulations tested, the liquid SNEDDS composed of peceol (oil), Tween 20 (surfactant) and Labrasol (cosurfactant) at a weight ratio of 15/55/30, produced the smallest emulsion droplet size. The cilostazol-loaded liquid SNEDDS formulation was suspended in the distilled water and subjected to SPG membrane emulsification. Calcium silicate was added as a solid carrier in this liquid SNEDDS, completely suspended and spray-dried, leading to the production of a cilostazol-loaded solid SNEDDS. The emulsion droplet size, solubility and dissolution of the emulsified solid SNEDDS were assessed as compared to the solid SNEDDS prepared without emulsification. Moreover, the physicochemical characteristics and pharmacokinetics in rats were evaluated with the emulsified solid SNEDDS. The emulsified solid SNEDDS provided significantly smaller and more uniform nanoemulsions than did the non-emulsified solid SNEDDS. The emulsified solid SNEDDS showed significantly higher drug solubility and dissolution as compared to the non-emulsified solid SNEDDS. The crystalline drug in it was converted into the amorphous state. Moreover, in rats, it gave significantly higher initial plasma concentrations and AUC compared to the drug powder, suggesting its improved oral bioavailability of cilostazol. Thus, this novel solid SNEDDS developed using a membrane emulsification technique represents a potentially powerful oral delivery system for cilostazol. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Molecular-level elucidation of saccharin-assisted rapid dissolution and high supersaturation level of drug from Eudragit® E solid dispersion.

    Science.gov (United States)

    Ueda, Keisuke; Kanaya, Harunobu; Higashi, Kenjirou; Yamamoto, Keiji; Moribe, Kunikazu

    2018-03-01

    In this work, the effect of saccharin (SAC) addition on the dissolution and supersaturation level of phenytoin (PHT)/Eudragit® E (EUD-E) solid dispersion (SD) at neutral pH was examined. The PHT/EUD-E SD showed a much slower dissolution of PHT compared to the PHT/EUD-E/SAC SD. EUD-E formed a gel layer after the dispersion of the PHT/EUD-E SD into an aqueous medium, resulting in a slow dissolution of PHT. Pre-dissolving SAC in the aqueous medium significantly improved the dissolution of the PHT/EUD-E SD. Solid-state 13 C NMR measurements showed an ionic interaction between the tertiary amino group of EUD-E and the amide group of SAC in the EUD-E gel layer. Consequently, the ionized EUD-E could easily dissolve from the gel layer, promoting PHT dissolution. Solution-state 1 H NMR measurements revealed the presence of ionic interactions between SAC and the amino group of EUD-E in the PHT/EUD-E/SAC solution. In contrast, interactions between PHT and the hydrophobic group of EUD-E strongly inhibited the crystallization of the former from its supersaturated solution. The PHT supersaturated solution was formed from the PHT/EUD-E/SAC SD by the fast dissolution of PHT and the strong crystallization inhibition effect of EUD-E after aqueous dissolution. Copyright © 2018 Elsevier B.V. All rights reserved.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

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

    Science.gov (United States)

    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.

  17. Conformation of LSM/YSZ and LSM ceramic films obtained by the citrate and solid mixture techniques; Conformacao de filmes ceramicos de LSM e LSM/YSZ obtidos pelas tecnicas citratos e mistura de solidos

    Energy Technology Data Exchange (ETDEWEB)

    Chiba, R.; Vargas, R.A.; Andreoli, M.; Seo, E.S.M., E-mail: rchiba@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (CCTM/IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Ciencia e Tecnologia de Materiais. Lab. de SOFC - Insumos e Componentes

    2009-07-01

    In this work, the ceramic films of LSM/YSZ (strontium-doped lanthanum manganite/Yttria-stabilized zirconia) and LSM used as cathodes of the solid oxide fuel cells (SOFC) are conformed by the wet powder spraying technique. The composite LSM/YSZ was obtained by the solid mixture technique and LSM by the citrate technique. For the formation of the LSM/YSZ and LSM ceramic films was necessary the preparation of dispersed ceramic suspensions for the deposition in YSZ substrate, used as electrolyte of the CaCOS. These powders were conformed using an aerograph for the deposition of the LSM/YSZ and LSM thin films of approximately 40 microns. The half-cells had been characterized by X-ray diffractometry (XRD), identifying the phases hexagonal (LSM) and cubica (YSZ). And electronic scanning electron microscopy (SEM) was used to evaluate the adherence and porosity of the ceramic films according to the characteristics of the cathode. (author)

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

    Directory of Open Access Journals (Sweden)

    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.

  19. 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.

  20. Co-ordinated research programme on the use of nuclear and nuclear-related techniques in the study of environmental pollution associated with solid wastes

    International Nuclear Information System (INIS)

    1988-01-01

    A co-ordinated research programme on the use of nuclear and nuclear-related techniques in the study of environmental pollution associated with solid wastes was started by the Agency in December 1987 and now comprises nineteen participants from seventeen countries. Topics of interest in this programme include studies of atmospheric aerosols, coal fly ash, incinerator ash, sewage sludge and a variety of other environmental specimens contaminated with solid wastes. The analytical techniques being used in this programme include neutron activation analysis (NAA), particle induced X-ray emission (PIXE) and energy-dispersive X-ray fluorescence (ED-XRF). This report summarizes the discussions that took place during the first research co-ordination meeting. Working papers presented by the participants are included as annexes. The main outcome of the meeting was agreement to include a ''core'' programme comprising studies of (1) aerosols collected from areas of low and high pollution, (2) coal fly ash composition, and (3) leaching of toxic elements from coal fly ash

  1. 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.

  2. Eco-efficiency analysis of techniques for disposal of urban solid waste

    International Nuclear Information System (INIS)

    Dmitrijevas, Cibele

    2010-01-01

    Municipal solid waste is one of the major problems of modern society. In this sense it is necessary to discuss solutions to the fate of waste generated daily, increasingly in larger amounts, being imperative to advance the search for alternatives, not only in search of new technologies and solutions, as well as the improvement of methodologies currently employed to solve this relevant issue, especially in large urban centers. This paper presents the results of a comparative economic-environmental assessment performed by a method developed by BASF, two potential technologies: landfill and incineration with energy recovery. To facilitate the work, the information used were both real data - landfill and incinerator - Essencis Solucoes Ambientais S.A., (assuming some assumptions) and the use of secondary data, using the study of Arena et al., 2003. This ecoefficiency analysis tool covers the methodology of Life Cycle Assessment (LCA), which is a technique to evaluate the inputs and outputs of matter and energy and the potential environmental impacts associated with all stages of resource extraction and their transformations , and the use and final disposal of the product. The data in the environmental assessment are presented according to major categories, using a weighting method developed by BASF and understand the consumption of natural resources, consumption of energy resources, air emissions, water and soil, potential for human toxicity, accidents work, occupational diseases and land use. Economic evaluation in this work took into account the costs involved in operation and maintenance of disposal techniques or treatment of waste. The comparative study found the treatment or disposal of 7.324109 billion kilograms of waste. As a result, the array of eco-efficiency indicates that the incinerator is the alternative that stands out, considering the environmental and economic profile, within the assumptions made in this study and taking into account which is a

  3. PHYSIOLOGICAL REGULATION OF PROTEASE AND ANTIBIOTICS IN PENICILLIUM SP. USING SUBMERGED AND SOLID STATE FERMENTATION TECHNIQUES

    Directory of Open Access Journals (Sweden)

    HAIDER M. HAMZAH

    2009-03-01

    Full Text Available A fungal strain belonging to the genus Penicillium was isolated from soil sample and has been diagnosed as Penicillium sp. according to its morphological characteristics of the colonies on solid media and also microscopical examination of the fungal parts. Antibiotics, protease activity and pH values were determined after cultivation of the fungus using submerged fermentation (SF and solid state fermentation (SSF. The two different patterns of fermentation processes seem to influence the physiological behavior of the fungus differently. Experiments were made using nutrient broth medium (N.B for SF and wheat bran in SSF. The pH values were adjacent to 5.5. Wheat bran was enriched with fish scales and egg shale in a ratio of (1:2:0.005 w/w and the mixture was moistened by adding (30 ml whey solution. After 7 days of incubation, the pH value of SF was increased to 8.0 at 30ºC. The SF was appeared efficient for antibiotics production. Using well diffusion technique the extracted antibiotics solution was active against some pathogenic bacteria such as Staphylococcus aureus, E. coli, Proteus sp., Salmonella sp., Pseudomonas aeruginosa and Streptococcus sp. In SSF relative proteases concentrations were found to be highly reactive than SF. This was proved by the appearance of the zone (20 mm and 32 mm due to the hydrolysis of milk and blood proteins respectively using pH 5.5 at 30ºC for 24 hrs. The activity of proteases was (10.4 U/ml.

  4. Rayleigh Wave Dispersion Due to Spatial (FEM) Discretization of a thin Elastic Solid Having Non-Curved Boundary

    Czech Academy of Sciences Publication Activity Database

    Brepta, R.; Valeš, F.; Červ, Jan; Tikal, B.

    1996-01-01

    Roč. 58, č. 6 (1996), s. 1233-1244 ISSN 0045-7949 R&D Projects: GA ČR(CZ) GA101/93/1195 Institutional research plan: CEZ:AV0Z2076919 Keywords : thin elastic body * Rayleigh waves * grid dispersion Subject RIV: BI - Acoustics Impact factor: 0.254, year: 1996 http://apps.isiknowledge.com/full_record.do?product=UA&search_mode=GeneralSearch&qid=1&SID=U2EJknka3H@mKemE37@&page=1&doc=1&colname=WOS

  5. The amorphous solid dispersion of the poorly soluble ABT-102 forms nano/microparticulate structures in aqueous medium: impact on solubility

    Directory of Open Access Journals (Sweden)

    Frank KJ

    2012-11-01

    Full Text Available Kerstin J Frank,1,3 Ulrich Westedt,2 Karin M Rosenblatt,2 Peter Hölig,2 Jörg Rosenberg,2 Markus Mägerlein,2 Gert Fricker,3 Martin Brandl11Department of Physics, Chemistry and Pharmacy, University of Southern Denmark, Odense, Denmark; 2Abbott GmbH and Co. KG, Ludwigshafen, Germany; 3Department of Pharmaceutical Technology, University of Heidelberg, Heidelberg, GermanyAbstract: Amorphous solid dispersions (ASDs are a promising formulation approach for poorly soluble active pharmaceutical ingredients (APIs, because they ideally enhance both dissolution rate and solubility. However, the mechanism behind this is not understood in detail. In the present study, we investigated the supramolecular and the nano/microparticulate structures that emerge spontaneously upon dispersion of an ASD in aqueous medium and elucidated their influence on solubility. The ASD, prepared by hot melt extrusion, contained the poorly soluble ABT-102 (solubility in buffer, 0.05 µg/mL, a hydrophilic polymer, and three surfactants. The apparent solubility of ABT-102 from the ASD-formulation was enhanced up to 200 times in comparison to crystalline ABT-102. At the same time, the molecular solubility, as assessed by inverse equilibrium dialysis, was enhanced two times. Asymmetrical flow field-flow fractionation in combination with a multiangle light-scattering detector, an ultraviolet detector, and a refractometer enabled us to separate and identify the various supramolecular assemblies that were present in the aqueous dispersions of the API-free ASD (placebo and of binary/ternary blends of the ingredients. Thus, the supramolecular assemblies with a molar mass between 20,000 and 90,000 could be assigned to the polyvinylpyrrolidone/vinyl acetate 64, while two other kinds of assemblies were assigned to different surfactant assemblies (micelles. The amount of ABT-102 remaining associated with each of the assemblies upon fractionation was quantified offline with high

  6. Characterization of solid polymer dispersions of active pharmaceutical ingredients by 19F MAS NMR and factor analysis

    Czech Academy of Sciences Publication Activity Database

    Urbanová, Martina; Brus, Jiří; Šeděnková, Ivana; Policianová, Olivia; Kobera, Libor

    2013-01-01

    Roč. 100, 1 January (2013), s. 59-66 ISSN 1386-1425 R&D Projects: GA ČR GPP106/11/P426; GA MŠk 2B08021 Institutional research plan: CEZ:AV0Z40500505 Institutional support: RVO:61389013 Keywords : solid-state NMR * factor analysis * 19F MAS NMR Subject RIV: FR - Pharmacology ; Medidal Chemistry Impact factor: 2.129, year: 2013

  7. Influence of dispersing technique and irradiation on the structure of polyethylene in polypropylene matrix in a wide temperature range

    International Nuclear Information System (INIS)

    Antipov, E.M.; Kuptsov, S.A.; Kuz'min, N.N.; Pavlov, S.A.; AN SSSR, Moscow. Inst. Neftekhimicheskogo Sinteza)

    1988-01-01

    The structure of PE dispersed into PP matrix through solution or melt has been studied by X-ray analysis method. In oriented composition melting of HDPE after action of ionizing irradiation is accompanied by transition of some crystallites into pseudohexagonal modification. The fraction of transformed chains depends on the irradiation dose, dispersion method and conditions of orientation

  8. Techniques and Protocols for Dispersing Nanoparticle Powders in Aqueous Media-Is there a Rationale for Harmonization?

    Science.gov (United States)

    Hartmann, Nanna B; Jensen, Keld Alstrup; Baun, Anders; Rasmussen, Kirsten; Rauscher, Hubert; Tantra, Ratna; Cupi, Denisa; Gilliland, Douglas; Pianella, Francesca; Riego Sintes, Juan M

    2015-01-01

    Selecting appropriate ways of bringing engineered nanoparticles (ENP) into aqueous dispersion is a main obstacle for testing, and thus for understanding and evaluating, their potential adverse effects to the environment and human health. Using different methods to prepare (stock) dispersions of the same ENP may be a source of variation in the toxicity measured. Harmonization and standardization of dispersion methods applied in mammalian and ecotoxicity testing are needed to ensure a comparable data quality and to minimize test artifacts produced by modifications of ENP during the dispersion preparation process. Such harmonization and standardization will also enhance comparability among tests, labs, and studies on different types of ENP. The scope of this review was to critically discuss the essential parameters in dispersion protocols for ENP. The parameters are identified from individual scientific studies and from consensus reached in larger scale research projects and international organizations. A step-wise approach is proposed to develop tailored dispersion protocols for ecotoxicological and mammalian toxicological testing of ENP. The recommendations of this analysis may serve as a guide to researchers, companies, and regulators when selecting, developing, and evaluating the appropriateness of dispersion methods applied in mammalian and ecotoxicity testing. However, additional experimentation is needed to further document the protocol parameters and investigate to what extent different stock dispersion methods affect ecotoxicological and mammalian toxicological responses of ENP.

  9. Techniques and Protocols for Dispersing Nanoparticle Powders in Aqueous Media—is there a Rationale for Harmonization?

    DEFF Research Database (Denmark)

    Hartmann, Nanna B.; Jensen, Keld Alstrup; Baun, Anders

    2015-01-01

    scientific studies and from consensus reached in larger scale research projects and international organizations. A step-wise approach is proposed to develop tailored dispersion protocols for ecotoxicological and mammalian toxicological testing of ENP. The recommendations of this analysis may serve as a guide......Selecting appropriate ways of bringing engineered nanoparticles (ENP) into aqueous dispersion is a main obstacle for testing, and thus for understanding and evaluating, their potential adverse effects to the environment and human health. Using different methods to prepare (stock) dispersions...... of the same ENP may be a source of variation in the toxicity measured. Harmonization and standardization of dispersion methods applied in mammalian and ecotoxicity testing are needed to ensure a comparable data quality and to minimize test artifacts produced by modifications of ENP during the dispersion...

  10. Solid transport in mountain rivers: monitoring techniques and long term assessment as flood prevention tools

    Science.gov (United States)

    Longoni, Laura; Brambilla, Davide; Ivanov, Vladislav; Messa, Giacomo; Veronelli, Andrea; Radice, Alessio; Papini, Monica

    2017-04-01

    Floods are calamitous phenomena with an ever-increasing frequency around the globe, that often result in socio-economic damage and casualties. The role of the solid fraction in the river dynamic has been widely debated in the last decade and its importance is recognized as critical and not negligible in flood simulations as it has been evidenced that the severity of an event is often the result of the coupling of a flood wave with elevated solid transport rates. Nevertheless, assessing the quantity of sediment mobilized in a particular event is not feasible without a long term analysis of the river's dynamics and its morphological evolution since it is defined by past events. This work is focused on the techniques to improve knowledge about sediment production and transport through hydrological networks as a necessary component of a wise flood prevention planning. In particular, a multidisciplinary approach that combines hydraulic and geological knowledge is required in order to understand the evolution of the river sediment and how it will influence the following critical event. The methods are presented through a case study in Italy where a series of different approaches have been integrated to gain a comprehensive understanding of the problem: the sediment movement has been studied by a Eulerian as well as a Lagrangian approaches while hydraulic properties of the stream have been measured. The research started with an attempt to monitor sediment movements: in June 2016 300 sample pebbles, equipped with RFID (Radio Frequency IDentification) transponders, have been deployed in the river and tracked after every major rainfall event. The obtained data-set has been combined with a morphological analysis and a river flow discharge computed through PIV (Particle Image Velocimetry) method in order to identify the relation between a given rainfall event and sediment transport. Moreover, critical sediment size has been estimated from field data using three approaches: two

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

    Science.gov (United States)

    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.

  12. Measurement of soluble solids content in watermelon by Vis/NIR diffuse transmittance technique.

    Science.gov (United States)

    Tian, Hai-qing; Ying, Yi-bin; Lu, Hui-shan; Fu, Xia-ping; Yu, Hai-yan

    2007-02-01

    Watermelon is a popular fruit in the world with soluble solids content (SSC) being one of the major characteristics used for assessing its quality. This study was aimed at obtaining a method for nondestructive SSC detection of watermelons by means of visible/near infrared (Vis/NIR) diffuse transmittance technique. Vis/NIR transmittance spectra of intact watermelons were acquired using a low-cost commercially available spectrometer operating over the range 350~1000 nm. Spectra data were analyzed by two multivariate calibration techniques: partial least squares (PLS) and principal component regression (PCR) methods. Two experiments were designed for two varieties of watermelons [Qilin (QL), Zaochunhongyu (ZC)], which have different skin thickness range and shape dimensions. The influences of different data preprocessing and spectra treatments were also investigated. Performance of different models was assessed in terms of root mean square errors of calibration (RMSEC), root mean square errors of prediction (RMSEP) and correlation coefficient (r) between the predicted and measured parameter values. Results showed that spectra data preprocessing influenced the performance of the calibration models. The first derivative spectra showed the best results with high correlation coefficient of determination [r=0.918 (QL); r=0.954 (ZC)], low RMSEP [0.65 degrees Brix (QL); 0.58 degrees Brix (ZC)], low RMSEC [0.48 degrees Brix (QL); 0.34 degrees Brix (ZC)] and small difference between the RMSEP and the RMSEC by PLS method. The nondestructive Vis/NIR measurements provided good estimates of SSC index of watermelon, and the predicted values were highly correlated with destructively measured values for SSC. The models based on smoothing spectra (Savitzky-Golay filter smoothing method) did not enhance the performance of calibration models obviously. The results indicated the feasibility of Vis/NIR diffuse transmittance spectral analysis for predicting watermelon SSC in a

  13. Raman Spectroscopy of Solid Oxide Fuel Cells: Technique Overview and Application to Carbon Deposition Analysis

    KAUST Repository

    Maher, R. C.

    2013-07-30

    Raman spectroscopy is a powerful characterization tool for improving the understanding of solid oxide fuel cells (SOFCs), capable of providing direct, molecularly specific information regarding the physical and chemical processes occurring within functional SOFCs in real time. In this paper we give a summary of the technique itself and highlight ex situ and in situ studies that are particularly relevant for SOFCs. This is followed by a case study of carbon formation on SOFC Ni-based anodes exposed to carbon monoxide (CO) using both ex situ and in situ Raman spectroscopy combined with computational simulations. In situ measurements clearly show that carbon formation is significantly reduced for polarized SOFCs compared to those held at open circuit potential (OCP). Ex situ Raman mapping of the surfaces showed clear variations in the rate of carbon formation across the surface of polarized anodes. Computational simulations describing the geometry of the cell showed that this is due to variations in gas access. These results demonstrate the ability of Raman spectroscopy in combination with traditional characterization tools, to provide detailed understanding of critical processes occurring within functional SOFCs. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Raman Spectroscopy of Solid Oxide Fuel Cells: Technique Overview and Application to Carbon Deposition Analysis

    KAUST Repository

    Maher, R. C.; Duboviks, V.; Offer, G. J.; Kishimoto, M.; Brandon, N. P.; Cohen, L. F.

    2013-01-01

    Raman spectroscopy is a powerful characterization tool for improving the understanding of solid oxide fuel cells (SOFCs), capable of providing direct, molecularly specific information regarding the physical and chemical processes occurring within functional SOFCs in real time. In this paper we give a summary of the technique itself and highlight ex situ and in situ studies that are particularly relevant for SOFCs. This is followed by a case study of carbon formation on SOFC Ni-based anodes exposed to carbon monoxide (CO) using both ex situ and in situ Raman spectroscopy combined with computational simulations. In situ measurements clearly show that carbon formation is significantly reduced for polarized SOFCs compared to those held at open circuit potential (OCP). Ex situ Raman mapping of the surfaces showed clear variations in the rate of carbon formation across the surface of polarized anodes. Computational simulations describing the geometry of the cell showed that this is due to variations in gas access. These results demonstrate the ability of Raman spectroscopy in combination with traditional characterization tools, to provide detailed understanding of critical processes occurring within functional SOFCs. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Selective solid-phase extraction of Hg(II) using silica gel surface - imprinting technique

    International Nuclear Information System (INIS)

    Zheng, H.; Geng, T.; Hu, L.

    2008-01-01

    A new ion-imprinted amino-functionalized silica gel sorbent was synthesized by surface-imprinting technique for preconcentration and separation of Hg(II) prior to its determination by inductively coupled plasma optical emission spectrometry (ICP-OES). Compared to the traditional solid sorbents and non-imprinted polymer particles, the ion-imprinted polymers (IIPs) have higher adsorption capacity and selectivity for Hg(II). The maximum static adsorption capacity of the imprinted and non-imprinted sorbent for Hg(II) was 29.89 mg g -1 and 11.21 mg g -1 , respectively. The highest selectivity coefficient for Hg(II) in the presence of Zn(II) exceeded 230. The detection limit (3σ) of the method was 0.25 μg L -1 . The relative standard deviation of the method was 2.5% for eight replicate determinations of 10 μg of Hg 2+ in 200 mL-in-volume water sample. The procedure was validated by performing the analysis of the certified river sediment sample (GBW 08603, China) using the standard addition method. The developed method was also successfully applied to the determination of trace mercury in Chinese traditional medicine and water samples with satisfactory results. (authors)

  16. Bevacizumab loaded solid lipid nanoparticles prepared by the coacervation technique: preliminary in vitro studies

    Science.gov (United States)

    Battaglia, Luigi; Gallarate, Marina; Peira, Elena; Chirio, Daniela; Solazzi, Ilaria; Giordano, Susanna Marzia Adele; Gigliotti, Casimiro Luca; Riganti, Chiara; Dianzani, Chiara

    2015-06-01

    Glioblastoma, the most common primary brain tumor in adults, has an inauspicious prognosis, given that overcoming the blood-brain barrier is the major obstacle to the pharmacological treatment of brain tumors. As neoangiogenesis plays a key role in glioblastoma growth, the US Food and Drug Administration approved bevacizumab (BVZ), an antivascular endothelial growth factor antibody for the treatment of recurrent glioblastoma in patients whose the initial therapy has failed. In this experimental work, BVZ was entrapped in solid lipid nanoparticles (SLNs) prepared by the fatty-acid coacervation technique, thanks to the formation of a hydrophobic ion pair. BVZ activity, which was evaluated by means of four different in vitro tests on HUVEC cells, increased by 100- to 200-fold when delivered in SLNs. Moreover, SLNs can enhance the permeation of fluorescently labelled BVZ through an hCMEC/D3 cell monolayer—an in vitro model of the blood brain barrier. These results are promising, even if further in vivo studies are required to evaluate the effective potential of BVZ-loaded SLNs in glioblastoma treatment.

  17. 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.

  18. 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.

  19. 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.

  20. Enhanced dissolution rate of dronedarone hydrochloride via preparation of solid dispersion using vinylpyrrolidone-vinyl acetate copolymer (Kollidone® VA 64)

    Energy Technology Data Exchange (ETDEWEB)

    Jung, Hyuck Jun; Kang, Myung Joo [College of Pharmacy, Dankook University, Cheonan (Korea, Republic of); Han, Sang Duk [Dong-A ST Rese arch Institute, Pharmaceutical Product Research Laboratories, Yongin (Korea, Republic of)

    2015-09-15

    Solid dispersion (SD) systems have been widely used to increase the dissolution rate and oral absorption of poorly water-soluble compounds. In order to enhance the dissolution rate of dronedarone hydrochloride (DRN), a recent antiarrhythmic agent, SDs of DRN were formulated using conventional solvent evaporation method with amorphous polymers including hydroxypropyl methyl cellulose (HPMC), poly(vinyl pyrrolidone) (PVP), and vinylpyrrolidone-vinyl acetate copolymer (VA64). The prepared SDs were characterized in terms of drug crystallinity, morphology, and in vitro dissolution profile in aqueous medium. The physical characterization using differential scanning calorimetry and X-ray powder diffraction revealed that the active compound was molecularly dispersed in all polymeric carriers tested, in a stable amorphous form in drug to polymer ratios ranging from 1:0.5 to 1:2. The dissolution rates of DRN in all SDs were much higher than those from the corresponding physical mixture and drug powder alone. In particular, the greatest dissolution enhancement was obtained from the VA64-based SD in a drug to polymer weight ratio of 1:1, achieving almost complete drug release after 120 min at pH 1.2. Thus, VA64-based SD with higher drug dissolution rate along with a simple preparation process is suggested as an alternative for the oral formulation of the benzofuran derivative.

  1. 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.

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

    Directory of Open Access Journals (Sweden)

    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

  3. 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.

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

    Science.gov (United States)

    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.

  5. 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.

  6. 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.

  7. 1-Butyl-3-aminopropyl imidazolium-functionalized graphene oxide as a nanoadsorbent for the simultaneous extraction of steroids and β-blockers via dispersive solid-phase microextraction.

    Science.gov (United States)

    Serrano, Maria; Chatzimitakos, Theodoros; Gallego, Mercedes; Stalikas, Constantine D

    2016-03-04

    In this study, we describe the synthesis of graphene oxide functionalized with the ionic liquid 1-butyl-3-aminopropyl imidazolium chloride and its use as an adsorbent for the dispersive solid-phase microextraction (micro SPE) of four anabolic steroids and six β-blockers from aqueous samples of environmental importance, prior to their HPLC-diode array detector analysis. As the ionic liquid is covalently attached to graphene oxide sheets, it is made possible for it to participate in the dispersive micro SPE procedure. The limits of detection and limits of quantification of the proposed method were found to be in the range of 7-23ng/L and between 20 and 70ng/L, respectively. The linearity was satisfactory, with the determination coefficients to range from 0.9940 to 0.9998 while the within- and between-day relative standard deviation of the method ranged between 3.1 and 7.6% and from 4.0 to 8.5%, respectively. In order to test the applicability of the proposed method in real-life samples, the effluent from a municipal wastewater treatment plant as well as natural water samples from two rivers and a lake were collected and analyzed. After the analysis of samples, the effluent from municipal wastewater treatment plant was fortified with the analytes, at concentrations equal to 2 and 10 times the LOQs. Recoveries were calculated after subtracting the native (no-spike) concentrations of analytes, when needed. All the recoveries were in the range of 87-98%. A comparison study attests to the superiority of the developed nanomaterial over graphene oxide and graphene for the dispersive micro SPE of steroids and β-blockers. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. The use of atomic force microscopy as an important technique to analyze the dispersion of nanometric fillers and morphology in nanocomposites and polymer blends based on elastomers

    Energy Technology Data Exchange (ETDEWEB)

    Sousa, Fabiula Danielli Bastos de; Scuracchio, Carlos Henrique, E-mail: fabiuladesousa@gmail.com [Universidade Federal do ABC (CECS/UFABC), Santo Andre, SP (Brazil). Centro de Engenharia, Modelagem e Ciencias Sociais Aplicadas

    2014-11-15

    AFM has been recognized as one of the most powerful tools for the analysis of surface morphologies because it creates three-dimensional images at angstrom and nano scale. This technique has been exhaustively used in the analyses of dispersion of nanometric components in nanocomposites and in polymer blends, because of the easiness of sample preparation and lower equipment maintenance costs compared to electron microscopy. In this review, contributions using AFM are described, with emphasis on the dispersion of nanofillers in polymeric matrices. It is aimed to show the importance of technical analysis for nanocomposites and polymer blends based on elastomers. (author)

  9. The Effect of the SCAMPER Technique in Raising Awareness Regarding the Collection and Utilization of Solid Waste

    Science.gov (United States)

    Çelikler, Dilek; Harman, Gonca

    2015-01-01

    The aim of this study was to determine the effect of the SCAMPER technique in raising awareness among science students regarding the collection and utilization of solid waste. The participants included a total of 65 third-year students. According to the study results, the science students described schools and visual media as their main source of…

  10. Evaluation of a solid-phase RIA technique and a solid-phase ELISA technique for demonstrating hepatitis-B surface antigen

    International Nuclear Information System (INIS)

    Vranckx, R.; Cole, J.; Peetermans, M.

    1978-01-01

    The sensitivities of a solid-phase radioimmunoassay (RIA), a solid-phase enzyme immunoassay (ELISA) and a haemagglutination test (RPHA) for the detection of the hepatitis-B surface antigen (HBsAg) were compared (1) by screening a panel of 300 sera (97 positives and 203 negatives), and (2) by titrating serial dilutions of 10 positive sera. Ninety-seven sera were positive by RIA, 95% were detected by ELISA and 81% were detected by RPHA. In the serial dilutions, the average end-points of the titrations were 0.005ng/ml for RIA, 0.01ng/ml for ELISA and 0.04 ng/ml for RPHA. It can be concluded that the sensitivity of the ELISA test is intermediate between that of the RIA and the RPHA. The ELISA and the RPHA tests seem to be a little more sensitive for the detection of subtype ay than for the detection of subtype ad. (author)

  11. 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.

  12. Study of the dissolution velocity of dispersed solid particles. Development of a calculation method for analyzing the kinetic curves. Extension to the study of composed kinetics

    International Nuclear Information System (INIS)

    Jorda, Michel.

    1976-01-01

    The dissolution of a solid in an aqueous phase is studied, the solid consisting of dispersed particles. A continuous colorimetric analysis method is developed to study the dissolution process and a two-parameter optimization method is established to investigate the kinetic curves obtained. This method is based on the differential equation dx/dt=K(1-x)sup(n). (n being the decrease in the dissolution velocity when the dissolved part increases and K a velocity parameter). The dissolution of SO 4 Cu and MnO 4 K in water and UO 3 in SO 4 H 2 is discussed. It is shown that the dissolution velocity of UO 3 is proportional to the concentration of the H + ions in the solution as far as this one is not higher than 0.25N. The study of the temperature dependence of the UO 3 dissolution reaction shows that a transition phase takes place from 25 to 65 0 C between a phase in which the dissolution is controlled by the diffusion of the H + ions and the chemical reaction at the interface and a phase in which the kinetics is only controlled by the diffusion [fr

  13. A Novel Solid State Non-Dispersive Infrared CO2 Gas Sensor Compatible with Wireless and Portable Deployment

    Directory of Open Access Journals (Sweden)

    Desmond Gibson

    2013-05-01

    Full Text Available This paper describes development of a novel mid-infrared light emitting diode (LED and photodiode (PD light source/detector combination and use within a non-dispersive infrared (NDIR carbon dioxide gas sensor. The LED/PD based NDIR sensor provides fast stabilisation time (time required to turn on the sensor from cold, warm up, take and report a measurement, and power down again ≈1 second, longevity (>15 years, low power consumption and low cost. Described performance is compatible with “fit and forget” wireless deployed sensors in applications such as indoor air quality monitoring/control & energy conservation in buildings, transport systems, horticultural greenhouses and portable deployment for safety, industrial and medical applications. Fast stabilisation time, low intrinsic power consumption and cycled operation offer typical energy consumption per measurement of mJ’s, providing extended operation using battery and/or energy harvesting strategies (measurement interval of ≈ 2 minutes provides >10 years operation from one AA battery. Specific performance data is provided in relation to measurement accuracy and noise, temperature performance, cross sensitivity, measurement range (two pathlength variants are described covering ambient through to 100% gas concentration, comparison with NDIR utilizing thermal source/pyroelectric light source/detector combination and compatibility with energy harvesting. Semiconductor based LED/PD processing together with injection moulded reflective optics and simple assembly provide a route to low cost high volume manufacturing.

  14. A novel solid state non-dispersive infrared CO2 gas sensor compatible with wireless and portable deployment.

    Science.gov (United States)

    Gibson, Desmond; MacGregor, Calum

    2013-05-29

    This paper describes development of a novel mid-infrared light emitting diode (LED) and photodiode (PD) light source/detector combination and use within a non-dispersive infrared (NDIR) carbon dioxide gas sensor. The LED/PD based NDIR sensor provides fast stabilisation time (time required to turn on the sensor from cold, warm up, take and report a measurement, and power down again ≈1 second), longevity (>15 years), low power consumption and low cost. Described performance is compatible with "fit and forget" wireless deployed sensors in applications such as indoor air quality monitoring/control & energy conservation in buildings, transport systems, horticultural greenhouses and portable deployment for safety, industrial and medical applications. Fast stabilisation time, low intrinsic power consumption and cycled operation offer typical energy consumption per measurement of mJ's, providing extended operation using battery and/or energy harvesting strategies (measurement interval of ≈ 2 minutes provides >10 years operation from one AA battery). Specific performance data is provided in relation to measurement accuracy and noise, temperature performance, cross sensitivity, measurement range (two pathlength variants are described covering ambient through to 100% gas concentration), comparison with NDIR utilizing thermal source/pyroelectric light source/detector combination and compatibility with energy harvesting. Semiconductor based LED/PD processing together with injection moulded reflective optics and simple assembly provide a route to low cost high volume manufacturing.

  15. Effervescence-assisted dispersive solid-phase extraction using ionic-liquid-modified magnetic β-cyclodextrin/attapulgite coupled with high-performance liquid chromatography for fungicide detection in honey and juice.

    Science.gov (United States)

    Wu, Xiaoling; Yang, Miyi; Zeng, Haozhe; Xi, Xuefei; Zhang, Sanbing; Lu, Runhua; Gao, Haixiang; Zhou, Wenfeng

    2016-11-01

    In this study, a simple effervescence-assisted dispersive solid-phase extraction method was developed to detect fungicides in honey and juice. Most significantly, an innovative ionic-liquid-modified magnetic β-cyclodextrin/attapulgite sorbent was used because its large specific surface area enhanced the extraction capacity and also led to facile separation. A one-factor-at-a-time approach and orthogonal design were employed to optimize the experimental parameters. Under the optimized conditions, the entire extraction procedure was completed within 3 min. In addition, the calibration curves exhibited good linearity, and high enrichment factors were achieved for pure water and honey samples. For the honey samples, the extraction efficiencies for the target fungicides ranged from 77.0 to 94.3% with relative standard deviations of 2.3-5.44%. The detection and quantitation limits were in the ranges of 0.07-0.38 and 0.23-1.27 μg/L, respectively. Finally, the developed technique was successfully applied to real samples, and satisfactory results were achieved. This analytical technique is cost-effective, environmentally friendly, and time-saving. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Bio-dispersive liquid liquid microextraction based on nano rhaminolipid aggregates combined with magnetic solid phase extraction using Fe3O4@PPy magnetic nanoparticles for the determination of methamphetamine in human urine.

    Science.gov (United States)

    Haeri, Seyed Ammar; Abbasi, Shahryar; Sajjadifar, Sami

    2017-09-15

    In the present investigation, extraction and preconcentration of methamphetamine in human urine samples was carried out using a novel bio-dispersive liquid liquid microextraction (Bio-DLLME) technique coupled with magnetic solid phase extraction (MSPE). Bio-DLLME is a kind of microextraction technique based nano-materials which have potential capabilities in many application fields. Bio-DLLME is based on the use of a binary part system consisting of methanol and nano rhaminolipid biosurfactant. Use of this binary mixture is ecologically accepted due to their specificity, biocompatibility and biodegradable nature. The potential of nano rhaminolipid biosurfactant as a biological agent in the extraction of organic compounds has been investigated in recent years. They are able to partition at the oil/water interfaces and reduce the interfacial tension in order to increase solubility of hydrocarbons. The properties of the prepared Fe 3 O 4 @PPy magnetic nanoparticles were characterized using Fourier transform infrared spectroscopy and X-ray diffraction methods The influences of the experimental parameters on the quantitative recovery of analyte were investigated. Under optimized conditions, the enrichment factor was 310, the calibration graph was linear in the methamphetamine concentration range from 1 to 60μgL -1 , with a correlation coefficient of 0.9998. The relative standard deviations for six replicate measurements was 5.2%. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Design of in situ dispersible and calcium cross-linked alginate pellets as intestinal-specific drug carrier by melt pelletization technique.

    Science.gov (United States)

    Nurulaini, Harjoh; Wong, Tin Wui

    2011-06-01

    Conventional alginate pellets underwent rapid drug dissolution and loss of multiparticulate characteristics such as aggregation in acidic medium, thereby promoting oral dose dumping. This study aimed to design sustained-release dispersible alginate pellets through rapid in situ matrix dispersion and cross-linking by calcium salts during dissolution. Pellets made of alginate and calcium salts were prepared using a solvent-free melt pelletization technique that prevented reaction between processing materials during agglomeration and allowed such a reaction to occur only in dissolution phase. Drug release was remarkably retarded in acidic medium when pellets were formulated with water-soluble calcium acetate instead of acid-soluble calcium carbonate. Different from calcium salt-free and calcium carbonate-loaded matrices that aggregated or underwent gradual erosion, rapid in situ solvation of calcium acetate in pellets during dissolution resulted in burst of gas bubbles, fast pellet breakup, and dispersion. The dispersed fragments, though exhibiting a larger specific surface area for drug dissolution than intact matrix, were rapidly cross-linked by Ca(2+) from calcium acetate and had drug release retarded till a change in medium pH from 1.2 to 6.8. Being dispersible and pH-dependent in drug dissolution, these pellets are useful as multiparticulate intestinal-specific drug carrier without exhibiting dose dumping tendency of a "single-unit-like" system via pellet aggregation. Copyright © 2011 Wiley-Liss, Inc.

  18. Large-eddy simulation and Lagrangian stochastic modelling of solid particle and droplet dispersion and mixing. Application to atmospheric pollution; Dispersion et melange turbulents de particules solides et de gouttelettes par une simulation des grandes echelles et une modelisation stochastique lagrangienne. Application a la pollution de l'atmosphere

    Energy Technology Data Exchange (ETDEWEB)

    Vinkovic, I.

    2005-07-15

    In order to study atmospheric pollution and the dispersion of industrial stack emissions, a large eddy simulation with the dynamic Smagorinsky-Germano sub-grid-scale model is coupled with Lagrangian tracking of fluid particles containing scalar, solid particles and droplets. The movement of fluid particles at a sub-grid level is given by a three-dimensional Langevin model. The stochastic model is written in terms of sub-grid-scale statistics at a mesh level. By introducing a diffusion model, the coupling between the large-eddy simulation and the modified three-dimensional Langevin model is applied to passive scalar dispersion. The results are validated by comparison with the wind-tunnel experiments of Fackrell and Robins (1982). The equation of motion of a small rigid sphere in a turbulent flow is introduced. Solid particles and droplets are tracked in a Lagrangian way. The velocity of solid particles and droplets is considered to have a large scale component (directly computed by the large-eddy simulation) and a sub-grid scale part. Because of inertia and gravity effects, solid particles and droplets, deviate from the trajectories of the surrounding fluid particles. Therefore, a modified Lagrangian correlation timescale is introduced into the Langevin model previously developed for the sub-grid velocity of fluid particles. Two-way coupling and collisions are taken into account. The results of the large-eddy simulation with solid particles are compared with the wind-tunnel experiments of Nalpanis et al. (1993) and of Taniere et al. (1997) on sand particles in saltation and in modified saltation, respectively. A model for droplet coalescence and breakup is implemented which allows to predict droplet interactions under turbulent flow conditions in the frame of the Euler/Lagrange approach. Coalescence and breakup are considered as a stochastic process with simple scaling symmetry assumption for the droplet radius, initially proposed by Kolmogorov (1941). At high

  19. SOLUBILITY AND BIOAVAILABILITY ENHANCEMENT STRATEGIES FOR EFFECTIVE DELIVERY OF POORLY WATER SOLUBLE DRUGS BY NANO FORMULATIONS AND SOLID DISPERSIONS

    OpenAIRE

    Rayapolu Ranga Goud*, Gunnala Krishnaveni, Girija Prasad Patro

    2018-01-01

    For the ancient few years, there has been a substantial research done on diverse methodologies for poorly water soluble and lipophilic drugs. More in modern times voluminous molecules cannot be distributed due to low solubility. Now a day frequently, particulate vesicle systems such as nanoparticles, liposomes, microspheres, niosomes, pronisomes, ethosomes, and proliposomes have been used as drug carriers. Drug delivery designates the technique and methodology to conveying medications or drug...

  20. Biological treatment of soils contaminated with hydrophobic organics using slurry and solid phase techniques

    International Nuclear Information System (INIS)

    Cassidy, D.P.; Irvine, R.L.

    1995-01-01

    Both slurry-phase and solid-phase bioremediation are effective ex situ soil decontamination methods. Slurry is energy intensive relative to solid-phase treatment, but provides homogenization and uniform nutrient distribution. Limited contaminant bioavailability at concentrations above the required cleanup level reduces biodegradation rates and renders solid phase bioremediation more cost effective than complete treatment in a bioslurry reactor. Slurrying followed by solid-phase bioremediation combines the advantages and minimizes the weaknesses of each treatment method when used alone. A biological treatment system consisting of slurrying followed by aeration in solid phase bioreactors was developed and tested in the laboratory using a silty clay load contaminated with diesel fuel. The first set of experiments was designed to determine the impact of the water content and mixing time during slurrying on the ate and extent of contaminant removal in continuously aerated solid phase bioreactors. The second set of experiments compared the volatile and total diesel fuel removal in solid phase bioreactors using periodic and continuous aeration strategies

  1. 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).

  2. 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.

  3. Biological treatment of soils contaminated with hydrophobic organics using slurry- and solid-phase techniques

    Science.gov (United States)

    Cassidy, Daniel H.; Irvine, Robert L.

    1995-10-01

    Both slurry-phase and solid-phase bioremediation are effective ex situ soil decontamination methods. Slurrying is energy intensive relative to solid-phase treatment, but provides homogenization and uniform nutrient distribution. Limited contaminant bioavailability at concentrations above the required cleanup level reduces biodegradation rates and renders solid phase bioremediation more cost effective than complete treatment in a bio-slurry reactor. Slurrying followed by solid-phase bioremediation combines the advantages and minimizes the weaknesses of each treatment method when used alone. A biological treatment system consisting of slurrying followed by aeration in solid phase bioreactors was developed and tested in the laboratory using a silty clay loam contaminated with diesel fuel. The first set of experiments was designed to determine the impact of the water content and mixing time during slurrying on the rate an extent of contaminant removal in continuously aerated solid phase bioreactors. The second set of experiments compared the volatile and total diesel fuel removal in solid phase bioreactors using periodic and continuous aeration strategies. Results showed that slurrying for 1.5 hours at a water content less than saturation markedly increased the rate and extent of contaminant biodegradation in the solid phase bioreactors compared with soil having no slurry pretreatment. Slurrying the soil at or above its saturation moisture content resulted in lengthy dewatering times which prohibited aeration, thereby delaying the onset of biological treatment in the solid phase bioreactors. Results also showed that properly operated periodic aeration can provide less volatile contaminant removal and a grater fraction of biological contaminant removal than continuous aeration.

  4. Evaluation of a solid phase R.I.A. technique and solid phase E.L.I.S.A. technique for the demonstration of hepatitis B surface antigen

    International Nuclear Information System (INIS)

    Vranckx, R.; Cole, J.; Peetermans, M.

    1977-01-01

    We compared the sensitivity of a solidphase radio-immunoassay (R.I.A.), a solid-phase enzyme-immunoassay (E.L.I.S.A.) and a hemagglutination test (R.P.H.A.) for the detection of the HBs Ag in two ways: 1) by screening a panel of 300 sera (97 positives and 203 negatives) 2) by titrating serial dilutions of 10 positive sera. Ninety seven sera were positive by R.I.A., 95% were detected by E.L.I.S.A. and 81% were detected by R.P.H.A. In the serial dilutions the average end points of the titration were for R.I.A. 0.005 ng/ml, for E.L.I.S.A. 0,01 ng/ml and for R.P.H.A. 0.04 ng/ml. It can be concluded that the sensitivity of the E.L.I.S.A. test is intermediate between the sensitivity of the R.I.A. and the sensitivity of the R.P.H.A. The E.L.I.S.A. and the R.P.H.A. tests seam to be a little more sensitive for the detection of subtype ay than the detection of subtype ad. (orig.) [de

  5. PHYSIOLOGICAL REGULATION OF PROTEASE AND ANTIBIOTICS IN PENICILLIUM SP. USING SUBMERGED AND SOLID STATE FERMENTATION TECHNIQUES

    OpenAIRE

    HAIDER M. HAMZAH; ANWAR H.L. Ali; HAMID G. HASSAN

    2009-01-01

    A fungal strain belonging to the genus Penicillium was isolated from soil sample and has been diagnosed as Penicillium sp. according to its morphological characteristics of the colonies on solid media and also microscopical examination of the fungal parts. Antibiotics, protease activity and pH values were determined after cultivation of the fungus using submerged fermentation (SF) and solid state fermentation (SSF). The two different patterns of fermentation processes seem to influence the ph...

  6. 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